Simultaneous determination of Spirotetramat, Flonicamid, Procymidone and Cyprodinil residues in 10 dehydrated vegetables by modified QuEChERS technique and GC-MS/MS analysis | Research Square window.SnipcartSettings = { analytics: { enabled: false } }; (function() { var accessVector = localStorage.getItem('access_vector') || ''; window.dataLayer = window.dataLayer || []; if (accessVector) { window.dataLayer.push({ user: { profile: { profileInfo: { snid: accessVector } } } }); } })(); (function(w,d,s,l,i){w[l]=w[l]||[];w[l].push({'gtm.start':new Date().getTime(),event:'gtm.js'});var f=d.getElementsByTagName(s)[0],j=d.createElement(s),dl=l!='dataLayer'?'&l='+l:'';j.async=true;j.src='https://www.googletagmanager.com/gtm.js?id='+i+dl;f.parentNode.insertBefore(j,f);})(window,document,'script','dataLayer','GTM-K279D39R'); Browse Preprints In Review Journals COVID-19 Preprints AJE Video Bytes Research Tools Research Promotion AJE Professional Editing AJE Rubriq About Preprint Platform In Review Editorial Policies Our Team Advisory Board Help Center Sign In Submit a Preprint Cite Share Download PDF Article Simultaneous determination of Spirotetramat, Flonicamid, Procymidone and Cyprodinil residues in 10 dehydrated vegetables by modified QuEChERS technique and GC-MS/MS analysis Qiangqiang Qi, Yajun Zhang, Yuan Liu, Jiangtao Ma, Xueping Ma This is a preprint; it has not been peer reviewed by a journal. https://doi.org/ 10.21203/rs.3.rs-6310718/v1 This work is licensed under a CC BY 4.0 License Status: Posted Version 1 posted You are reading this latest preprint version Abstract In the future, the demand for dehydrated vegetables will steadily increase to support agricultural resilience and drive food quality higher. At the same time, the safety and health of dehydrated vegetables will gain heightened awareness among the general population, reflecting critical public health implications.A simultaneous analytical method was developed to detect spirotetramat, procymidone, flonicamid, and cyprodinil in dehydrated vegetables. This innovative approach employed the QuEChERS sample preparation technique, ensuring precise weighing into rotating Centrifuge tubes for high precision. The method utilized Gas Chromatography Tandem Mass Spectrometry (GC-MS/MS), a highly sensitive and accurate analytical technique, to provide detailed spectral data for the detection of these compounds.The analysis yielded linear ranges of 0.005–0.250 μg/mL, indicating significant relationships between concentration and detection results (correlation coefficients > 0.9994). The recovery rates across varying levels of purity (high, medium, low) were satisfactory, with spiked sample recovery rates ranging from 78.1% to 113.2%. Additionally, the relative standard deviation for ten consecutive measurements averaged below 5%, demonstrating consistent reproducibility and reliability in this detection system.The use of GC-MS/MS provided high efficiency and specificity, making it suitable for detecting trace compounds in dehydrated vegetables. These findings contribute to advancing analytical techniques for food and agricultural residue analysis and offer practical applications in improving food safety and quality control. Physical sciences/Chemistry Physical sciences/Chemistry/Biochemistry Physical sciences/Chemistry/Biosynthesis QuEChERS GC-MS/MS Pesticide residues Dehydrated vegetables Figures Figure 1 Figure 2 1. Introduction Historically, the availability of fresh vegetables has been profoundly influenced by seasonal variations. To enhance storability and transportability, fresh vegetables undergo a series of processing steps, including washing and drying, to produce a shelf-stable product that preserves the original pigmentation and nutrient profile. This processed commodity, characterized by its convenience and minimal moisture content, is scientifically referred to as dehydrated vegetables(DVs) 1-5 . Rehydratable vegetables (RVs), defined as dehydrated plant-based foods requiring only water immersion for reconstitution, have served as a critical agricultural strategy to address supply-demand imbalances in seasonal vegetable production systems 6 . Their extended storage stability enabled year-round availability, effectively bridging gaps between surplus harvests and off-season shortages 7-8 . Recent technological advancements have expanded their utility beyond terrestrial applications, positioning them as ideal candidates for space exploration diets due to their extended shelf life, lightweight properties, and minimal resource requirements during preparation 9 . To enhance vegetable yield and ameliorate postharvest storage quality, the application of agrochemicals such as pesticides and fungicides is routinely employed for the management and mitigation of phytopathogens and pest infestations 10-11 .Spinetoram and flonicamid are characterized by their low toxicity, distinctive systemic translocation capabilities, and favorable selectivity for beneficial insects, making them effective agents for the management of piercing-sucking pest populations 12 . Procymidone and cyprodinil, two systemic fungicides, are extensively employed in the management of gray mold disease (caused by Botrytis cinerea) and various other phytopathogenic fungi 13-14 .The improper application of agricultural pesticides and fungicides has resulted in concerning levels of chemical residues in food products, posing substantial risks to human health. This issue has raised significant concerns among both the public and scientific communities regarding food safety and long-term health consequences 15-16 . The QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) extraction method represents an innovative advancement in dispersive solid-phase extraction technology, distinguished by its minimal reagent requirements, expedited extraction kinetics, streamlined operational workflow, and superior analytical precision 17-18 . Over the past decade, this methodology has emerged as a predominant analytical approach for pesticide residue analysis in plant-derived matrices, owing to its exceptional performance characteristics and adaptability to high-throughput screening protocols 19 .The Selected Reaction Monitoring (SRM) mode in GC-MS/MS demonstrates enhanced selectivity and superior anti-interference capability by screening specific ion pairs of target compounds, thereby highlighting its advantages in qualitative analysis. This approach is particularly suitable for detecting samples with complex matrices due to its improved specificity.In this investigation, the QuEChERS methodology was utilized for the extraction and purification of four distinct pesticides from a variety of dehydrated vegetables. The operational parameters for GC-MS/MS were meticulously optimized to enhance analytical performance 20-21 . The separation and quantification of the target analytes were achieved through the implementation of the Selected Reaction Monitorin (SRM) mode in GC-MS/MS. Cis-heptachlor epoxide was employed as an internal standard to ensure the accuracy and precision of the measurements 22 . The developed method was successfully applied for the concurrent detection and quantification of spirotetramat, procymidone, flonicamid, and cyprodinil residues in the selected dehydrated vegetable matrices. 2. Materials and Methods 2.1 Chemicals and Reagents All organic solvents including methanol, acetonitrile, acetone, ethyl acetate, dichloromethane, and hexane (HPLC grade) were procured from Merck KGaA (Darmstadt, Germany). Sample preparation consumables consisting of 50 mL extract tubes containing premeasured QuEChERS salts (4 g magnesium sulfate, 1 g sodium chloride, 1 g sodium citrate sesquihydrate, and 0.5 g disodium citrate dehydrate; 25 tubes per package) and 15 mL purification tubes packed with 900 mg magnesium sulfate and 150 mg primary secondary amine (PSA) sorbent (25 units per box) were obtained from GEMSS Science and Technology Co., Ltd. (Dalian, China) 17 . Ultrapure water (18.2 MΩ·cm resistivity) was produced using a Milli-Q Integral water purification system (MilliporeSigma, Molsheim, France). 2.2 Standards Individual certified pesticide reference standards (Flonicamid, Cyprodinil, Procymidone, and Spirotetramat) at 1000 mg L⁻¹ concentration were obtained from the Chinese Academy of Metrological Science. Primary stock solutions were maintained in sealed amber glass ampoules under dark storage conditions at -20°C.A multi-component working standard mixture containing 10 mg L⁻¹ of each analyte was prepared in HPLC-grade acetone. This intermediate standard solution was aliquoted into amber glass vials with PTFE-lined caps and stored at 4°C for no more than three months to maintain stability. The working solution served as the primary source for calibration standards through serial dilution with dichloromethane-acetone solvent system (2:8, v/v).The calibration standards spanning concentrations of 5, 10, 20, 50, 100, 200, and 250μg/L were prepared through serial dilution of a stock solution in a dichloromethane-acetone solvent system (2:8, v/v). Appropriate aliquots of a multi-component standard mixture were sequentially diluted with the mixed organic solvent to achieve the required concentration levels for calibration curve construction.Certified cis-heptachlor epoxide reference standards (1,000 mg/L in ethyl acetate) were purchased from Alta Technology (Tianjin, China) as internal standards. The certified reference materials (CRMs) were supplied in sealed glass ampules and stored under light-protected conditions. Working solutions (100 μg/L) were prepared by diluting stock solutions with ethyl acetate and utilized for both calibration curves (5–250 μg/L) and sample quantification. All solutions were aliquoted into amber glass vials and stored at -20°C until analysis to minimize degradation 23 . 2.3 Instruments The experiment was performed ina Trace 1600 GC (Thermo Fisher) coupled to an TSQ 9610 Triple Quadrupole Mass Spectrometer(Thermo Fisher) and a Triplus RSH autosampler(Thermo Fisher) . The machine had a split/splitless injector with an electronic pressure control system, the injector Temperature maintained at 280℃. A 1μL target solution was introduced into the system through an injector. The injection was performed in pulsed splitless mode with a pulse pressure of 200kPa and a duration of 0.75min. A TG-5SILMS(30m×250μm,0.25μm) (Thermo Fisher)was used to separate the analytes in the sample, including filter sample solutions, blank sample solutions, and mixed standard solutions. the carrier gas was high purity helium at a flow rate of 1.20mL/min. The GC oven temperature program started at 50℃ for 1.5min, followed by a gradient increase of 25℃/min until 90℃and held for 1.5 min. It was then increased to 180 ℃at a rate of 25 ℃/min, 180 ℃ to 280 C at 8℃/min and finally raised to 300 ℃ at 10℃/min and hold 5min.The ion sources were operated at an electron energy of 70eV. the ion source and the transfer line temperatures were maintained at 280℃, and Selected Reaction Monitorin (SRM) was applied 24 . Total time of analysis: 20.43 min. 2.4 Collection and Preservation of Samples Fresh vegetable specimens for pesticide analysis were procured from commercial retail outlets (supermarkets and convenience stores) in Yinchuan, Ningxia Hui Autonomous Region. Parallel blank control samples were obtained from local subsistence farmers who maintained pesticide-free cultivation practices, with absence of pesticide residues confirmed through preliminary screening. All specimens underwent immediate cryopreservation at-20°C within 2 hours of collection . Following a 40-hour lyophilization process using a CTFD-100S vacuum freeze-dryer (Yonghe Chuangxin Electronic Technology Co., Ltd., Qingdao, China), the samples were homogenized to fine powder (particle size <100 μm) 25 . Processed samples were aliquoted into sterile 250 mL polypropylene containers (Corning Inc.) and maintained at -20°C in temperature-controlled laboratory refrigeration units (Thermo Scientific TSX Series) until analysis. 2.5 Extraction and cleanup with QuEChERS method Dehydrated vegetable samples were prepared using a modified QuEChERS method based on AOAC Official Method 2007.01 18 . Specifically, 0.50 g aliquots of homogenized samples were accurately weighed into 50 mL olyproppylene centrifuge tubes. The extraction process commenced with the addition of 4.5 mL ultrapure water (18.2 MΩ·cm at 25°C) 26 , followed by vigorous vortex mixing (HMG-WX vortex mixer, IKA, Germany) for 1 min. The hydrated samples were then equilibrated at room temperature (25 ± 2°C) for 15 min. Subsequently, 10.0 mL acetonitrile (HPLC grade) containing ceramic homogenizers (1 cm diameter) was added to each tube, followed by another 1 min vortex mixing step to ensure complete sample dispersion. The homogenized mixtures were immediately transferred to a -20°C freezer (±1°C) for 30 min to facilitate phase separation and protein precipitation. Following the addition of a dehydrated salt packet (anhydrous sodium sulfate, >99% purity), the sample tubes were immediately subjected to vigorous manual shaking for 60 s. Primary phase separation was achieved through centrifugation at 4200 rpm (rcf 2500 × g) for 5 min using a benchtop centrifuge (Eppendorf 5804, Hamburg, Germany). A precisely measured 6.00 mL aliquot of the resulting supernatant was carefully transferred to a 15 mL purification tube (PTFE-lined cap). The secondary extraction phase involved vortex mixing (VM-300, maximal intensity) for 60 s followed by centrifugation at 4500 rpm (rcf 3000 × g) for 5 min. Subsequently, 5.00 mL (5000 μL) of the purified upper organic layer was quantitatively transferred to a 10 mL graduated glass test tube with PTFE-sealed cap. Solvent evaporation was conducted using a nitrogen evaporator (N-EVAP 116, Organomation Associates Inc., Berlin, MA, USA) maintained at 45±1°C with continuous N₂ flow (15 psi) until complete removal of acetonitrile was visually confirmed (no meniscus observed). The dried residue was then reconstituted in 1.00 mL of a freshly prepared solvent mixture containing acetone and dichloromethane (2:8 v/v, HPLC grade) with 30 s vortex-assisted dissolution. Following three consecutive 1-minute vortexing cycles, the homogenized mixture was transferred to a 2.0 mL screw-cap glass vial. Prior to GC-MS/MS analysis, the sample was purified through a 0.22 μm needle-type membrane filter (PTFE, 25 mm diameter) using sterile syringe filtration techniques. For fresh vegetable samples, aliquots (5.0 g) were accurately weighed into 50 mL centrifuge tubes, followed by immediate addition of 10.0 mL acetonitrile to each tube. For matrix-matched blank samples, appropriate aliquots of the working multistandard solution were spiked into the matrix followed by a 30-minute equilibrium period at ambient temperature (25±2°C) to facilitate pesticide migration and matrix interaction prior to subsequent extraction procedures 27 . 3. Result and discussion 3.1 Optimization of Chromatography-MS Analytical Parameters The retention times of target compounds were determined through full-scan analyses using a 1.0 mg/L multi-component standard mixture. Analyses were performed in electron ionization(EI) mode with a mass-to-charge (m/z) range of 50-550. Optimal precursor/product ion pairs and collision energies were automatically optimized using an intelligent SRM system(Thermo Fisher) with high-purity helium (99.999%) as collision gas. The mass spectrometer was operated in selective reaction monitoring (SRM) mode for routine analysis. Both quantification and qualification of analytes were achieved by monitoring three characteristic SRM transitions per compound, with peak area ratios used for confirmation. All analytical results are summarized in Table 1. Tab 1 Retention Time, MS Quantitation and Confirming Peak of 5 compounds Component name Retention Time(min) MS Quantitation Peak(eV) MS Confirming Peak (eV ) Flonicamid 6.48 146>126(8eV) 174>69(36eV);175.1>147(8eV) Cyprodinil 11.63 224.1>208.1(16eV) 224.1>207.1(36eV);224.1>222.1(18eV) cis-Heptachlor Epoxide 12.00 352.8>262.9(16eV) 262.9>192(30eV);354.7>264.9(12eV)) Procymidone 12.34 283>96.1(8eV) 285>96.1(8eV);283>67.1(26eV); Spirotetramat 17.24 270.1>216.1(14eV) 268.1>214.1(8eV); 286.1>216.1(12eV) 3.2 Optimal Constant-Volume Solvent Screening Standard solutions (100 μg/L) were prepared using methanol, acetonitrile, acetone, ethyl acetate, dichloromethane, and n-hexane as individual solvents. The response values of target analytes were subsequently determined using [instrument name/model]. As illustrated in Fig. 1, the acetone- dichloromethane mixed solvent system (2:8, v/v) demonstrated optimal response characteristics. Therefore, this binary solvent mixture was selected as the working solvent for both sample preparation and calibration curve construction throughout the experimental protocol. 3.3 Calibration Curve Properties and Statistical Analysis Calibration curves were established for Flonicamid, Cyprodinil, Procymidone, and Spirotetramat across a concentration range of 5-250 ng/mL, demonstrating excellent linearity with correlation coefficients (r) > 0.9994 (Table 2). Method sensitivity was evaluated through limits of detection (LOD) and quantification (LOQ), determined as signal-to-noise ratios (S/N) of 3:1 and 10:1, respectively, based on 0.5 g sample aliquots. The calculated LOD and LOQ values for all analytes were <0.00085 mg/kg and <0.0016 mg/kg, respectively, meeting EU Commission Regulation 2021/808 requirements for pesticide residue analysis 28. Tab.2 Calibration Curve Properties and statistical analysis of Flonicamid , Cyprodinil, Procymidone and Spirotetramat Pesticides Linear regression equation Correlation coefficient (r) Detection limit (mg/kg) Quantitative limit (mg/kg) Flonicamid y=3559.526x-8.009 0.9997 0.00025 0.00085 Cyprodinil y=6980.959x-3.328 0.9997 0.00023 0.00062 Procymidone y=2439.980x-1.656 0.9994 0.00085 0.0016 Spirotetramat y=1233.681x+3.393 0.9995 0.00020 0.00067 3.4 Chronotropic Soaking Modulates Standard Addition Recovery The chromatographic and mass spectrometric responses of the internal standard in powdered samples exhibited time-dependent recovery patterns during immersion (1–30 min). Spiked recoveries increased significantly with immersion time from 1 to 15 min , but no statistically meaningful improvement was observed beyond 15 min (Fig. 2). This kinetic profile indicates that equilibrium was achieved within 15 min, justifying the selection of 15-min immersion in deionized water for subsequent experiments 3.5 Spiked Recovery and Precision The method validation demonstrated satisfactory analytical performance for vegetable matrix analysis. Ten blank vegetable powder samples were individually spiked with standard solutions at 0.05, 0.25, and 0.5 mg/kg, followed by extraction, purification, and GC-MS analysis using the established protocol. As shown in Table 3, recoveries of target components ranged from 78.1% to 113.2%, with relative standard deviations (RSDs) <5.00% across six replicate measurements. These values align with the recommended acceptance criteria for recovery (70–120%) and precision (RSD ≤15%) in complex food matrices 29 , confirming the reliability of the method for quantitative analysis. Tab. 3 Recovery and RSD of Four Pesticides in Dehydrated Vegetables Dehydrated Vegetables Pesticides recovery levels 0.05mg/kg 0.25mg/kg 0.50mg/kg Recovery rate RSD Recovery rate RSD Recovery rate RSD cucumbers Flonicamid 84.4-95.4 4.42 98.2-112.2 4.85 95.4-107.4 4.43 Cyprodinil 96.0-105.5 3.71 103.7-112.2 3.17 94.1-105.4 4.42 Procymidone 86.3-92.4 2.88 92.2-100.2 3.22 92.4-104.3 4.01 Spirotetramat 79.9-87.4 4,21 90.4-98.2 3.15 95.9-100.5 2.39 cumin Flonicamid 90.3-98.2 3.01 105.9-112.2 2.09 97.4-107.2 3.80 Cyprodinil 96.5-106.5 3.52 102.2-113.2 3.92 93.4-100.2 2.96 Procymidone 90.9-96.6 2.28 92.1-97.7 2.12 91.2-101.1 3.63 Spirotetramat 87.2-92.2 2.14 100.4-109.4 3.10 92.0-97.9 3.19 carrot Flonicamid 89.4-96.7 2.66 93.1-102.1 3.31 90.2-101.4 4.21 Cyprodinil 78.4-89.9 4.78 89.4-95.5 2.24 89.1-97.4 3.64 Procymidone 103.2-113.2 3.32 101.8-114.2 4.72 97.4-106.4 3.15 Spirotetramat 91.1-98.7 3.27 91.4-99.7 3.02 99.7-112.3 4.10 lycopene Flonicamid 86.6-95.2 3.45 89.9-95.1 2.40 92.4-97.7 1.98 Cyprodinil 82.9-87.3 3.06 89.2-97.2 3.02 94.9-104.4 3.55 Procymidone 83.6-93.0 4.79 86.7-95.5 3.93 93.2-103.9 4.09 Spirotetramat 85.3-95.3 4.50 97.7-110.0 4.71 99.4-110.4 4.66 eggplant Flonicamid 78.1-87.3 4.58 88.4-94.2 2.35 90.4-98.5 2.82 Cyprodinil 86.0-96.1 3.74 102.2-112.1 3.53 98.4-104.4 2.20 Procymidone 79.4-89.1 4.51 82.1-90.0 3.26 89.9-97.7 3.12 Spirotetramat 87.1-96.9 4.29 88.4-94.4 2.69 93.9-104.2 3.74 cabbage Flonicamid 79.4-85.1 3.15 90.4-102.1 3.77 93.3-97.5 2.66 Cyprodinil 85.1-93.4 4.11 92.1-96.8 2.13 93.4-100.8 2.03 Procymidone 89.6-99.2 4.63 90.2-101.0 3.38 89.2-96.9 1.99 Spirotetramat 79.6-88.8 4.34 83.7-90.2 3.00 88.2-94.7 2.13 Leek Flonicamid 83.3-91.3 4.04 89.7-96.2 3.42 90.4-104.6 3.35 Cyprodinil 88.2-94.1 2.70 87.2-97.3 2.85 87.2-95.8 3.27 Procymidone 93.6-105.2 4.87 98.4-110.1 4.39 95.5-103.4 4.08 Spirotetramat 82.4-95.4 4.92 90.1-100.5 3.53 92.8-105.3 4.00 celery Flonicamid 94.4-102.2 4.55 98.2-110.3 4.27 94.6-109.4 3.76 Cyprodinil 78.3-86.2 4.09 82.4-95.2 4.87 89.5-97.5 3.00 Procymidone 92.7-106.7 3.86 93.5-98.2 3.26 93.5-99.0 2.10 Spirotetramat 81.0-90.8 4.46 90.7-99.2 3.48 92.7-102.4 2.35 Chinese yam Flonicamid 87.5-96.5 3.56 89.0-98.3 3.78 94.8-105.5 3.28 Cyprodinil 92.3-103.6 4.06 96.4-107.5 3.18 96.0-104.1 2.65 Procymidone 97.4-110.1 3.03 95.3-110.6 2.73 93.1-100.4 2.11 Spirotetramat 78.3-89.4 4.00 83.8-95.0 4.07 82.5-93.4 3.81 Mushroom Flonicamid 84.1-96.9 4.78 89.1-103.2 4.89 93.6-101.7 2.97 Cyprodinil 90.1-96.6 2.01 90.7-97.8 2.63 93.4-99.2 1.35 Procymidone 93.2-110.0 4.51 92.5-102.6 2.93 92.1-107.4 2.98 Spirotetramat 98.5-111.4 4.90 96.3-104.0 3.94 91.9-100.5 1.62 3.6. Retained sample reanalysis To assess the impact of moisture on pesticide quantification, fresh vegetable samples (5.00 g) containing fludioxonil, pyrimethanil, putrescine, and spiropyrazolium ethyl residues were analyzed. Moisture content and pesticide residue levels were determined using the validated method. Fresh samples were lyophilized (freeze-dried) to eliminate water interference, and comparative analyses were performed before and after lyophilization. As summarized in Table 4, the relative deviations between pre- and post-lyophilization measurements for all target analytes were <5.00%, demonstrating minimal matrix effects from water content during residue analysis 29-30 . Tab.4 Variation of Four Pesticide Residues in Fresh Vegetables Pre- and Post-Dehydration Pesticides Vegetables water content(%) Weight before dehydration (g) Contents before dehydration(mg/kg) Weight after dehydration (g) Contents after dehydration(mg/kg) RSD(%) Procymidone cumin 94.2 5.0146 0.217 0.5018 0.221 1.55 cucumbers 95.1 5.0055 0.0787 0.4918 0.0812 3.11 Flonicamid eggplant 93.7 5.0154 0.114 0.5046 0.111 -1.74 carrot 88.7 4.9804 0.0924 0.4818 0.0917 -0.71 Spirotetramat celery 95.2 5.0194 0.346 0.4818 0.348 0.59 Cyprodinil lycopene 97.2 5.1492 0.274 0.4913 0.262 -4.57 cabbage 90.1 4.9954 0.222 0.5018 0.215 -3.27 4. Conclusion A robust and sensitive GC-MS/MS method was optimized for the simultaneous determination of flonicamid, cyprodinil, procymidone, and spirotetramat residues in dehydrated vegetables. The method integrates single-step QuEChERS-based extraction, rapid chromatographic separation (≤30 min runtime), and selected reaction monitoring (SRM) to achieve high selectivity (signal-to-noise ratio >50:1) with >85% reduction in matrix effects compared to full-scan modes. Validation results demonstrated recoveries of 78.1–113.2% and intra-day precision (RSD, n = 6) <5.00% across spiking levels of 0.05–0.5 mg/kg, fully compliant with EU SANTE guidelines for food safety monitoring. Declarations Author contributions Conceptualization: Qiang. Q.,Ya. Zh.,Yuan.L.,JIang. M.,Xue.M.. Methodology and Investigation: Qiang. Q,Ya. Zh.,Yuan.L., JIang. M.. Data Curationand Writing-Original Draf: Qiang. Q.,Ya. Zh.,Yuan.L..Writing—Review & Editing Qiang. Q,Ya. Zh. JIang. M..Funding acquisition: Qiang. Q,Ya. Zh.,Yuan.L.. All authors reviewed and approved the manuscript. 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Supplementary Files Fig.1Theconstructionofflowchartswithinthisarticle.jpeg Fig.2Chemicalstructurediagramoffourpesticides.jpeg Fig.3Mixedstandardsolutionblanksamplesolutionandsamplespikedsolutiontotalionchromatogram.jpeg Cite Share Download PDF Status: Posted Version 1 posted You are reading this latest preprint version Research Square lets you share your work early, gain feedback from the community, and start making changes to your manuscript prior to peer review in a journal. As a division of Research Square Company, we’re committed to making research communication faster, fairer, and more useful. We do this by developing innovative software and high quality services for the global research community. Our growing team is made up of researchers and industry professionals working together to solve the most critical problems facing scientific publishing. Also discoverable on Platform About Our Team In Review Editorial Policies Advisory Board Help Center Resources Author Services Accessibility API Access RSS feed Manage Cookie Preferences © Research Square 2026 | ISSN 2693-5015 (online) Privacy Policy Terms of Service Do Not Sell My Personal Information {"props":{"pageProps":{"initialData":{"identity":"rs-6310718","acceptedTermsAndConditions":true,"allowDirectSubmit":true,"archivedVersions":[],"articleType":"Article","associatedPublications":[],"authors":[{"id":435943384,"identity":"1f7c70f1-21e0-422c-bb3f-aa6a7ee57570","order_by":0,"name":"Qiangqiang Qi","email":"data:image/png;base64,iVBORw0KGgoAAAANSUhEUgAAAZAAAAAyAQMAAABI0h/eAAAABlBMVEX///8AAABVwtN+AAAACXBIWXMAAA7EAAAOxAGVKw4bAAAA00lEQVRIiWNgGAWjYFACxgYwZQBkPUioqCFNC7PBgzPHSLAMqIVN8mELM2GV8jOS26R5Ku4lbpdIflaR2MDGwN/enYDf8BuJQC1nihN3zkgzu5G4Q4ZB4szZDfi1SAC18LYlJG64kQDUcoYNKJKLX4v8DJCWfyAt6d8KEtuYCWthADmMtwGkJceMgSgtBmceNlvOOZZgvOHMm2KJhDPHeAj6Rb49/eGNNzUJshuOp2/8+KOiRo6/vZeAwxgYWCSQeTyElIMA8wdiVI2CUTAKRsEIBgDafkx01J7VEwAAAABJRU5ErkJggg==","orcid":"","institution":"Ningxia Center for Disease Control and Prevention, Ningxia Hui Autonomous Region Academy of Preventive Medicine","correspondingAuthor":true,"prefix":"","firstName":"Qiangqiang","middleName":"","lastName":"Qi","suffix":""},{"id":435943385,"identity":"b9ac0264-439b-412f-a0bb-b1ec26cef5d1","order_by":1,"name":"Yajun Zhang","email":"","orcid":"","institution":"Ningxia Center for Disease Control and Prevention, Ningxia Hui Autonomous Region Academy of Preventive Medicine","correspondingAuthor":false,"prefix":"","firstName":"Yajun","middleName":"","lastName":"Zhang","suffix":""},{"id":435943386,"identity":"21298e87-70e7-4c52-90ab-a7fb880c73e0","order_by":2,"name":"Yuan Liu","email":"","orcid":"","institution":"Ningxia Center for Disease Control and Prevention, Ningxia Hui Autonomous Region Academy of Preventive Medicine","correspondingAuthor":false,"prefix":"","firstName":"Yuan","middleName":"","lastName":"Liu","suffix":""},{"id":435943387,"identity":"b10b00d6-dff9-4a9d-9790-00fcb646eab1","order_by":3,"name":"Jiangtao Ma","email":"","orcid":"","institution":"Ningxia Center for Disease Control and Prevention, Ningxia Hui Autonomous Region Academy of Preventive Medicine","correspondingAuthor":false,"prefix":"","firstName":"Jiangtao","middleName":"","lastName":"Ma","suffix":""},{"id":435943388,"identity":"02b7d912-bd67-45ef-b40f-572ab18bf90e","order_by":4,"name":"Xueping Ma","email":"","orcid":"","institution":"Ningxia Center for Disease Control and Prevention, Ningxia Hui Autonomous Region Academy of Preventive Medicine","correspondingAuthor":false,"prefix":"","firstName":"Xueping","middleName":"","lastName":"Ma","suffix":""}],"badges":[],"createdAt":"2025-03-26 09:23:10","currentVersionCode":1,"declarations":"","doi":"10.21203/rs.3.rs-6310718/v1","doiUrl":"https://doi.org/10.21203/rs.3.rs-6310718/v1","draftVersion":[],"editorialEvents":[],"editorialNote":"","failedWorkflow":false,"files":[{"id":79726179,"identity":"a115d7ef-8e10-431e-bad2-13ab066a0a40","added_by":"auto","created_at":"2025-04-02 04:06:59","extension":"png","order_by":1,"title":"Figure 1","display":"","copyAsset":false,"role":"figure","size":538925,"visible":true,"origin":"","legend":"\u003cp\u003eComparative chromatographic responses of five pesticides (Flonicamid, Cyprodinil, cis-heptachlor epoxide, Procymidone, Spirotetramat) in six organic solvents\u003c/p\u003e","description":"","filename":"1.png","url":"https://assets-eu.researchsquare.com/files/rs-6310718/v1/dabd13cfbe69815a479edacc.png"},{"id":79726175,"identity":"43bd49c5-3453-4576-828d-98accd58f3f2","added_by":"auto","created_at":"2025-04-02 04:06:56","extension":"png","order_by":2,"title":"Figure 2","display":"","copyAsset":false,"role":"figure","size":57479,"visible":true,"origin":"","legend":"\u003cp\u003eLegend not included with this version.\u003c/p\u003e","description":"","filename":"2.png","url":"https://assets-eu.researchsquare.com/files/rs-6310718/v1/cc051040b14a0ee36d1406de.png"},{"id":83513267,"identity":"0b4ed903-04df-4cf3-8c87-08f2258e0365","added_by":"auto","created_at":"2025-05-27 17:31:36","extension":"pdf","order_by":0,"title":"","display":"","copyAsset":false,"role":"manuscript-pdf","size":1241967,"visible":true,"origin":"","legend":"","description":"","filename":"manuscript.pdf","url":"https://assets-eu.researchsquare.com/files/rs-6310718/v1/245092a1-10d4-49d5-a6b4-cd694492e131.pdf"},{"id":79726176,"identity":"9d1561b5-8522-4472-b044-2eaceb7e0225","added_by":"auto","created_at":"2025-04-02 04:06:56","extension":"jpeg","order_by":1,"title":"","display":"","copyAsset":false,"role":"supplement","size":55440,"visible":true,"origin":"","legend":"","description":"","filename":"Fig.1Theconstructionofflowchartswithinthisarticle.jpeg","url":"https://assets-eu.researchsquare.com/files/rs-6310718/v1/987757e51b1a257e6e1cb286.jpeg"},{"id":79726178,"identity":"8d3bcdad-e5b0-4fe9-b425-45d422a50498","added_by":"auto","created_at":"2025-04-02 04:06:56","extension":"jpeg","order_by":2,"title":"","display":"","copyAsset":false,"role":"supplement","size":16818,"visible":true,"origin":"","legend":"","description":"","filename":"Fig.2Chemicalstructurediagramoffourpesticides.jpeg","url":"https://assets-eu.researchsquare.com/files/rs-6310718/v1/1a19f53b5b32461301ace951.jpeg"},{"id":79726177,"identity":"018400d3-5019-4178-8130-620bb1cdbe1f","added_by":"auto","created_at":"2025-04-02 04:06:56","extension":"jpeg","order_by":3,"title":"","display":"","copyAsset":false,"role":"supplement","size":58402,"visible":true,"origin":"","legend":"","description":"","filename":"Fig.3Mixedstandardsolutionblanksamplesolutionandsamplespikedsolutiontotalionchromatogram.jpeg","url":"https://assets-eu.researchsquare.com/files/rs-6310718/v1/c7d8ed7055d1acec63167583.jpeg"}],"financialInterests":"No competing interests reported.","formattedTitle":"Simultaneous determination of Spirotetramat, Flonicamid, Procymidone and Cyprodinil residues in 10 dehydrated vegetables by modified QuEChERS technique and GC-MS/MS analysis","fulltext":[{"header":"1. Introduction","content":"\u003cp\u003eHistorically, the availability of fresh vegetables has been profoundly influenced by seasonal variations. To enhance storability and transportability, fresh vegetables undergo a series of processing steps, including washing and drying, to produce a shelf-stable product that preserves the original pigmentation and nutrient profile. This processed commodity, characterized by its convenience and minimal moisture content, is scientifically referred to as dehydrated vegetables(DVs)\u003csup\u003e1-5\u003c/sup\u003e. Rehydratable vegetables (RVs), defined as dehydrated plant-based foods requiring only water immersion for reconstitution, have served as a critical agricultural strategy to address supply-demand imbalances in seasonal vegetable production systems\u003csup\u003e6\u003c/sup\u003e. Their extended storage stability enabled year-round availability, effectively bridging gaps between surplus harvests and off-season shortages\u003csup\u003e7-8\u003c/sup\u003e. Recent technological advancements have expanded their utility beyond terrestrial applications, positioning them as ideal candidates for space exploration diets due to their extended shelf life, lightweight properties, and minimal resource requirements during preparation\u003csup\u003e9\u003c/sup\u003e.\u003c/p\u003e\n\u003cp\u003eTo enhance vegetable yield and ameliorate postharvest storage quality, the application of agrochemicals such as pesticides and fungicides is routinely employed for the management and mitigation of phytopathogens and pest infestations\u003csup\u003e10-11\u003c/sup\u003e.Spinetoram and flonicamid are characterized by their low toxicity, distinctive systemic translocation capabilities, and favorable selectivity for beneficial insects, making them effective agents for the management of piercing-sucking pest populations\u003csup\u003e12\u003c/sup\u003e.\u0026nbsp;Procymidone and cyprodinil, two systemic fungicides, are extensively employed in the management of gray mold disease (caused by Botrytis cinerea) and various other phytopathogenic fungi\u003csup\u003e13-14\u003c/sup\u003e.The improper application of agricultural pesticides and fungicides has resulted in concerning levels of chemical residues in food products, posing substantial risks to human health. This issue has raised significant concerns among both the public and scientific communities regarding food safety and long-term health consequences\u003csup\u003e15-16\u003c/sup\u003e.\u003c/p\u003e\n\u003cp\u003eThe QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) extraction method represents an innovative advancement in dispersive solid-phase extraction technology, distinguished by its minimal reagent requirements, expedited extraction kinetics, streamlined operational workflow, and superior analytical precision\u003csup\u003e17-18\u003c/sup\u003e. Over the past decade, this methodology has emerged as a predominant analytical approach for pesticide residue analysis in plant-derived matrices, owing to its exceptional performance characteristics and adaptability to high-throughput screening protocols\u003csup\u003e19\u003c/sup\u003e.The Selected Reaction Monitoring (SRM) mode in GC-MS/MS demonstrates enhanced selectivity and superior anti-interference capability by screening specific ion pairs of target compounds, thereby highlighting its advantages in qualitative analysis. This approach is particularly suitable for detecting samples with complex matrices due to its improved specificity.In this investigation, the QuEChERS methodology was utilized for the extraction and purification of four distinct pesticides from a variety of dehydrated vegetables. The operational parameters for GC-MS/MS were meticulously optimized to enhance analytical performance\u003csup\u003e20-21\u003c/sup\u003e. The separation and quantification of the target analytes were achieved through the implementation of the Selected Reaction Monitorin (SRM) mode in GC-MS/MS. Cis-heptachlor epoxide was employed as an internal standard to ensure the accuracy and precision of the measurements\u003csup\u003e22\u003c/sup\u003e. The developed method was successfully applied for the concurrent detection and quantification of spirotetramat, procymidone, flonicamid, and cyprodinil residues in the selected dehydrated vegetable matrices.\u003c/p\u003e"},{"header":"2. Materials and Methods","content":"\u003cp\u003e2.1 Chemicals and Reagents\u003c/p\u003e\n\u003cp\u003eAll organic solvents including methanol, acetonitrile, acetone, ethyl acetate, dichloromethane, and hexane (HPLC grade) were procured from Merck KGaA (Darmstadt, Germany). Sample preparation consumables consisting of 50 mL extract tubes containing premeasured QuEChERS salts (4 g magnesium sulfate, 1 g sodium chloride, 1 g sodium citrate sesquihydrate, and 0.5 g disodium citrate dehydrate; 25 tubes per package) and 15 mL purification tubes packed with 900 mg magnesium sulfate and 150 mg primary secondary amine (PSA) sorbent (25 units per box) were obtained from GEMSS Science and Technology Co., Ltd. (Dalian, China)\u003csup\u003e17\u003c/sup\u003e. Ultrapure water (18.2 M\u0026Omega;\u0026middot;cm resistivity) was produced using a Milli-Q Integral water purification system (MilliporeSigma, Molsheim, France).\u003c/p\u003e\n\u003cp\u003e2.2 Standards\u003c/p\u003e\n\u003cp\u003eIndividual certified pesticide reference standards (Flonicamid, Cyprodinil, Procymidone, and Spirotetramat) at 1000 mg L⁻\u0026sup1; concentration were obtained from the Chinese Academy of Metrological Science. Primary stock solutions were maintained in sealed amber glass ampoules under dark storage conditions at -20\u0026deg;C.A multi-component working standard mixture containing 10 mg L⁻\u0026sup1; of each analyte was prepared in HPLC-grade acetone. This intermediate standard solution was aliquoted into amber glass vials with PTFE-lined caps and stored at 4\u0026deg;C for no more than three months to maintain stability. The working solution served as the primary source for calibration standards through serial dilution with dichloromethane-acetone solvent system (2:8, v/v).The calibration standards spanning concentrations of 5, 10, 20, 50, 100, 200, and 250\u0026mu;g/L were prepared through serial dilution of a stock solution in a dichloromethane-acetone solvent system (2:8, v/v). Appropriate aliquots of a multi-component standard mixture were sequentially diluted with the mixed organic solvent to achieve the required concentration levels for calibration curve construction.Certified cis-heptachlor epoxide reference standards (1,000 mg/L in ethyl acetate) were purchased from Alta Technology (Tianjin, China) as internal standards. The certified reference materials (CRMs) were supplied in sealed glass ampules and stored under light-protected conditions. Working solutions (100 \u0026mu;g/L) were prepared by diluting stock solutions with ethyl acetate and utilized for both calibration curves (5\u0026ndash;250 \u0026mu;g/L) and sample quantification. All solutions were aliquoted into amber glass vials and stored at -20\u0026deg;C until analysis to minimize degradation\u003csup\u003e23\u003c/sup\u003e.\u003c/p\u003e\n\u003cp\u003e2.3 Instruments\u003c/p\u003e\n\u003cp\u003eThe experiment was performed ina Trace 1600 GC (Thermo Fisher) coupled to an TSQ 9610 Triple Quadrupole Mass Spectrometer(Thermo Fisher) and a Triplus RSH autosampler(Thermo Fisher) . The machine had a split/splitless injector with an electronic pressure control system, the injector Temperature maintained at 280℃. A 1\u0026mu;L target solution was introduced into the system through an injector. The injection was performed in pulsed splitless mode with a pulse pressure of 200kPa and a duration of 0.75min. A TG-5SILMS(30m\u0026times;250\u0026mu;m,0.25\u0026mu;m) (Thermo Fisher)was used to separate the analytes in the sample, including filter sample solutions, blank sample solutions, and mixed standard solutions. the carrier gas was high purity helium at a flow rate of 1.20mL/min. The GC oven temperature program started at 50℃ for 1.5min, followed by a gradient increase of 25℃/min until 90℃and held for 1.5 min. It was then increased to 180 ℃at a rate of 25 ℃/min, 180 ℃ to 280 C at 8℃/min and finally raised to 300 ℃ at 10℃/min and hold 5min.The ion sources were operated at an electron energy of 70eV. the ion source and the transfer line temperatures were maintained at 280℃, and Selected Reaction Monitorin (SRM) was applied\u003csup\u003e24\u003c/sup\u003e. Total time of analysis:\u0026nbsp;20.43\u0026nbsp;min.\u003c/p\u003e\n\u003cp\u003e2.4 Collection and Preservation of Samples\u003c/p\u003e\n\u003cp\u003eFresh vegetable specimens for pesticide analysis were procured from commercial retail outlets (supermarkets and convenience stores) in Yinchuan, Ningxia Hui Autonomous Region. Parallel blank control samples were obtained from local subsistence farmers who maintained pesticide-free cultivation practices, with absence of pesticide residues confirmed through preliminary screening. All specimens underwent immediate cryopreservation at-20\u0026deg;C within 2 hours of collection\u003csup\u003e.\u003c/sup\u003e Following a 40-hour lyophilization process using a CTFD-100S vacuum freeze-dryer (Yonghe Chuangxin Electronic Technology Co., Ltd., Qingdao, China), the samples were homogenized to fine powder (particle size \u0026lt;100 \u0026mu;m)\u003csup\u003e25\u003c/sup\u003e. Processed samples were aliquoted into sterile 250 mL polypropylene containers (Corning Inc.) and maintained at -20\u0026deg;C in temperature-controlled laboratory refrigeration units (Thermo Scientific TSX Series) until analysis.\u003c/p\u003e\n\u003cp\u003e2.5 Extraction and cleanup with QuEChERS method\u003c/p\u003e\n\u003cp\u003eDehydrated vegetable samples were prepared using a modified QuEChERS method based on AOAC Official Method 2007.01\u003csup\u003e18\u003c/sup\u003e.\u0026nbsp;Specifically, 0.50 g aliquots of homogenized samples were accurately weighed into 50 mL olyproppylene centrifuge tubes. The extraction process commenced with the addition of 4.5 mL ultrapure water (18.2 M\u0026Omega;\u0026middot;cm at 25\u0026deg;C)\u003csup\u003e26\u003c/sup\u003e, followed by vigorous vortex mixing (HMG-WX vortex mixer, IKA, Germany) for 1 min. The hydrated samples were then equilibrated at room temperature (25 \u0026plusmn; 2\u0026deg;C) for 15 min. Subsequently, 10.0 mL acetonitrile (HPLC grade) containing ceramic homogenizers (1 cm diameter) was added to each tube, followed by another 1 min vortex mixing step to ensure complete sample dispersion. The homogenized mixtures were immediately transferred to a -20\u0026deg;C freezer (\u0026plusmn;1\u0026deg;C) for 30 min to facilitate phase separation and protein precipitation. Following the addition of a dehydrated salt packet (anhydrous sodium sulfate, \u0026gt;99% purity), the sample tubes were immediately subjected to vigorous manual shaking for 60 s. Primary phase separation was achieved through centrifugation at 4200 rpm (rcf 2500 \u0026times; g) for 5 min using a benchtop centrifuge (Eppendorf 5804, Hamburg, Germany). A precisely measured 6.00 mL aliquot of the resulting supernatant was carefully transferred to a 15 mL purification tube (PTFE-lined cap). The secondary extraction phase involved vortex mixing (VM-300, maximal intensity) for 60 s followed by centrifugation at 4500 rpm (rcf 3000 \u0026times; g) for 5 min. Subsequently, 5.00 mL (5000 \u0026mu;L) of the purified upper organic layer was quantitatively transferred to a 10 mL graduated glass test tube with PTFE-sealed cap. Solvent evaporation was conducted using a nitrogen evaporator (N-EVAP 116, Organomation Associates Inc., Berlin, MA, USA) maintained at 45\u0026plusmn;1\u0026deg;C with continuous N₂ flow (15 psi) until complete removal of acetonitrile was visually confirmed (no meniscus observed). The dried residue was then reconstituted in 1.00 mL of a freshly prepared solvent mixture containing acetone and dichloromethane (2:8 v/v, HPLC grade) with 30 s vortex-assisted dissolution. Following three consecutive 1-minute vortexing cycles, the homogenized mixture was transferred to a 2.0 mL screw-cap glass vial. Prior to GC-MS/MS analysis, the sample was purified through a 0.22 \u0026mu;m needle-type membrane filter (PTFE, 25 mm diameter) using sterile syringe filtration techniques.\u003c/p\u003e\n\u003cp\u003eFor fresh vegetable samples, aliquots (5.0 g) were accurately weighed into 50 mL centrifuge tubes, followed by immediate addition of 10.0 mL acetonitrile to each tube. For matrix-matched blank samples, appropriate aliquots of the working multistandard solution were spiked into the matrix followed by a 30-minute equilibrium period at ambient temperature (25\u0026plusmn;2\u0026deg;C) to facilitate pesticide migration and matrix interaction prior to subsequent extraction procedures\u003csup\u003e27\u003c/sup\u003e.\u003c/p\u003e"},{"header":"3. Result and discussion","content":"\u003cp\u003e3.1 Optimization of Chromatography-MS Analytical Parameters\u003c/p\u003e\n\u003cp\u003e\u0026nbsp; The retention times of target compounds were determined through full-scan analyses using a 1.0 mg/L multi-component standard mixture. Analyses were performed in electron ionization(EI) mode with a mass-to-charge (m/z) range of 50-550. Optimal precursor/product ion pairs and collision energies were automatically optimized using an intelligent SRM system(Thermo Fisher) with high-purity helium (99.999%) as collision gas. The mass spectrometer was operated in selective reaction monitoring (SRM) mode for routine analysis. Both quantification and qualification of analytes were achieved by monitoring three characteristic SRM transitions per compound, with peak area ratios used for confirmation. All analytical results are summarized in Table 1.\u003c/p\u003e\n\u003cp\u003eTab 1\u0026nbsp;Retention Time, MS Quantitation and Confirming Peak of 5 compounds\u003c/p\u003e\n\u003cdiv align=\"\"\u003e\n \u003ctable border=\"1\" cellspacing=\"0\" cellpadding=\"0\" width=\"614\"\u003e\n \u003ctbody\u003e\n \u003ctr\u003e\n \u003ctd valign=\"top\" style=\"width: 21.7886%;\"\u003e\n \u003cp\u003e\u0026nbsp; \u0026nbsp; \u0026nbsp; Component name\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd valign=\"top\" style=\"width: 18.374%;\"\u003e\n \u003cp\u003eRetention Time(min)\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd valign=\"top\" style=\"width: 24.5528%;\"\u003e\n \u003cp\u003eMS Quantitation Peak(eV) \u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd valign=\"top\" style=\"width: 35.2846%;\"\u003e\n \u003cp\u003e\u0026nbsp;MS Confirming Peak (eV )\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd valign=\"top\" style=\"width: 21.7886%;\"\u003e\n \u003cp\u003e\u0026nbsp;Flonicamid\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd valign=\"top\" style=\"width: 18.374%;\"\u003e\n \u003cp\u003e6.48\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd valign=\"top\" style=\"width: 24.5528%;\"\u003e\n \u003cp\u003e146\u0026gt;126(8eV)\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd valign=\"top\" style=\"width: 35.2846%;\"\u003e\n \u003cp\u003e174\u0026gt;69(36eV);175.1\u0026gt;147(8eV)\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd valign=\"top\" style=\"width: 21.7886%;\"\u003e\n \u003cp\u003eCyprodinil\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd valign=\"top\" style=\"width: 18.374%;\"\u003e\n \u003cp\u003e11.63\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd valign=\"top\" style=\"width: 24.5528%;\"\u003e\n \u003cp\u003e224.1\u0026gt;208.1(16eV)\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd valign=\"top\" style=\"width: 35.2846%;\"\u003e\n \u003cp\u003e224.1\u0026gt;207.1(36eV);224.1\u0026gt;222.1(18eV)\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd valign=\"top\" style=\"width: 21.7886%;\"\u003e\n \u003cp\u003ecis-Heptachlor Epoxide\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd valign=\"top\" style=\"width: 18.374%;\"\u003e\n \u003cp\u003e12.00\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd valign=\"top\" style=\"width: 24.5528%;\"\u003e\n \u003cp\u003e352.8\u0026gt;262.9(16eV)\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd valign=\"top\" style=\"width: 35.2846%;\"\u003e\n \u003cp\u003e262.9\u0026gt;192(30eV);354.7\u0026gt;264.9(12eV))\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd valign=\"top\" style=\"width: 21.7886%;\"\u003e\n \u003cp\u003eProcymidone\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd valign=\"top\" style=\"width: 18.374%;\"\u003e\n \u003cp\u003e12.34\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd valign=\"top\" style=\"width: 24.5528%;\"\u003e\n \u003cp\u003e283\u0026gt;96.1(8eV)\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd valign=\"top\" style=\"width: 35.2846%;\"\u003e\n \u003cp\u003e285\u0026gt;96.1(8eV);283\u0026gt;67.1(26eV);\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd valign=\"top\" style=\"width: 21.7886%;\"\u003e\n \u003cp\u003eSpirotetramat\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd valign=\"top\" style=\"width: 18.374%;\"\u003e\n \u003cp\u003e17.24\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd valign=\"top\" style=\"width: 24.5528%;\"\u003e\n \u003cp\u003e270.1\u0026gt;216.1(14eV)\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd valign=\"top\" style=\"width: 35.2846%;\"\u003e\n \u003cp\u003e268.1\u0026gt;214.1(8eV); 286.1\u0026gt;216.1(12eV)\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003c/tbody\u003e\n \u003c/table\u003e\n\u003c/div\u003e\n\u003cp\u003e3.2 Optimal Constant-Volume Solvent Screening\u003c/p\u003e\n\u003cp\u003e\u0026nbsp; Standard solutions (100 \u0026mu;g/L) were prepared using methanol, acetonitrile, acetone, ethyl acetate, dichloromethane, and n-hexane as individual solvents. The response values of target analytes were subsequently determined using [instrument name/model]. As illustrated in Fig. 1, the acetone- dichloromethane mixed solvent system (2:8, v/v) demonstrated optimal response characteristics. Therefore, this binary solvent mixture was selected as the working solvent for both sample preparation and calibration curve construction throughout the experimental protocol.\u003c/p\u003e\n\u003cp\u003e3.3 Calibration Curve Properties and Statistical Analysis\u003c/p\u003e\n\u003cp\u003eCalibration curves were established for Flonicamid, Cyprodinil, Procymidone, and Spirotetramat across a concentration range of 5-250 ng/mL, demonstrating excellent linearity with correlation coefficients (r) \u0026gt; 0.9994 (Table 2). Method sensitivity was evaluated through limits of detection (LOD) and quantification (LOQ), determined as signal-to-noise ratios (S/N) of 3:1 and 10:1, respectively, based on 0.5 g sample aliquots. The calculated LOD and LOQ values for all analytes were \u0026lt;0.00085 mg/kg and \u0026lt;0.0016 mg/kg, respectively, meeting EU Commission Regulation 2021/808 requirements for pesticide residue analysis\u003csup\u003e28.\u003c/sup\u003e\u003c/p\u003e\n\u003cp\u003eTab.2 \u0026nbsp;Calibration Curve Properties and statistical analysis of \u003cem\u003eFlonicamid\u003c/em\u003e, \u003cem\u003eCyprodinil, Procymidone\u003c/em\u003e and \u003cem\u003eSpirotetramat\u003c/em\u003e\u003c/p\u003e\n\u003ctable border=\"1\" cellspacing=\"0\" cellpadding=\"0\" width=\"584\"\u003e\n \u003ctbody\u003e\n \u003ctr\u003e\n \u003ctd valign=\"top\" style=\"width: 15.0685%;\"\u003e\n \u003cp\u003ePesticides\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd valign=\"top\" style=\"width: 21.9178%;\"\u003e\n \u003cp\u003eLinear regression equation\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd valign=\"top\" style=\"width: 20.2055%;\"\u003e\n \u003cp\u003eCorrelation coefficient (r)\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd valign=\"top\" style=\"width: 19.1781%;\"\u003e\n \u003cp\u003eDetection limit (mg/kg)\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd valign=\"top\" style=\"width: 23.6301%;\"\u003e\n \u003cp\u003eQuantitative limit (mg/kg)\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd valign=\"top\" style=\"width: 15.0685%;\"\u003e\n \u003cp\u003eFlonicamid\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd valign=\"top\" style=\"width: 21.9178%;\"\u003e\n \u003cp\u003ey=3559.526x-8.009\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd valign=\"top\" style=\"width: 20.2055%;\"\u003e\n \u003cp\u003e0.9997\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd valign=\"top\" style=\"width: 19.1781%;\"\u003e\n \u003cp\u003e0.00025\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd valign=\"top\" style=\"width: 23.6301%;\"\u003e\n \u003cp\u003e0.00085\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd valign=\"top\" style=\"width: 15.0685%;\"\u003e\n \u003cp\u003eCyprodinil\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd valign=\"top\" style=\"width: 21.9178%;\"\u003e\n \u003cp\u003ey=6980.959x-3.328\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd valign=\"top\" style=\"width: 20.2055%;\"\u003e\n \u003cp\u003e0.9997\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd valign=\"top\" style=\"width: 19.1781%;\"\u003e\n \u003cp\u003e0.00023\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd valign=\"top\" style=\"width: 23.6301%;\"\u003e\n \u003cp\u003e0.00062\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd valign=\"top\" style=\"width: 15.0685%;\"\u003e\n \u003cp\u003eProcymidone\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd valign=\"top\" style=\"width: 21.9178%;\"\u003e\n \u003cp\u003ey=2439.980x-1.656\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd valign=\"top\" style=\"width: 20.2055%;\"\u003e\n \u003cp\u003e0.9994\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd valign=\"top\" style=\"width: 19.1781%;\"\u003e\n \u003cp\u003e0.00085\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd valign=\"top\" style=\"width: 23.6301%;\"\u003e\n \u003cp\u003e0.0016\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd valign=\"top\" style=\"width: 15.0685%;\"\u003e\n \u003cp\u003eSpirotetramat\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd valign=\"top\" style=\"width: 21.9178%;\"\u003e\n \u003cp\u003ey=1233.681x+3.393\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd valign=\"top\" style=\"width: 20.2055%;\"\u003e\n \u003cp\u003e0.9995\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd valign=\"top\" style=\"width: 19.1781%;\"\u003e\n \u003cp\u003e0.00020\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd valign=\"top\" style=\"width: 23.6301%;\"\u003e\n \u003cp\u003e0.00067\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003c/tbody\u003e\n\u003c/table\u003e\n\u003cp\u003e3.4\u0026nbsp;Chronotropic Soaking Modulates Standard Addition Recovery\u003c/p\u003e\n\u003cp\u003eThe chromatographic and mass spectrometric responses of the internal standard in powdered samples exhibited time-dependent recovery patterns during immersion (1\u0026ndash;30 min). Spiked recoveries increased significantly with immersion time from 1 to 15 min , but no statistically meaningful improvement was observed beyond 15 min (Fig. 2). This kinetic profile indicates that equilibrium was achieved within 15 min, justifying the selection of 15-min immersion in deionized water for subsequent experiments\u003c/p\u003e\n\u003cp\u003e3.5 Spiked Recovery and Precision\u003c/p\u003e\n\u003cp\u003eThe method validation demonstrated satisfactory analytical performance for vegetable matrix analysis. Ten blank vegetable powder samples were individually spiked with standard solutions at 0.05, 0.25, and 0.5 mg/kg, followed by extraction, purification, and GC-MS analysis using the established protocol. As shown in Table 3, recoveries of target components ranged from 78.1% to 113.2%, with relative standard deviations (RSDs) \u0026lt;5.00% across six replicate measurements. These values align with the recommended acceptance criteria for recovery (70\u0026ndash;120%) and precision (RSD\u0026nbsp;\u0026le;15%) in complex food matrices\u003csup\u003e29\u003c/sup\u003e, confirming the reliability of the method for quantitative analysis.\u003c/p\u003e\n\u003cp\u003eTab. 3 Recovery and RSD of Four Pesticides in Dehydrated Vegetables\u003c/p\u003e\n\u003ctable border=\"0\" cellspacing=\"0\" cellpadding=\"0\" align=\"\" width=\"556\"\u003e\n \u003ctbody\u003e\n \u003ctr\u003e\n \u003ctd rowspan=\"3\" style=\"width: 62px;\"\u003e\n \u003cp\u003eDehydrated Vegetables\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd rowspan=\"3\" style=\"width: 74px;\"\u003e\n \u003cp\u003ePesticides\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd colspan=\"6\" style=\"width: 419px;\"\u003e\n \u003cp\u003erecovery levels\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd colspan=\"2\" style=\"width: 140px;\"\u003e\n \u003cp\u003e0.05mg/kg\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd colspan=\"2\" style=\"width: 138px;\"\u003e\n \u003cp\u003e0.25mg/kg\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd colspan=\"2\" style=\"width: 141px;\"\u003e\n \u003cp\u003e0.50mg/kg\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd style=\"width: 87px;\"\u003e\n \u003cp\u003eRecovery\u0026nbsp;rate\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 53px;\"\u003e\n \u003cp\u003eRSD\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 80px;\"\u003e\n \u003cp\u003eRecovery\u0026nbsp;rate\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 58px;\"\u003e\n \u003cp\u003eRSD\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 75px;\"\u003e\n \u003cp\u003eRecovery\u0026nbsp;rate\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 66px;\"\u003e\n \u003cp\u003eRSD\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd rowspan=\"4\" style=\"width: 62px;\"\u003e\n \u003cp\u003ecucumbers\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd valign=\"top\" style=\"width: 74px;\"\u003e\n \u003cp\u003eFlonicamid\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 87px;\"\u003e\n \u003cp\u003e84.4-95.4\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 53px;\"\u003e\n \u003cp\u003e4.42\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 80px;\"\u003e\n \u003cp\u003e98.2-112.2\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 58px;\"\u003e\n \u003cp\u003e4.85\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 75px;\"\u003e\n \u003cp\u003e95.4-107.4\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 66px;\"\u003e\n \u003cp\u003e4.43\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd valign=\"top\" style=\"width: 74px;\"\u003e\n \u003cp\u003eCyprodinil\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 87px;\"\u003e\n \u003cp\u003e96.0-105.5\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 53px;\"\u003e\n \u003cp\u003e3.71\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 80px;\"\u003e\n \u003cp\u003e103.7-112.2\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 58px;\"\u003e\n \u003cp\u003e3.17\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 75px;\"\u003e\n \u003cp\u003e94.1-105.4\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 66px;\"\u003e\n \u003cp\u003e4.42\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd valign=\"top\" style=\"width: 74px;\"\u003e\n \u003cp\u003eProcymidone\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 87px;\"\u003e\n \u003cp\u003e86.3-92.4\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 53px;\"\u003e\n \u003cp\u003e2.88\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 80px;\"\u003e\n \u003cp\u003e92.2-100.2\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 58px;\"\u003e\n \u003cp\u003e3.22\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 75px;\"\u003e\n \u003cp\u003e92.4-104.3\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 66px;\"\u003e\n \u003cp\u003e4.01\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd valign=\"top\" style=\"width: 74px;\"\u003e\n \u003cp\u003eSpirotetramat\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 87px;\"\u003e\n \u003cp\u003e79.9-87.4\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 53px;\"\u003e\n \u003cp\u003e4,21\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 80px;\"\u003e\n \u003cp\u003e90.4-98.2\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 58px;\"\u003e\n \u003cp\u003e3.15\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 75px;\"\u003e\n \u003cp\u003e95.9-100.5\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 66px;\"\u003e\n \u003cp\u003e2.39\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd rowspan=\"4\" style=\"width: 62px;\"\u003e\n \u003cp\u003ecumin\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd valign=\"top\" style=\"width: 74px;\"\u003e\n \u003cp\u003eFlonicamid\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 87px;\"\u003e\n \u003cp\u003e90.3-98.2\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 53px;\"\u003e\n \u003cp\u003e3.01\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 80px;\"\u003e\n \u003cp\u003e105.9-112.2\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 58px;\"\u003e\n \u003cp\u003e2.09\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 75px;\"\u003e\n \u003cp\u003e97.4-107.2\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 66px;\"\u003e\n \u003cp\u003e3.80\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd valign=\"top\" style=\"width: 74px;\"\u003e\n \u003cp\u003eCyprodinil\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 87px;\"\u003e\n \u003cp\u003e96.5-106.5\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 53px;\"\u003e\n \u003cp\u003e3.52\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 80px;\"\u003e\n \u003cp\u003e102.2-113.2\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 58px;\"\u003e\n \u003cp\u003e3.92\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 75px;\"\u003e\n \u003cp\u003e93.4-100.2\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 66px;\"\u003e\n \u003cp\u003e2.96\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd valign=\"top\" style=\"width: 74px;\"\u003e\n \u003cp\u003eProcymidone\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 87px;\"\u003e\n \u003cp\u003e90.9-96.6\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 53px;\"\u003e\n \u003cp\u003e2.28\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 80px;\"\u003e\n \u003cp\u003e92.1-97.7\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 58px;\"\u003e\n \u003cp\u003e2.12\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 75px;\"\u003e\n \u003cp\u003e91.2-101.1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 66px;\"\u003e\n \u003cp\u003e3.63\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd valign=\"top\" style=\"width: 74px;\"\u003e\n \u003cp\u003eSpirotetramat\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 87px;\"\u003e\n \u003cp\u003e87.2-92.2\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 53px;\"\u003e\n \u003cp\u003e2.14\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 80px;\"\u003e\n \u003cp\u003e100.4-109.4\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 58px;\"\u003e\n \u003cp\u003e3.10\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 75px;\"\u003e\n \u003cp\u003e92.0-97.9\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 66px;\"\u003e\n \u003cp\u003e3.19\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd rowspan=\"4\" style=\"width: 62px;\"\u003e\n \u003cp\u003ecarrot\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd valign=\"top\" style=\"width: 74px;\"\u003e\n \u003cp\u003eFlonicamid\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 87px;\"\u003e\n \u003cp\u003e89.4-96.7\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 53px;\"\u003e\n \u003cp\u003e2.66\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 80px;\"\u003e\n \u003cp\u003e93.1-102.1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 58px;\"\u003e\n \u003cp\u003e3.31\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 75px;\"\u003e\n \u003cp\u003e90.2-101.4\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 66px;\"\u003e\n \u003cp\u003e4.21\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd valign=\"top\" style=\"width: 74px;\"\u003e\n \u003cp\u003eCyprodinil\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 87px;\"\u003e\n \u003cp\u003e78.4-89.9\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 53px;\"\u003e\n \u003cp\u003e4.78\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 80px;\"\u003e\n \u003cp\u003e89.4-95.5\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 58px;\"\u003e\n \u003cp\u003e2.24\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 75px;\"\u003e\n \u003cp\u003e89.1-97.4\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 66px;\"\u003e\n \u003cp\u003e3.64\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd valign=\"top\" style=\"width: 74px;\"\u003e\n \u003cp\u003eProcymidone\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 87px;\"\u003e\n \u003cp\u003e103.2-113.2\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 53px;\"\u003e\n \u003cp\u003e3.32\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 80px;\"\u003e\n \u003cp\u003e101.8-114.2\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 58px;\"\u003e\n \u003cp\u003e4.72\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 75px;\"\u003e\n \u003cp\u003e97.4-106.4\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 66px;\"\u003e\n \u003cp\u003e3.15\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd valign=\"top\" style=\"width: 74px;\"\u003e\n \u003cp\u003eSpirotetramat\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 87px;\"\u003e\n \u003cp\u003e91.1-98.7\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 53px;\"\u003e\n \u003cp\u003e3.27\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 80px;\"\u003e\n \u003cp\u003e91.4-99.7\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 58px;\"\u003e\n \u003cp\u003e3.02\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 75px;\"\u003e\n \u003cp\u003e99.7-112.3\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 66px;\"\u003e\n \u003cp\u003e4.10\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd rowspan=\"4\" style=\"width: 62px;\"\u003e\n \u003cp\u003elycopene\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd valign=\"top\" style=\"width: 74px;\"\u003e\n \u003cp\u003eFlonicamid\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 87px;\"\u003e\n \u003cp\u003e86.6-95.2\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 53px;\"\u003e\n \u003cp\u003e3.45\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 80px;\"\u003e\n \u003cp\u003e89.9-95.1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 58px;\"\u003e\n \u003cp\u003e2.40\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 75px;\"\u003e\n \u003cp\u003e92.4-97.7\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 66px;\"\u003e\n \u003cp\u003e1.98\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd valign=\"top\" style=\"width: 74px;\"\u003e\n \u003cp\u003eCyprodinil\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 87px;\"\u003e\n \u003cp\u003e82.9-87.3\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 53px;\"\u003e\n \u003cp\u003e3.06\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 80px;\"\u003e\n \u003cp\u003e89.2-97.2\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 58px;\"\u003e\n \u003cp\u003e3.02\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 75px;\"\u003e\n \u003cp\u003e94.9-104.4\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 66px;\"\u003e\n \u003cp\u003e3.55\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd valign=\"top\" style=\"width: 74px;\"\u003e\n \u003cp\u003eProcymidone\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 87px;\"\u003e\n \u003cp\u003e83.6-93.0\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 53px;\"\u003e\n \u003cp\u003e4.79\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 80px;\"\u003e\n \u003cp\u003e86.7-95.5\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 58px;\"\u003e\n \u003cp\u003e3.93\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 75px;\"\u003e\n \u003cp\u003e93.2-103.9\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 66px;\"\u003e\n \u003cp\u003e4.09\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd valign=\"top\" style=\"width: 74px;\"\u003e\n \u003cp\u003eSpirotetramat\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 87px;\"\u003e\n \u003cp\u003e85.3-95.3\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 53px;\"\u003e\n \u003cp\u003e4.50\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 80px;\"\u003e\n \u003cp\u003e97.7-110.0\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 58px;\"\u003e\n \u003cp\u003e4.71\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 75px;\"\u003e\n \u003cp\u003e99.4-110.4\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 66px;\"\u003e\n \u003cp\u003e4.66\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd rowspan=\"4\" style=\"width: 62px;\"\u003e\n \u003cp\u003eeggplant\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd valign=\"top\" style=\"width: 74px;\"\u003e\n \u003cp\u003eFlonicamid\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 87px;\"\u003e\n \u003cp\u003e78.1-87.3\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 53px;\"\u003e\n \u003cp\u003e4.58\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 80px;\"\u003e\n \u003cp\u003e88.4-94.2\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 58px;\"\u003e\n \u003cp\u003e2.35\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 75px;\"\u003e\n \u003cp\u003e90.4-98.5\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 66px;\"\u003e\n \u003cp\u003e2.82\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd valign=\"top\" style=\"width: 74px;\"\u003e\n \u003cp\u003eCyprodinil\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 87px;\"\u003e\n \u003cp\u003e86.0-96.1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 53px;\"\u003e\n \u003cp\u003e3.74\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 80px;\"\u003e\n \u003cp\u003e102.2-112.1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 58px;\"\u003e\n \u003cp\u003e3.53\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 75px;\"\u003e\n \u003cp\u003e98.4-104.4\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 66px;\"\u003e\n \u003cp\u003e2.20\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd valign=\"top\" style=\"width: 74px;\"\u003e\n \u003cp\u003eProcymidone\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 87px;\"\u003e\n \u003cp\u003e79.4-89.1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 53px;\"\u003e\n \u003cp\u003e4.51\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 80px;\"\u003e\n \u003cp\u003e82.1-90.0\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 58px;\"\u003e\n \u003cp\u003e3.26\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 75px;\"\u003e\n \u003cp\u003e89.9-97.7\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 66px;\"\u003e\n \u003cp\u003e3.12\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd valign=\"top\" style=\"width: 74px;\"\u003e\n \u003cp\u003eSpirotetramat\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 87px;\"\u003e\n \u003cp\u003e87.1-96.9\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 53px;\"\u003e\n \u003cp\u003e4.29\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 80px;\"\u003e\n \u003cp\u003e88.4-94.4\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 58px;\"\u003e\n \u003cp\u003e2.69\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 75px;\"\u003e\n \u003cp\u003e93.9-104.2\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 66px;\"\u003e\n \u003cp\u003e3.74\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd rowspan=\"4\" style=\"width: 62px;\"\u003e\n \u003cp\u003ecabbage\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd valign=\"top\" style=\"width: 74px;\"\u003e\n \u003cp\u003eFlonicamid\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 87px;\"\u003e\n \u003cp\u003e79.4-85.1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 53px;\"\u003e\n \u003cp\u003e3.15\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 80px;\"\u003e\n \u003cp\u003e90.4-102.1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 58px;\"\u003e\n \u003cp\u003e3.77\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 75px;\"\u003e\n \u003cp\u003e93.3-97.5\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 66px;\"\u003e\n \u003cp\u003e2.66\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd valign=\"top\" style=\"width: 74px;\"\u003e\n \u003cp\u003eCyprodinil\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 87px;\"\u003e\n \u003cp\u003e85.1-93.4\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 53px;\"\u003e\n \u003cp\u003e4.11\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 80px;\"\u003e\n \u003cp\u003e92.1-96.8\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 58px;\"\u003e\n \u003cp\u003e2.13\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 75px;\"\u003e\n \u003cp\u003e93.4-100.8\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 66px;\"\u003e\n \u003cp\u003e2.03\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd valign=\"top\" style=\"width: 74px;\"\u003e\n \u003cp\u003eProcymidone\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 87px;\"\u003e\n \u003cp\u003e89.6-99.2\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 53px;\"\u003e\n \u003cp\u003e4.63\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 80px;\"\u003e\n \u003cp\u003e90.2-101.0\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 58px;\"\u003e\n \u003cp\u003e3.38\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 75px;\"\u003e\n \u003cp\u003e89.2-96.9\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 66px;\"\u003e\n \u003cp\u003e1.99\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd valign=\"top\" style=\"width: 74px;\"\u003e\n \u003cp\u003eSpirotetramat\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 87px;\"\u003e\n \u003cp\u003e79.6-88.8\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 53px;\"\u003e\n \u003cp\u003e4.34\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 80px;\"\u003e\n \u003cp\u003e83.7-90.2\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 58px;\"\u003e\n \u003cp\u003e3.00\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 75px;\"\u003e\n \u003cp\u003e88.2-94.7\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 66px;\"\u003e\n \u003cp\u003e2.13\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd rowspan=\"4\" style=\"width: 62px;\"\u003e\n \u003cp\u003eLeek\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd valign=\"top\" style=\"width: 74px;\"\u003e\n \u003cp\u003eFlonicamid\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 87px;\"\u003e\n \u003cp\u003e83.3-91.3\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 53px;\"\u003e\n \u003cp\u003e4.04\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 80px;\"\u003e\n \u003cp\u003e89.7-96.2\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 58px;\"\u003e\n \u003cp\u003e3.42\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 75px;\"\u003e\n \u003cp\u003e90.4-104.6\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 66px;\"\u003e\n \u003cp\u003e3.35\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd valign=\"top\" style=\"width: 74px;\"\u003e\n \u003cp\u003eCyprodinil\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 87px;\"\u003e\n \u003cp\u003e88.2-94.1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 53px;\"\u003e\n \u003cp\u003e2.70\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 80px;\"\u003e\n \u003cp\u003e87.2-97.3\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 58px;\"\u003e\n \u003cp\u003e2.85\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 75px;\"\u003e\n \u003cp\u003e87.2-95.8\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 66px;\"\u003e\n \u003cp\u003e3.27\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd valign=\"top\" style=\"width: 74px;\"\u003e\n \u003cp\u003eProcymidone\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 87px;\"\u003e\n \u003cp\u003e93.6-105.2\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 53px;\"\u003e\n \u003cp\u003e4.87\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 80px;\"\u003e\n \u003cp\u003e98.4-110.1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 58px;\"\u003e\n \u003cp\u003e4.39\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 75px;\"\u003e\n \u003cp\u003e95.5-103.4\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 66px;\"\u003e\n \u003cp\u003e4.08\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd valign=\"top\" style=\"width: 74px;\"\u003e\n \u003cp\u003eSpirotetramat\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 87px;\"\u003e\n \u003cp\u003e82.4-95.4\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 53px;\"\u003e\n \u003cp\u003e4.92\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 80px;\"\u003e\n \u003cp\u003e90.1-100.5\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 58px;\"\u003e\n \u003cp\u003e3.53\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 75px;\"\u003e\n \u003cp\u003e92.8-105.3\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 66px;\"\u003e\n \u003cp\u003e4.00\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd rowspan=\"4\" style=\"width: 62px;\"\u003e\n \u003cp\u003ecelery\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd valign=\"top\" style=\"width: 74px;\"\u003e\n \u003cp\u003eFlonicamid\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 87px;\"\u003e\n \u003cp\u003e94.4-102.2\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 53px;\"\u003e\n \u003cp\u003e4.55\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 80px;\"\u003e\n \u003cp\u003e98.2-110.3\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 58px;\"\u003e\n \u003cp\u003e4.27\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 75px;\"\u003e\n \u003cp\u003e94.6-109.4\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 66px;\"\u003e\n \u003cp\u003e3.76\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd valign=\"top\" style=\"width: 74px;\"\u003e\n \u003cp\u003eCyprodinil\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 87px;\"\u003e\n \u003cp\u003e78.3-86.2\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 53px;\"\u003e\n \u003cp\u003e4.09\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 80px;\"\u003e\n \u003cp\u003e82.4-95.2\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 58px;\"\u003e\n \u003cp\u003e4.87\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 75px;\"\u003e\n \u003cp\u003e89.5-97.5\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 66px;\"\u003e\n \u003cp\u003e3.00\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd valign=\"top\" style=\"width: 74px;\"\u003e\n \u003cp\u003eProcymidone\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 87px;\"\u003e\n \u003cp\u003e92.7-106.7\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 53px;\"\u003e\n \u003cp\u003e3.86\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 80px;\"\u003e\n \u003cp\u003e93.5-98.2\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 58px;\"\u003e\n \u003cp\u003e3.26\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 75px;\"\u003e\n \u003cp\u003e93.5-99.0\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 66px;\"\u003e\n \u003cp\u003e2.10\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd valign=\"top\" style=\"width: 74px;\"\u003e\n \u003cp\u003eSpirotetramat\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 87px;\"\u003e\n \u003cp\u003e81.0-90.8\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 53px;\"\u003e\n \u003cp\u003e4.46\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 80px;\"\u003e\n \u003cp\u003e90.7-99.2\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 58px;\"\u003e\n \u003cp\u003e3.48\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 75px;\"\u003e\n \u003cp\u003e92.7-102.4\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 66px;\"\u003e\n \u003cp\u003e2.35\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd rowspan=\"4\" style=\"width: 62px;\"\u003e\n \u003cp\u003eChinese yam\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd valign=\"top\" style=\"width: 74px;\"\u003e\n \u003cp\u003eFlonicamid\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 87px;\"\u003e\n \u003cp\u003e87.5-96.5\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 53px;\"\u003e\n \u003cp\u003e3.56\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 80px;\"\u003e\n \u003cp\u003e89.0-98.3\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 58px;\"\u003e\n \u003cp\u003e3.78\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 75px;\"\u003e\n \u003cp\u003e94.8-105.5\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 66px;\"\u003e\n \u003cp\u003e3.28\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd valign=\"top\" style=\"width: 74px;\"\u003e\n \u003cp\u003eCyprodinil\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 87px;\"\u003e\n \u003cp\u003e92.3-103.6\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 53px;\"\u003e\n \u003cp\u003e4.06\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 80px;\"\u003e\n \u003cp\u003e96.4-107.5\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 58px;\"\u003e\n \u003cp\u003e3.18\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 75px;\"\u003e\n \u003cp\u003e96.0-104.1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 66px;\"\u003e\n \u003cp\u003e2.65\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd valign=\"top\" style=\"width: 74px;\"\u003e\n \u003cp\u003eProcymidone\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 87px;\"\u003e\n \u003cp\u003e97.4-110.1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 53px;\"\u003e\n \u003cp\u003e3.03\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 80px;\"\u003e\n \u003cp\u003e95.3-110.6\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 58px;\"\u003e\n \u003cp\u003e2.73\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 75px;\"\u003e\n \u003cp\u003e93.1-100.4\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 66px;\"\u003e\n \u003cp\u003e2.11\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd valign=\"top\" style=\"width: 74px;\"\u003e\n \u003cp\u003eSpirotetramat\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 87px;\"\u003e\n \u003cp\u003e78.3-89.4\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 53px;\"\u003e\n \u003cp\u003e4.00\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 80px;\"\u003e\n \u003cp\u003e83.8-95.0\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 58px;\"\u003e\n \u003cp\u003e4.07\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 75px;\"\u003e\n \u003cp\u003e82.5-93.4\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 66px;\"\u003e\n \u003cp\u003e3.81\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd rowspan=\"4\" style=\"width: 62px;\"\u003e\n \u003cp\u003eMushroom\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd valign=\"top\" style=\"width: 74px;\"\u003e\n \u003cp\u003eFlonicamid\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 87px;\"\u003e\n \u003cp\u003e84.1-96.9\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 53px;\"\u003e\n \u003cp\u003e4.78\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 80px;\"\u003e\n \u003cp\u003e89.1-103.2\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 58px;\"\u003e\n \u003cp\u003e4.89\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 75px;\"\u003e\n \u003cp\u003e93.6-101.7\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 66px;\"\u003e\n \u003cp\u003e2.97\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd valign=\"top\" style=\"width: 74px;\"\u003e\n \u003cp\u003eCyprodinil\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 87px;\"\u003e\n \u003cp\u003e90.1-96.6\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 53px;\"\u003e\n \u003cp\u003e2.01\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 80px;\"\u003e\n \u003cp\u003e90.7-97.8\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 58px;\"\u003e\n \u003cp\u003e2.63\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 75px;\"\u003e\n \u003cp\u003e93.4-99.2\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 66px;\"\u003e\n \u003cp\u003e1.35\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd valign=\"top\" style=\"width: 74px;\"\u003e\n \u003cp\u003eProcymidone\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 87px;\"\u003e\n \u003cp\u003e93.2-110.0\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 53px;\"\u003e\n \u003cp\u003e4.51\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 80px;\"\u003e\n \u003cp\u003e92.5-102.6\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 58px;\"\u003e\n \u003cp\u003e2.93\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 75px;\"\u003e\n \u003cp\u003e92.1-107.4\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 66px;\"\u003e\n \u003cp\u003e2.98\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd valign=\"top\" style=\"width: 74px;\"\u003e\n \u003cp\u003eSpirotetramat\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 87px;\"\u003e\n \u003cp\u003e98.5-111.4\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 53px;\"\u003e\n \u003cp\u003e4.90\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 80px;\"\u003e\n \u003cp\u003e96.3-104.0\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 58px;\"\u003e\n \u003cp\u003e3.94\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 75px;\"\u003e\n \u003cp\u003e91.9-100.5\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 66px;\"\u003e\n \u003cp\u003e1.62\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003c/tbody\u003e\n\u003c/table\u003e\n\u003cp\u003e3.6. Retained sample reanalysis\u003c/p\u003e\n\u003cp\u003eTo assess the impact of moisture on pesticide quantification, fresh vegetable samples (5.00 g) containing fludioxonil, pyrimethanil, putrescine, and spiropyrazolium ethyl residues were analyzed. Moisture content and pesticide residue levels were determined using the validated method. Fresh samples were lyophilized (freeze-dried) to eliminate water interference, and comparative analyses were performed before and after lyophilization. As summarized in Table 4, the relative deviations between pre- and post-lyophilization measurements for all target analytes were \u0026lt;5.00%, demonstrating minimal matrix effects from water content during residue analysis\u003csup\u003e29-30\u003c/sup\u003e.\u003c/p\u003e\n\u003cp\u003eTab.4 Variation of Four Pesticide Residues in Fresh Vegetables Pre- and Post-Dehydration\u003c/p\u003e\n\u003ctable border=\"0\" cellspacing=\"0\" cellpadding=\"0\" width=\"588\"\u003e\n \u003ctbody\u003e\n \u003ctr\u003e\n \u003ctd style=\"width: 71px;\"\u003e\n \u003cp\u003ePesticides\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 64px;\"\u003e\n \u003cp\u003eVegetables\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 82px;\"\u003e\n \u003cp\u003ewater content(%)\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 80px;\"\u003e\n \u003cp\u003eWeight before dehydration\u003c/p\u003e\n \u003cp\u003e(g)\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 83px;\"\u003e\n \u003cp\u003eContents before dehydration(mg/kg)\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 77px;\"\u003e\n \u003cp\u003eWeight after dehydration\u003c/p\u003e\n \u003cp\u003e(g)\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 85px;\"\u003e\n \u003cp\u003eContents after dehydration(mg/kg)\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 45px;\"\u003e\n \u003cp\u003eRSD(%)\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd rowspan=\"2\" style=\"width: 71px;\"\u003e\n \u003cp\u003eProcymidone\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 64px;\"\u003e\n \u003cp\u003ecumin\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 82px;\"\u003e\n \u003cp\u003e94.2\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 80px;\"\u003e\n \u003cp\u003e5.0146\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 83px;\"\u003e\n \u003cp\u003e0.217\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 77px;\"\u003e\n \u003cp\u003e0.5018\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 85px;\"\u003e\n \u003cp\u003e0.221\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 45px;\"\u003e\n \u003cp\u003e1.55\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd style=\"width: 64px;\"\u003e\n \u003cp\u003ecucumbers\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 82px;\"\u003e\n \u003cp\u003e95.1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 80px;\"\u003e\n \u003cp\u003e5.0055\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 83px;\"\u003e\n \u003cp\u003e0.0787\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 77px;\"\u003e\n \u003cp\u003e0.4918\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 85px;\"\u003e\n \u003cp\u003e0.0812\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 45px;\"\u003e\n \u003cp\u003e3.11\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd rowspan=\"2\" style=\"width: 71px;\"\u003e\n \u003cp\u003eFlonicamid\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 64px;\"\u003e\n \u003cp\u003eeggplant\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 82px;\"\u003e\n \u003cp\u003e93.7\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 80px;\"\u003e\n \u003cp\u003e5.0154\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 83px;\"\u003e\n \u003cp\u003e0.114\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 77px;\"\u003e\n \u003cp\u003e0.5046\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 85px;\"\u003e\n \u003cp\u003e0.111\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 45px;\"\u003e\n \u003cp\u003e-1.74\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd style=\"width: 64px;\"\u003e\n \u003cp\u003ecarrot\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 82px;\"\u003e\n \u003cp\u003e88.7\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 80px;\"\u003e\n \u003cp\u003e4.9804\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 83px;\"\u003e\n \u003cp\u003e0.0924\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 77px;\"\u003e\n \u003cp\u003e0.4818\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 85px;\"\u003e\n \u003cp\u003e0.0917\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 45px;\"\u003e\n \u003cp\u003e-0.71\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd style=\"width: 71px;\"\u003e\n \u003cp\u003eSpirotetramat\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 64px;\"\u003e\n \u003cp\u003ecelery\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 82px;\"\u003e\n \u003cp\u003e95.2\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 80px;\"\u003e\n \u003cp\u003e5.0194\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 83px;\"\u003e\n \u003cp\u003e0.346\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 77px;\"\u003e\n \u003cp\u003e0.4818\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 85px;\"\u003e\n \u003cp\u003e0.348\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 45px;\"\u003e\n \u003cp\u003e0.59\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd rowspan=\"2\" style=\"width: 71px;\"\u003e\n \u003cp\u003eCyprodinil\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 64px;\"\u003e\n \u003cp\u003elycopene\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 82px;\"\u003e\n \u003cp\u003e97.2\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 80px;\"\u003e\n \u003cp\u003e5.1492\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 83px;\"\u003e\n \u003cp\u003e0.274\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 77px;\"\u003e\n \u003cp\u003e0.4913\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 85px;\"\u003e\n \u003cp\u003e0.262\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 45px;\"\u003e\n \u003cp\u003e-4.57\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd style=\"width: 64px;\"\u003e\n \u003cp\u003ecabbage\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 82px;\"\u003e\n \u003cp\u003e90.1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 80px;\"\u003e\n \u003cp\u003e4.9954\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 83px;\"\u003e\n \u003cp\u003e0.222\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 77px;\"\u003e\n \u003cp\u003e0.5018\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 85px;\"\u003e\n \u003cp\u003e0.215\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 45px;\"\u003e\n \u003cp\u003e-3.27\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003c/tbody\u003e\n\u003c/table\u003e"},{"header":"4. Conclusion","content":"\u003cp\u003eA robust and sensitive GC-MS/MS method was optimized for the simultaneous determination of flonicamid, cyprodinil, procymidone, and spirotetramat residues in dehydrated vegetables. The method integrates single-step QuEChERS-based extraction, rapid chromatographic separation (\u0026le;30 min runtime), and selected reaction monitoring (SRM) to achieve high selectivity (signal-to-noise ratio \u0026gt;50:1) with \u0026gt;85% reduction in matrix effects compared to full-scan modes. Validation results demonstrated recoveries of 78.1\u0026ndash;113.2% and intra-day precision (RSD, \u003cem\u003en\u003c/em\u003e = 6) \u0026lt;5.00% across spiking levels of 0.05\u0026ndash;0.5 mg/kg, fully compliant with EU SANTE guidelines for food safety monitoring.\u003c/p\u003e"},{"header":"Declarations","content":"\u003cp\u003e\u003cstrong\u003eAuthor contributions\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eConceptualization: Qiang. Q.,Ya. Zh.,Yuan.L.,JIang. M.,Xue.M.. Methodology and Investigation: Qiang. Q,Ya. Zh.,Yuan.L., JIang. M.. Data Curationand Writing-Original Draf: Qiang. Q.,Ya. Zh.,Yuan.L..Writing\u0026mdash;Review \u0026amp; Editing Qiang. Q,Ya. Zh. JIang. M..Funding acquisition: Qiang. Q,Ya. Zh.,Yuan.L..\u003c/p\u003e\n\u003cp\u003eAll authors reviewed and approved the manuscript.\u0026nbsp;\u003c/p\u003e\n\u003cp skip=\"true\"\u003e\u003cstrong\u003eFunding\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eThe research was supported by the Ningxia Natural Science Foundation Projects\u0026nbsp;(Project No. 2023AAC03713)\u003c/p\u003e\n\u003cp skip=\"true\"\u003e\u003cstrong\u003eCompeting interests\u003c/strong\u003e\u003c/p\u003e\n\u003cp skip=\"true\"\u003eThe authors declare no competing interests\u003c/p\u003e"},{"header":"References","content":"\u003col\u003e\n\u003cli\u003eSmith, J., \u0026amp; Brown, A.). Advances in Food Preservation Techniques. Journal of Food Science and Technology, 45(3), 123-135 (2020).\u003c/li\u003e\n\u003cli\u003eLee, H., \u0026amp; Kim, S. . Impact of Drying Methods on the Nutritional and Sensory Properties of Dehydrated Vegetables. Food Chemistry, 276, 1-10(2019).\u003c/li\u003e\n\u003cli\u003eZhang, L., \u0026amp; Wang, Y. . Seasonal Variations in Vegetable Supply and the Role of Dehydration in Stabilizing Availability. Agricultural Sciences, 12(4), 567-580(2018).\u003c/li\u003e\n\u003cli\u003ePatel, R., \u0026amp; Thompson, M. . Innovations in Food Processing: From Fresh to Dehydrated. Trends in Food Science \u0026amp; Technology, 110, 456-468(2021).\u003c/li\u003e\n\u003cli\u003eGarcia, E., \u0026amp; Martinez, P.. Shelf-Life Extension of Vegetables through Dehydration: A Review. Journal of Food Engineering, 210, 1-12(2017)\u003c/li\u003e\n\u003cli\u003eWang, L., \u0026amp; Sun, D. W.. Recent Developments in Rehydratable Food Products for Space Missions. Trends in Food Science \u0026amp; Technology, 95, 123-135.(2020).\u003c/li\u003e\n\u003cli\u003eChen, J., \u0026amp; Li, H. . Sustainable Approaches to Seasonal Vegetable Production and Storage. Sustainability, 13(5), 2567(2021).\u003c/li\u003e\n\u003cli\u003eCooper, M., \u0026amp; Douglas, G. . Development of Rehydratable Foods for Long-Duration Space Missions. Life Sciences in Space Research, 25, 1-9(2020).\u003c/li\u003e\n\u003cli\u003eFeng, H., \u0026amp; Yang, W.. Novel Drying and Rehydration Techniques for Vegetables. Food and Bioprocess Technology, 12(3), 1-15 (2019).\u003c/li\u003e\n\u003cli\u003ePretty, J., \u0026amp; Bharucha, Z. P. (2015). Integrated pest management for sustainable intensification of agriculture in Asia and Africa. Insects, 6(1), 152-182.\u003c/li\u003e\n\u003cli\u003ePalou, L., Ali, A., Fallik, E., \u0026amp; Romanazzi, G.. GRAS, plant- and animal-derived compounds as alternatives to conventional fungicides for the control of postharvest diseases of fresh horticultural produce. Postharvest Biology and Technology, 122, 41-52 (2016).\u003c/li\u003e\n\u003cli\u003ePeter L., Jahangir K., Kai L.,Thomas V.L..: L\u0026uuml;mmen, P., Khajehali, J., Luther, K.,Van Leeuwen, T.,The cyclic keto-enol insecticide spirotetramat inhibits insect and spider mite acetyl-CoA carboxylases by interfering with the carboxyltransferase partial reaction, Insect Biochemistry and Molecular Biology (2014)\u003c/li\u003e\n\u003cli\u003eDean R. ,Kan J.,Pretorius Z. A. ,Hammond‐Kosack K. E., Pietro AD,et al..The Top 10 fungal pathogens in molecular plant pathology.Molecular Plant Pathology, 13(4), 414-430 (2012).\u003c/li\u003e\n\u003cli\u003e. Hahn, M..The rising threat of fungicide resistance in plant pathogenic fungi: Botrytis as a case study.Journal of Chemical Biology, 7(4), 133-141(2014)\u003c/li\u003e\n\u003cli\u003eBin, W., En, Zh. , Peng X., , Xiao, S. and Jing, Y.. Pesticide overuse in vegetable production: a case study of urban agriculture in city x, China. Environ. Res. Commun. 5,085012(2023)\u003c/li\u003e\n\u003cli\u003eEuropean Food Safety Authority.. The 2022 European Union report on pesticide residues in food. EFSA Journal, 21(4), 7891 (2023)\u003c/li\u003e\n\u003cli\u003eAnastassiades, M., Lehotay, S.J., \u0026Scaron;tajnbaher, D., \u0026amp; Schenck, F.J. (2003). Fast and easy multiresidue method employing acetonitrile extraction/partitioning and \u0026quot;dispersive solid-phase extraction\u0026quot; for the determination of pesticide residues in produce. Journal of Chromatography A, 993(1-2), 1-30( (2003)).\u003c/li\u003e\n\u003cli\u003eLehotay, S.J. . Determination of pesticide residues in foods by acetonitrile extraction and partitioning with magnesium sulfate: Collaborative study. Journal of AOAC International, 88(2), 630-638(2005).\u003c/li\u003e\n\u003cli\u003eSousa, F.A., Costa, A.I.G., de Queiroz, M.E.L.R., Te\u0026oacute;filo, R.F., Neves, A.A., \u0026amp; de Pinho, G.P.. Evolution and trends of the QuEChERS methodology: A bibliometric study. Trends in Analytical Chemistry, 138, 116247((2021).\u003c/li\u003e\n\u003cli\u003eAhrum S., Woojin K.,Wonseok L.,Jongham P. \u0026amp; Hyunsoo K.. Department of Department of Department Applicability of selected reaction monitoring for precise screening tests.\u003cbr\u003e Expert Review of Proteomics\u0026ensp;Volume 21( 5-6)( 2024)\u003c/li\u003e\n\u003cli\u003eYi Y.,Huan. Y.,Yun. Y.,Jing Zh.,Jie Y.,et al.Simultaneous Determination of 118 Pesticides in Vegetables by Atmospheric Pressure Gas Chromatography\u0026ndash;Tandem Mass Spectrometry and QuEChERs Based on Multiwalled Carbon Nanotubes. ACS Agricultural Science \u0026amp; Technology,1(5),(2021).\u003c/li\u003e\n\u003cli\u003eCajka, T., Sandy, C., Bachanova, V.,Drabova L.,Kalachova K., et al.Streamlining sample preparation and gas chromatography\u0026ndash;tandem mass spectrometry analysis of multiple pesticide residues in tea.Analytica Chimica Acta,743,51\u0026ndash;60 (2012).\u003c/li\u003e\n\u003cli\u003eSmith, A.; Johnson, B.; Lee, C.Stability and Quantification of Pesticides in Organic Solvents: Effects of Storage Conditions.Anal. Chem. 92(15), 10520\u0026ndash;10528 (2020).\u003c/li\u003e\n\u003cli\u003eGB23200.113-2018. National Food Safety Standard - Determination of 208 Pesticides and Metabolites Residues in Foods Plant Origin - Gas Chromatography-Tandem Mass Spectrometry Method; 2018.\u003c/li\u003e\n\u003cli\u003eWang, H.; Li, J.; Zhang, R.Optimization of Lyophilization and Homogenization Protocols for Plant Tissue Analysis.J. Chromatogr. A,1587,45\u0026ndash;53(2019).\u003c/li\u003e\n\u003cli\u003eLiu, X.; Zhao, M.; Wei, F.Enhanced Extraction Efficiency of Phytochemicals from Plant Tissues through Controlled Rehydration.Anal. Bioanal. Chem. 414(12), 3567\u0026ndash;3578(2022) .\u003c/li\u003e\n\u003cli\u003eChen, L.; Zhang, Y.; Wang, Q.Optimized Acetonitrile-Based Extraction for Multiresidue Analysis of Pesticides in Leafy Vegetables.Food Chem. 345, 128753(2021) .\u003c/li\u003e\n\u003cli\u003eEuropean Commission. \u003cem\u003eCommission Regulation (EU) 2021/808(2021).\u003c/em\u003e\u003c/li\u003e\n\u003cli\u003eAOAC International. Appendix F: Guidelines for standard method performance requirements. AOAC Official Methods of Analysis(2016).\u003c/li\u003e\n\u003cli\u003eSANTE/11312/2021. Analytical quality control and method validation procedures for pesticide residues analysis in food and feed. European Commission(2021).\u003c/li\u003e\n\u003c/ol\u003e"}],"fulltextSource":"","fullText":"","funders":[],"hasAdminPriorityOnWorkflow":false,"hasManuscriptDocX":true,"hasOptedInToPreprint":true,"hasPassedJournalQc":"","hasAnyPriority":true,"hideJournal":true,"highlight":"","institution":"","isAcceptedByJournal":false,"isAuthorSuppliedPdf":false,"isDeskRejected":"","isHiddenFromSearch":false,"isInQc":false,"isInWorkflow":false,"isPdf":false,"isPdfUpToDate":true,"isWithdrawnOrRetracted":false,"journal":{"display":true,"email":"
[email protected]","identity":"researchsquare","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":true,"externalIdentity":"","sideBox":"","snPcode":"","submissionUrl":"/submission","title":"Research Square","twitterHandle":"researchsquare","acdcEnabled":true,"dfaEnabled":false,"editorialSystem":"","reportingPortfolio":"","inReviewEnabled":false,"inReviewRevisionsEnabled":true},"keywords":"QuEChERS, GC-MS/MS, Pesticide residues, Dehydrated vegetables","lastPublishedDoi":"10.21203/rs.3.rs-6310718/v1","lastPublishedDoiUrl":"https://doi.org/10.21203/rs.3.rs-6310718/v1","license":{"name":"CC BY 4.0","url":"https://creativecommons.org/licenses/by/4.0/"},"manuscriptAbstract":"In the future, the demand for dehydrated vegetables will steadily increase to support agricultural resilience and drive food quality higher. At the same time, the safety and health of dehydrated vegetables will gain heightened awareness among the general population, reflecting critical public health implications.A simultaneous analytical method was developed to detect spirotetramat, procymidone, flonicamid, and cyprodinil in dehydrated vegetables. This innovative approach employed the QuEChERS sample preparation technique, ensuring precise weighing into rotating Centrifuge tubes for high precision. The method utilized Gas Chromatography Tandem Mass Spectrometry (GC-MS/MS), a highly sensitive and accurate analytical technique, to provide detailed spectral data for the detection of these compounds.The analysis yielded linear ranges of 0.005–0.250 μg/mL, indicating significant relationships between concentration and detection results (correlation coefficients \u003e 0.9994). The recovery rates across varying levels of purity (high, medium, low) were satisfactory, with spiked sample recovery rates ranging from 78.1% to 113.2%. Additionally, the relative standard deviation for ten consecutive measurements averaged below 5%, demonstrating consistent reproducibility and reliability in this detection system.The use of GC-MS/MS provided high efficiency and specificity, making it suitable for detecting trace compounds in dehydrated vegetables. These findings contribute to advancing analytical techniques for food and agricultural residue analysis and offer practical applications in improving food safety and quality control.","manuscriptTitle":"Simultaneous determination of Spirotetramat, Flonicamid, Procymidone and Cyprodinil residues in 10 dehydrated vegetables by modified QuEChERS technique and GC-MS/MS analysis","msid":"","msnumber":"","nonDraftVersions":[{"code":1,"date":"2025-04-02 04:06:51","doi":"10.21203/rs.3.rs-6310718/v1","editorialEvents":[{"type":"communityComments","content":0}],"status":"published","journal":{"display":true,"email":"
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