Determination of Boric acid by ICP-AES and ICP-MS in Caviars and Processed food

Determination of Boric acid by ICP-AES and ICP-MS in Caviars and Processed food | 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 Research Article Determination of Boric acid by ICP-AES and ICP-MS in Caviars and Processed food Jae-Wook Shin, Jung-Bok Kim This is a preprint; it has not been peer reviewed by a journal. https://doi.org/ 10.21203/rs.3.rs-4211245/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 . Boric acid is authorized as food additive in EU. However, it is not authorized for use in Korea. The analytical method of boric acid in foods has not been reported in Korea. In this study, an analytical method has been developed and validated for the determination of boric acid in caviars. We established the analytical assay for boric acid in caviars by Inductively Coupled Plasma Mass Spectrometry(ICP-MS). Caviar samples were digested in closed vessels made of PTFE in an Automatic Microwave Digestion System. We also performed a method validation including linearity, inter-day, intra-day, precision, accuracy, Limit of detection (LOD) and Limit of Quantitation(LOQ) and recovery. The calibration curve was obtained from 0.2 µg/mL to 10 µg/mL with a satisfactory correlation coefficient of 0.99. The LOD and LOQ were 0.04 µg/mL and 0.16 µg/mL. The recoveries of boric acid from spiked samples at levels of 0.5, 2 and 10 µg/mL ranged from 91.8 to 98.3% with relative standard deviation(RSD) between 0.4 and 2.4 %. Boric acid ICP-MS Method validation Caviars Figures Figure 1 Figure 2 Figure 3 1. Introduction In a modern society, consumers’ preferences and needs for food have become more diverse after industrial development. In addition, a wide variety of food additives have been used for the purpose of improving quality, nutrition and customer preference. The purpose of additives greatly varies, but they are mostly used to improve the quality of the main material or keep it stable. Diverse supplements used for the stability ingredients in pharmaceuticals and even preservatives used in food belong to additives as well (KFDA The Guideline of Drug Excipients, 2007 ). In the Korea Food Additives Code, 14 food preservatives are allowed, and the standards for the use of each preservative are stated. They are described as the criteria for the food on the Korean Food Standards Codex and Guidelines for Pharmaceutical Excipients. This study confirmed for standards and specifications of preservative in other country, such as USA (FDA food additive list and color additive list, 2022 ), EU (EU Food Standards Agency, 2012 ), and Japan (MHLW Ministry of Health, Labour and welfare, 2023). etc. Codex had designated 13 item of preservatives. When they were classified into systematic groups such as sorbic acid, benzoic acid, p-hydroxybenzoate and propionic acid (FMO Food and Agriculture Organization, 2006 , CODEX ALIMENTARIUS, 2021 ), they were all used in USA, EU and Japan, There was a little difference in detail for each country. In the case of korea, food additives are substances with a clear purpose of use, and their use other than the intended purpose is prohibited, and they are always used in processing and manufacturing food. As a result, various problems arise during international trade due to different types of food additives, current status of designation, and standards for use in each country. In food, a food preservative is a chemical substance added to improve food preservation. It plays a role of antiseptic which inhibits the growth of bacteria and also controls mold growth. Currently, many countries have banned the use of boric acid as a food additive but in some Asian countries. In case of Hong-kong, boric acid is still used for noodle and fish ball as food additive. Boric acid and sodium tetraborate are authorized as food additive, in EU and the maximum permissible dose is limited to 4000 mg/kg (EU Official Journal of the European Union, 2011 ). But boric acid is not authorized for use in Korea(Korean Food Code, 2023 , Korean Food Additives Code, 2021 ). and the analytical method of boric acid in foods has not been reported in Korea. For the analysis of boric acid and sodium tetraborate in food, after derivatization using triethanolamine, analysis method using GC-MS(Li-Min Zeng, Hao-Yang Wang, Yin-Long Guo, 2010), 11B-NMR analysis using Polarizing Plates(Seiya kunimasa, Makoto Tasaki, Hiromi Yamada, Shinji Morimoto, Manabu Togal, 2012), qualitative analysis method applying Curcumin paper method and 2-ethyl-1,3- A spectrophotometric analysis method using hexanediol/chloroform (EHD) solution has been reported (Yoshida M, Watabiki T, Ishida N, 1989 ). MC-ICPMS and NTIMS were used to analyze boron isotopes in boric acid, seawater, and marine CaCO3 samples(Gavin L. Foster, Bärbel Hönisch, Guillaume Paris, Gary S. Dwyer, James W.B. Rae, Tim Elliott, Jérôme Gaillardet, N. Gary Hemming, Pascale Louvat, Avner Vengosh, 2013). However, these analysis methods require a lot of time and money for qualitative and quantitative analysis of samples. According to the paper, the content of boric acid in food is 130–926 µg/mL in fish ball, 161–489 µg/mL in Kuey teow noodle, 918 ppm in agar-agar strips, 347 µg/mL in fresh prawn, and 819 µg/mL in mango (pickled). It was reported to be detected in various food samples (Ang Swi See, Abu Bakar Salleh, Fatimah Abu Bakar, Nor Azah Yusof, Ahmed Sahib Abdulamir and Lee Yook Heng, 2010, S Siti-Mizura, E S Tee and H E Ooi, 1991). Analyis of boron as boric acid in eye lotions using a sequential injection system (J. (Koos) F, van Staden, M.(Mutshutshu) Tsanwani, 2002). According to the reported AOAC Method, various sample preparation and analysis methods were used to analyze boric acid in the sample(AOAC official method 969.26, 2005; AOAC official method 990.34, 2005, AOAC official method 972.19, 2005, AOAC official method 975.26, 2005). In not allowed countries such as Korea, safety management is difficult because there is no analysis method for products distributed domestically and internationally. Thus, in this study the sample preparation and analysis method of boric acid in Caviar and processed food were established and validity was verified. In addition, using the established analysis method, analysis time, cost and low concentration analysis became possible. As well as, It is expected that it will be a good research data for setting standard specifications and safety management of boric acid. 2. Materials and Methods 2.1. Reagents and material Standard boric acid(Assay 99.999%) and sodium tetraborate (Assay 99.9%) was obtained from Sigma-Aldrich (St Louis, MO, USA). Boron CRM standard solution (Lot : 214065136) was purchased from Accustandard (New Haven, CT, USA), Nitric acid, Hydrogen peroxide and ammonium hydroxide. The study has obtained from Sigma-Aldrich (St Louis, MO, USA). Ultrapure deionized water (resistivity > 18 MΩ·cm) from a Milli-Q system (Millipore, Billerica, MA, USA) was used for all experiments. 2.2 Instrument and analysis conditions The ICP apparatus was a spectro SPECTRO BLUE ICP-AES system (USA) equipped with axial, radial and twin interface. The ICP-AES was consisted of Quartz nebulizer, Quartz spray chamber and Quartz injector. The analysis condition by ICP-AES were Nebulizer gas flow 0.8 L/min, coolant gas flow 13.0 L/min, Auxiliary gas flow 0.8 L/min, Plasma power 1400 W, and Pump speed 30 RPM. The wavelength were 182.641, 249.677 and 249.773nm. 249.773 nm was quantitative wavelength. 182.641 nm and 249.677 nm were qualitative wavelength(Table 1 ). ICP-MS was purchased from Therm Fisher Scientific in USA (Thermo Finnigan, San Jose, CA, USA). The analysis condition by ICP-AES were RF power 1550 W, PFA Nebulizer 100 uL/min, Nebulizer gas 0.79 L/min, Auxiliary gas 0.80 L/min, Cool gas 14 L/min and Sample uptake rate 0.25 mL/min. The Selected isotopes(m/z) was 11(11B). The detailed operating conditions of ICP-MS were optimized and were summarized in Table 2 . Table 1 ICP conditions for boric acid quantification Instrument parameters Condition - Quartz nebulizer - Quartz spray chamber - Quartz injector Nebulizer gas flow 0.8 L/min Coolant gas flow 13.0 L/min Auxiliary gas flow 0.8 L/min Plasma power 1400 W Pump speed 30 RPM. Wavelength 182.641, 249.677 , 249.773nm Table 2 ICP-MS conditions for boric acid quantification Instrument parameters Condition RF power 1550 W Nebulizer PFA Nebulizer 100 uL/min Argon gas flow rate Nebulizer gas 0.79 L/min Auxiliary gas 0.80 L/min Cool gas 14 L/min Sample uptake rate 0.25 mL/min Selected isotopes(m/z) 11( 11 B) 2.3 Sample preparation The study has subjected to microwave-assisted acid digestion to obtain the fully decomposed sample blend and procedure blank solutions. In optimized conditions for the microwave assisted acid digestion, CEM(MARS model) Ultrawave microwave digestion system CEM(MARS6, NC, USA) was used, which is equipped with 15 small digestion vessels in a single reaction chamber. The study has weighed 0.5g of caviar for ICP analysis. Immediately, nitric acid 5mL and Hydrogen peroxide 2mL were added to 0.5 g of sample in vessel. 5 mL of HNO 3 (about 65%) was added to each small digestion vessel. The digestion vessels were inserted into a Teflon outer bath, and 130 mL of deionized water and 2 mL of H 2 O 2 were added to the outer bath. The small digestion vessels with caps were heated in a closed microwave reaction chamber. Then, the reaction chamber temperature was maintained at 180°C for 30 min. The study has filled up by distilled water in 50mL volumn flask for analysis. Finally, the study has measured of boric acid in caviar by ICP and ICP-MS. 3. Result and discussion 3.1 Optimization of the ICP-OES and ICP-MS method The study has determinated for boron by ICP-AES in caviars. Firstly, we found wavelength analysis of boron in caviar by ICP-AES. we have the wavelength that are 182.641, 279.677 and 249.773 nm. The correlation coefficients for all calibration curves were at least 0.999 in microwave wavelength of three. The linearity range of the standard curves was 0.5–10 µg/mL. The BEC value of boron is measured 0.02 to 0.03ppm by ICP-AES(Fig. 1 ). We are selected one of three wavelenght for measure of boron by ICP-AES. The wavelength is 249.773nm for quantitative analysis. The 182.641 and 279.677nm are used for wavelength of qualitative analysis(Fig. 2 ). It is allowed as a preservative in Europe, such as boric acid and sodium tetraborate. Boric acid and sodium tetraborate have been managing as boric acid in Europe. As well, boric acid has been allowing as boron. The study has purchased boron standard solution in Accustandard. The concentration of boron standard solution is 1000 µg/mL. The study has measured boron in boric acid and sodium tetraborate by ICP-AES. As a result, we confirmed same concentration of boron in standard solution. 3.2 Sample preparation The study has subjected to microwave-assisted acid digestion to obtain the fully decomposed sample blend and procedure blank solutions. In optimized conditions for the microwave assisted acid digestion, CEM(MARS model) Ultrawave microwave digestion system (CEM(MARS6, NC, USA) was used, which is equipped with 15 small digestion vessels in a single reaction chamber. The study has weighed 0.5g of caviar for ICP analysis. Immediately, nitric acid 5mL and Hydrogen peroxide 2mL were added to 0.5 g of sample in vessel. 5 mL of HNO3 (about 65%) was added to each small digestion vessel. The digestion vessels were inserted into a Teflon outer bath, and 130 mL of deionized water and 2 mL of H 2 O 2 were added to the outer bath. The small digestion vessels with caps were heated in a closed microwave reaction chamber. Then, the reaction chamber temperature was maintained at 180°C for 30 min. The study has filled up by distilled water in 50mL volumn flask for analysis. Finally, the study has measured of boric acid in caviar with ICP(Fig. 3 ). 3.3 Method validation Validation method was conducted by means of the following parameters: linearity, matrix effect, precision and accuracy, LOD & LOQ, Uncertainty of measurement and Inter-lab reproducibility. Linearity was developed with matrix-effect calibration via analyzing sample of caviar. The calibration curve was confirmed from 0.5 µg/mL to 10 µg/mL with a satisfactory correlation coefficient (> 0.999). 3.3.1 Selectivity & specification The Selectivity and specification should be demonstrated by the analysis of representative blank matrix materials from multiple sources. The study has measured the blank sample that is collected for identify selectivity and specification. The study has confirmed no interference so it has acquired selectivity and specification. 3.3.2 Linearity The accuracy of boron from spiked sample at levels of 0.5–10.0 µg/mL ranged from 98.9 to 100.6% with RSD between 0.1 and 1.3%. The correlation coefficients for calibration curve was at least 0.999 in sample(Table 3 ). Table 3 Linearity of boron by ICP-AES Conc.(µg/mL, n = 3) 0.5 1 2 5 10 1 day 0.49 1.00 2.00 5.05 9.97 2 day 0.49 0.98 2.02 5.01 9.99 3 day 0.50 0.98 2.01 5.01 9.99 Mean 0.49 0.99 2.01 5.03 9.99 Precision (%) 1.3 1.3 0.6 0.5 0.1 Accuracy (%) 99.0 98.9 100.5 100.6 99.9 3.3.3 Precision and accuracy of Intra-day & inter-day The results of the boron precision and accuracy study are summarized in Tables 13 and 14. The spiking levels chosen for the precision and accuracy studies were 0.5, 2.0, and 10.0 ppm in matrices for all analyte. The precision of boron analysis was estimated using the RSD for both intra-day and inter-day. For all test samples, the RSDs of intra-day and inter-day precision ranged from 0.4 to 0.6% and 0.5 to 2.1%. Additionally, the study has confirmed the accuracy of intra-day and inter-day ranged from 99.1 to 100.6% and 96.8 to 100.2% (Table 4 , 5 ). Table 4 Precision and accuracy of Intra-day and Intra-day by ICP-AES Conc. (µg/mL,n = 3) 0.5 2.0 10.0 n = 1 0.50 2.00 10.02 n = 2 0.50 2.01 10.05 n = 3 0.49 2.03 10.11 Mean 0.50 2.01 10.06 Precision(%) 0.6 0.6 0.4 Accuracy(%) 99.1 100.6 100.6 Table 5 Precision and accuracy of Inter-day by ICP-AES Conc. (µg/mL,n = 3) 0.5 2.0 10.0 1 day 0.50 2.01 10.10 2 day 0.48 1.99 10.00 3 day 0.48 1.99 9.90 Mean 0.48 2.00 10.02 Precision(%) 2.1 0.5 0.6 Accuracy(%) 96.8 100.0 100.2 3.3.4 LOD & LOQ The study has used ICP-AES in order to calculate LOD and LOQ. As well, the study has checked S/N ratio of boron in matrix. The study has calculated MDL using Environmental Protection Agency (EPA) method for detection of MDL (40 CFR Part 136. APPENDEX B, revision 1.11). For ICP-AES, the LOD and LOQ of boron were 0.03 µg/mL and 0.1 µg/mL. 3.3.5 Result of recovery The recoveries of boron from spiked samples at levels of 0.5, 2 and 10.0 µg/mL ranged from 98.0 to 102.0% with RSDs between 0.1 and 0.4%(Table 6 ). Table 6 The result of recovery for boric acid Conc.(µg/mL) Detected value(µg/mL) Mean CV(%) Recovery(%) n = 1 n = 2 n = 3 0.5 0.48 0.50 0.50 0.49 0.1 98.0 2.0 2.03 2.03 2.05 2.04 0.4 102.0 10.0 10.19 10.15 10.12 10.15 0.3 101.5 3.3.6 Meauremetn of uncertainty To assess the suitability of the analytical method for use in the laboratory, the uncertainty measurement of boron in caviar spiked with 203.1 mg/kg boron was estimated using the ICP-AES. The uncertainty in the measurements was identified and used as parameters to determine the combined standard uncertainty based on GUM (guide to the expression of uncertainty in measurement) and the Draft EURACHEM/CITAC Guide(EURACHEM., 2000, ISO., 2002). The final U, for a level of confidence of approximately 95% and considering a coverage factor of 2, was found to be 203.1 ± 10.8 (mg/kg) for the ICP-AES method (Table 7 ). Table 7 Expanded uncertainty a of boron level using ICP-AES and 203.1 mg/kg in caviar Parameters of Uncertainty Result Unit Certified Concentration 203.1 mg/kg The result of uncertainty 203.1 ± 10.8 (k = 2, 95% confidence level) mg/kg Expanded uncertainty(U) 10.82 mg/kg Coverage factor(k) 2 dimensionless unit degrees of freedom,(veff) 19 dimensionless unit Combined Standard Uncertainty (u c ) 5.41 mg/kg Combined relative Standard Uncertainty (u r /r) 0.027 dimensionless unit 3.4 Result of sample analysis The method developed in this study was used to monitor the presence of boric acid and sodium tetraborate residue levels in caviars including various roe samples in domestic and foreign markets. A total of 104 real samples of caviars and various roe were collected from grocery markets in South Korea (39), and the Europe (65). Of the 104 analyzed samples, 33 contained 46.0 ~ 3942.2 mg/kg boric acid. Boric acid and sodium tetraborate were not found in any of the samples such as caviar, salted pollack roe and Flying Fish Roe. The boric acid concentrations were under the legal limit of 4000 mg/kg as specified in EU (Table 8 ). Table 8 The determination of boric acid by ICP-AES in caviars. * As boric acid : Boric acid conc.(mg/kg) = Boron x Mw(Boric acid) ÷ MW(Boron), N.D : Not detection Method of collection Name of sample The number of sample The number of detection Range (mg/kg) Type of food Domestic market in Korea Caviar 7 2 3106.2 ~ 3549.2 Various roe 32 0 ND Herring Roe, Lumpfish Roe, Soused roe, noodles, Flying Fish Roe, etc. Foreign market in Europe Caviar 31 31 46.0 ~ 3942.2 Various roe 24 0 ND Herring Roe, Lumpfish Roe, Salmon Roe, Trout roe, Flying Fish Roe etc. * As boric acid : Boric acid conc.(mg/kg) = Boron x Mw(Boric acid) ÷ MW(Boron), N.D : Not detection 4. Conclusions The study has determinated for boron by ICP-AES in caviars. Firstly, we found wavelength analysis of boron in caviar by ICP-AES. we have the wavelength that are 182.641, 279.677 and 249.773 nm. The correlation coefficients for all calibration curves were at least 0.999 in microwave wavelength of three. The linearity range of the standard curves was 0.5–10 µg/mL. The BEC value of boron is measured 0.02 to 0.03ppm by ICP-AES. The study has purchased boron standard solution in Accustandard. The concentration of boron standard solution is 1000µg/mL. The study has measured boron in boric acid and sodium tetraborate by ICP-AES. To assess the suitability of the analytical method for use in the laboratory, the uncertainty measurement of boron in caviar spiked with 203.1 ± 10.8 mg/kg boron was estimated using the ICP-AES. The study has subjected to microwave-assisted acid digestion to obtain the fully decomposed sample blend and procedure blank solutions. A total of 104 real samples of caviars and various roe were collected from grocery markets in South Korea (39), and the Europe (65). Of the 104 analyzed samples, 33 contained 46.0 ~ 3942.2 mg/kg boric acid. Boric acid and sodium tetraborate were not found in any of the samples such as caviar, salted pollack roe and Flying Fish Roe. The boric acid concentrations were under the legal limit of 4000 mg/kg as specified in EU (Table 17). Declarations Author Contribution he authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper. Acknowledgements This research was supported by a grant(14162MFDS971) the Ministry of Food and Drug Safety in 2014. References AOAC Official Method 969.26 AOAC. (2005). Boric Acid in Caviar Spectrophotometric Method. AOAC Official Method 970.34 AOAC. (2005). Boric Acid in Caviar Titrimetric Method. AOAC Official Method 972.19 AOAC. (2005). Boric Acid in Food Atomic Absorption Spectro photometric Method. AOAC Official Method 975.26 AOAC. (2005). Boric Acid in Food Emission Spectroscopic Method. CODEX ALIMENTARIUS.(2021). General Standard for Food Additives(GSFA). EU Official Journal of the European Union.(2011). COMMISSION REGULATION (EU) No 1129/2011 of 11 November 2011 L 295 p 115. EURACHEM. (2000). Quantifying uncertainty in analytical measurement (2nd ed). London: Eurachem. EU Food Standards Agency(2012), Current EU approved additives and their E Numbers. FDA food additive list and color additive list.(2022). FDA (http://www.fda.gov) CFR eCFR(http://www.ecfr.gov/cgi-bin/). FMO Food and Agriculture Organization. (2006). FAO JECFA Monographs Combined compendium of food additive specifications. Foster, G.L., Hönisch, B., Paris, G., Dwyer, G.S., Rae, J.W.B., Elliott, T., Jérôme Gaillardet, J., Gary Hemming, N., Louvat, P., Vengosh, A. (2013). Interlaboratory comparison of boron isotope analyses of boric acid, seawater and marine CaCO3 by MC-ICPMS and NTIMS. Chemical Geology , 358, 1-14. ISO. (2002). Guide to the expression of uncertainty in measurements. International Organization for Standardization (ISO), Geneva Switzerland. Kunimasa, S., Tasaki, M., Yamada, H., Morimoto, S., Togal, M.(2012). Development of a Quantitative Analysis Method for Unreacted Boric Acid in Polarizing Plates. Sumitomo Gagaku R&D Report , 1-12. KFDA The Guideline of Drug Excipients. (2007): Ministry of Food and Drug Safety, Osong, Korea. Korean Food Code. (2023). 8. General test methods, Ministry of Food and Drug Safety, Osong, Korea. Korean Food Additives Code. (2021). III. Standards and Specification for Food Contact Surface Sanitizing Solutions, Ministry of Food and Drug Safety, Osong, Korea. MHLW Ministry of Health, Labour and welfare.(2023). 4. The Japan Food Chemical Research Foundation Standards for Use of Food Additives. See, A.S., Salleh, A. B., Bakar, F.A., Yusof, N. A., Abdulamir, A.S., Heng, L.Y. (2010). Risk and Health Effect of Boric Acid. American Journal of Applied Sciences , 7(5), 620-627. Siti-Mizura, S., Tee, E.S., Ooi, H.E. (1991). Determination of Boric Acid in Foods: Comparative Study of Three Methods. J Sci Food Agric , 55, 261-268. Van Staden, J.F., M.(Mutshutshu) Tsanwani, M. ( 2002). Determination of boron as boric acid in eye lotions using a sequential injection system. Talanta , 58, 1103-1108. Yoshida, M., Watabiki, T., Ishida, N.(1989). Spectrophotometric determination of boric acid by the curcumin method. The Japanese Journal of Legal Medicine, 43(6), 490-496. Zeon, L.M., Wang, H.Y., Guo, Y. L.(2010). Fast quantitative analysis of boric acid by gas chromatography-mass spectrometry coupled with a simple and selective derivatization reaction using triethanolamine. J Am Soc Mass Spectrum, 21, 482-485. Additional Declarations No competing interests reported. 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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-4211245","acceptedTermsAndConditions":true,"allowDirectSubmit":true,"archivedVersions":[],"articleType":"Research Article","associatedPublications":[],"authors":[{"id":289980898,"identity":"73d38ade-7237-47d7-9c3c-7b82e3e75670","order_by":0,"name":"Jae-Wook Shin","email":"","orcid":"","institution":"Korea Advanced Food Research Institute","correspondingAuthor":false,"prefix":"","firstName":"Jae-Wook","middleName":"","lastName":"Shin","suffix":""},{"id":289980899,"identity":"383962bd-5704-4929-8b3e-b0bd3879cbb3","order_by":1,"name":"Jung-Bok Kim","email":"data:image/png;base64,iVBORw0KGgoAAAANSUhEUgAAAZAAAAAyAQMAAABI0h/eAAAABlBMVEX///8AAABVwtN+AAAACXBIWXMAAA7EAAAOxAGVKw4bAAAAyElEQVRIiWNgGAWjYNCCCgYGAyjTAK9CBDhDshbGNlK08E87/vDTzXmHE7eznz3A8KOGwdi8gYAWids5xtK52w4n7uzJS2DsOcZgJnOAkDW3cxjAWjYcyDFg4G1gsJEgpEP+dvrj37lzgFrOvzFg/EuMFoPbCWbSuQ1ALTdyDJiBtpgR1GJ4O8fMOudYuvGGG28MDssckzAmqEUO6LDbOTXWshvO5xg+fFNjYziDkBYoaAaTB4AhSKQGBoY6olWOglEwCkbBCAQASLRBG5A3icIAAAAASUVORK5CYII=","orcid":"","institution":"Yuhan University","correspondingAuthor":true,"prefix":"","firstName":"Jung-Bok","middleName":"","lastName":"Kim","suffix":""}],"badges":[],"createdAt":"2024-04-03 08:42:06","currentVersionCode":1,"declarations":"","doi":"10.21203/rs.3.rs-4211245/v1","doiUrl":"https://doi.org/10.21203/rs.3.rs-4211245/v1","draftVersion":[],"editorialEvents":[],"editorialNote":"","failedWorkflow":false,"files":[{"id":54757708,"identity":"c97b5022-a801-4ab8-b224-62e5ca4ec4aa","added_by":"auto","created_at":"2024-04-16 10:28:47","extension":"png","order_by":1,"title":"Figure 1","display":"","copyAsset":false,"role":"figure","size":76413,"visible":true,"origin":"","legend":"\u003cp\u003e\u003cstrong\u003eThe spectrum of measurement wavelength for boron.\u003c/strong\u003e\u003c/p\u003e","description":"","filename":"1.png","url":"https://assets-eu.researchsquare.com/files/rs-4211245/v1/e5c46ce50dd5bd819bd615b3.png"},{"id":54757411,"identity":"4e3d1cf1-718b-466e-8a02-9b2947a909cc","added_by":"auto","created_at":"2024-04-16 10:20:47","extension":"png","order_by":2,"title":"Figure 2","display":"","copyAsset":false,"role":"figure","size":149237,"visible":true,"origin":"","legend":"\u003cp\u003e\u003cstrong\u003eThe linearity of boron wavelength by ICP-AES\u003c/strong\u003e\u003c/p\u003e","description":"","filename":"2.png","url":"https://assets-eu.researchsquare.com/files/rs-4211245/v1/cc61631d99bf468dd63d33a0.png"},{"id":54757410,"identity":"86969402-fe21-4bf4-b30a-032b4ec580e7","added_by":"auto","created_at":"2024-04-16 10:20:47","extension":"png","order_by":3,"title":"Figure 3","display":"","copyAsset":false,"role":"figure","size":24702,"visible":true,"origin":"","legend":"\u003cp\u003e\u003cstrong\u003e\u0026nbsp;Sample preparation of boric acid and sodium tetraborate by ICP-AES\u003c/strong\u003e\u003c/p\u003e","description":"","filename":"3.png","url":"https://assets-eu.researchsquare.com/files/rs-4211245/v1/eb1bd652fb6cd847272a116f.png"},{"id":55547368,"identity":"d27375a2-cffc-4983-8206-48f01f5c6f67","added_by":"auto","created_at":"2024-04-29 19:37:22","extension":"pdf","order_by":0,"title":"","display":"","copyAsset":false,"role":"manuscript-pdf","size":809590,"visible":true,"origin":"","legend":"","description":"","filename":"manuscript.pdf","url":"https://assets-eu.researchsquare.com/files/rs-4211245/v1/b481307b-bda7-49a7-a719-f7a842c7edf3.pdf"}],"financialInterests":"No competing interests reported.","formattedTitle":"Determination of Boric acid by ICP-AES and ICP-MS in Caviars and Processed food","fulltext":[{"header":"1. Introduction","content":"\u003cp\u003eIn a modern society, consumers\u0026rsquo; preferences and needs for food have become more diverse after industrial development. In addition, a wide variety of food additives have been used for the purpose of improving quality, nutrition and customer preference. The purpose of additives greatly varies, but they are mostly used to improve the quality of the main material or keep it stable. Diverse supplements used for the stability ingredients in pharmaceuticals and even preservatives used in food belong to additives as well (KFDA The Guideline of Drug Excipients, \u003cspan citationid=\"CR14\" class=\"CitationRef\"\u003e2007\u003c/span\u003e). In the Korea Food Additives Code, 14 food preservatives are allowed, and the standards for the use of each preservative are stated. They are described as the criteria for the food on the Korean Food Standards Codex and Guidelines for Pharmaceutical Excipients. This study confirmed for standards and specifications of preservative in other country, such as USA (FDA food additive list and color additive list, \u003cspan citationid=\"CR9\" class=\"CitationRef\"\u003e2022\u003c/span\u003e), EU (EU Food Standards Agency, \u003cspan citationid=\"CR8\" class=\"CitationRef\"\u003e2012\u003c/span\u003e), and Japan (MHLW Ministry of Health, Labour and welfare, 2023). etc. Codex had designated 13 item of preservatives. When they were classified into systematic groups such as sorbic acid, benzoic acid, p-hydroxybenzoate and propionic acid (FMO Food and Agriculture Organization, \u003cspan citationid=\"CR10\" class=\"CitationRef\"\u003e2006\u003c/span\u003e, CODEX ALIMENTARIUS, \u003cspan citationid=\"CR5\" class=\"CitationRef\"\u003e2021\u003c/span\u003e), they were all used in USA, EU and Japan, There was a little difference in detail for each country.\u003c/p\u003e \u003cp\u003eIn the case of korea, food additives are substances with a clear purpose of use, and their use other than the intended purpose is prohibited, and they are always used in processing and manufacturing food. As a result, various problems arise during international trade due to different types of food additives, current status of designation, and standards for use in each country.\u003c/p\u003e \u003cp\u003eIn food, a food preservative is a chemical substance added to improve food preservation. It plays a role of antiseptic which inhibits the growth of bacteria and also controls mold growth. Currently, many countries have banned the use of boric acid as a food additive but in some Asian countries. In case of Hong-kong, boric acid is still used for noodle and fish ball as food additive. Boric acid and sodium tetraborate are authorized as food additive, in EU and the maximum permissible dose is limited to 4000 mg/kg (EU Official Journal of the European Union, \u003cspan citationid=\"CR6\" class=\"CitationRef\"\u003e2011\u003c/span\u003e). But boric acid is not authorized for use in Korea(Korean Food Code, \u003cspan citationid=\"CR15\" class=\"CitationRef\"\u003e2023\u003c/span\u003e, Korean Food Additives Code, \u003cspan citationid=\"CR16\" class=\"CitationRef\"\u003e2021\u003c/span\u003e). and the analytical method of boric acid in foods has not been reported in Korea. For the analysis of boric acid and sodium tetraborate in food, after derivatization using triethanolamine, analysis method using GC-MS(Li-Min Zeng, Hao-Yang Wang, Yin-Long Guo, 2010), 11B-NMR analysis using Polarizing Plates(Seiya kunimasa, Makoto Tasaki, Hiromi Yamada, Shinji Morimoto, Manabu Togal, 2012), qualitative analysis method applying Curcumin paper method and 2-ethyl-1,3- A spectrophotometric analysis method using hexanediol/chloroform (EHD) solution has been reported (Yoshida M, Watabiki T, Ishida N, \u003cspan citationid=\"CR22\" class=\"CitationRef\"\u003e1989\u003c/span\u003e). MC-ICPMS and NTIMS were used to analyze boron isotopes in boric acid, seawater, and marine CaCO3 samples(Gavin L. Foster, B\u0026auml;rbel H\u0026ouml;nisch, Guillaume Paris, Gary S. Dwyer, James W.B. Rae, Tim Elliott, J\u0026eacute;r\u0026ocirc;me Gaillardet, N. Gary Hemming, Pascale Louvat, Avner Vengosh, 2013).\u003c/p\u003e \u003cp\u003eHowever, these analysis methods require a lot of time and money for qualitative and quantitative analysis of samples. According to the paper, the content of boric acid in food is 130\u0026ndash;926 \u0026micro;g/mL in fish ball, 161\u0026ndash;489 \u0026micro;g/mL in Kuey teow noodle, 918 ppm in agar-agar strips, 347 \u0026micro;g/mL in fresh prawn, and 819 \u0026micro;g/mL in mango (pickled). It was reported to be detected in various food samples (Ang Swi See, Abu Bakar Salleh, Fatimah Abu Bakar, Nor Azah Yusof, Ahmed Sahib Abdulamir and Lee Yook Heng, 2010, S Siti-Mizura, E S Tee and H E Ooi, 1991). Analyis of boron as boric acid in eye lotions using a sequential injection system (J. (Koos) F, van Staden, M.(Mutshutshu) Tsanwani, 2002). According to the reported AOAC Method, various sample preparation and analysis methods were used to analyze boric acid in the sample(AOAC official method 969.26, 2005; AOAC official method 990.34, 2005, AOAC official method 972.19, 2005, AOAC official method 975.26, 2005).\u003c/p\u003e \u003cp\u003eIn not allowed countries such as Korea, safety management is difficult because there is no analysis method for products distributed domestically and internationally. Thus, in this study the sample preparation and analysis method of boric acid in Caviar and processed food were established and validity was verified. In addition, using the established analysis method, analysis time, cost and low concentration analysis became possible. As well as, It is expected that it will be a good research data for setting standard specifications and safety management of boric acid.\u003c/p\u003e"},{"header":"2. Materials and Methods","content":"\u003cdiv id=\"Sec3\" class=\"Section2\"\u003e \u003ch2\u003e2.1. Reagents and material\u003c/h2\u003e \u003cp\u003eStandard boric acid(Assay 99.999%) and sodium tetraborate (Assay 99.9%) was obtained from Sigma-Aldrich (St Louis, MO, USA). Boron CRM standard solution (Lot : 214065136) was purchased from Accustandard (New Haven, CT, USA), Nitric acid, Hydrogen peroxide and ammonium hydroxide. The study has obtained from Sigma-Aldrich (St Louis, MO, USA). Ultrapure deionized water (resistivity\u0026thinsp;\u0026gt;\u0026thinsp;18 MΩ\u0026middot;cm) from a Milli-Q system (Millipore, Billerica, MA, USA) was used for all experiments.\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec4\" class=\"Section2\"\u003e \u003ch2\u003e2.2 Instrument and analysis conditions\u003c/h2\u003e \u003cp\u003eThe ICP apparatus was a spectro SPECTRO BLUE ICP-AES system (USA) equipped with axial, radial and twin interface. The ICP-AES was consisted of Quartz nebulizer, Quartz spray chamber and Quartz injector. The analysis condition by ICP-AES were Nebulizer gas flow 0.8 L/min, coolant gas flow 13.0 L/min, Auxiliary gas flow 0.8 L/min, Plasma power 1400 W, and Pump speed 30 RPM. The wavelength were 182.641, 249.677 and 249.773nm. 249.773 nm was quantitative wavelength. 182.641 nm and 249.677 nm were qualitative wavelength(Table\u0026nbsp;\u003cspan refid=\"Tab1\" class=\"InternalRef\"\u003e1\u003c/span\u003e). ICP-MS was purchased from Therm Fisher Scientific in USA (Thermo Finnigan, San Jose, CA, USA). The analysis condition by ICP-AES were RF power 1550 W, PFA Nebulizer 100 uL/min, Nebulizer gas 0.79 L/min, Auxiliary gas 0.80 L/min, Cool gas 14 L/min and Sample uptake rate 0.25 mL/min. The Selected isotopes(m/z) was 11(11B). The detailed operating conditions of ICP-MS were optimized and were summarized in Table\u0026nbsp;\u003cspan refid=\"Tab2\" class=\"InternalRef\"\u003e2\u003c/span\u003e.\u003c/p\u003e \u003cp\u003e \u003cdiv class=\"gridtable\"\u003e\u003ctable float=\"Yes\" id=\"Tab1\" border=\"1\"\u003e \u003ccaption language=\"En\"\u003e \u003cdiv class=\"CaptionNumber\"\u003eTable 1\u003c/div\u003e \u003cdiv class=\"CaptionContent\"\u003e \u003cp\u003eICP conditions for boric acid quantification\u003c/p\u003e \u003c/div\u003e \u003c/caption\u003e \u003ccolgroup cols=\"2\"\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c1\" colnum=\"1\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c2\" colnum=\"2\"\u003e\u003c/div\u003e \u003cthead\u003e \u003ctr\u003e \u003cth align=\"left\" colname=\"c1\"\u003e \u003cp\u003eInstrument parameters\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c2\"\u003e \u003cp\u003eCondition\u003c/p\u003e \u003c/th\u003e \u003c/tr\u003e \u003c/thead\u003e \u003ctbody\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e- Quartz nebulizer\u003c/p\u003e \u003cp\u003e- Quartz spray chamber\u003c/p\u003e \u003cp\u003e- Quartz injector\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e\u0026nbsp;\u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eNebulizer gas flow\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e0.8 L/min\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eCoolant gas flow\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e13.0 L/min\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eAuxiliary gas flow\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e0.8 L/min\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003ePlasma power\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e1400 W\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003ePump speed\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e30 RPM.\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eWavelength\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e\u003cb\u003e182.641, 249.677\u003c/b\u003e, \u003cspan type=\"BoldUnderline\" class=\"BoldUnderline\" name=\"Emphasis\"\u003e249.773nm\u003c/span\u003e\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003c/tbody\u003e \u003c/colgroup\u003e \u003c/table\u003e\u003c/div\u003e \u003c/p\u003e \u003cp\u003e \u003cdiv class=\"gridtable\"\u003e\u003ctable float=\"Yes\" id=\"Tab2\" border=\"1\"\u003e \u003ccaption language=\"En\"\u003e \u003cdiv class=\"CaptionNumber\"\u003eTable 2\u003c/div\u003e \u003cdiv class=\"CaptionContent\"\u003e \u003cp\u003eICP-MS conditions for boric acid quantification\u003c/p\u003e \u003c/div\u003e \u003c/caption\u003e \u003ccolgroup cols=\"3\"\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c1\" colnum=\"1\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c2\" colnum=\"2\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c3\" colnum=\"3\"\u003e\u003c/div\u003e \u003cthead\u003e \u003ctr\u003e \u003cth align=\"left\" colspan=\"2\" nameend=\"c2\" namest=\"c1\"\u003e \u003cp\u003eInstrument parameters\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c3\"\u003e \u003cp\u003eCondition\u003c/p\u003e \u003c/th\u003e \u003c/tr\u003e \u003c/thead\u003e \u003ctbody\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eRF power\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e\u0026nbsp;\u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e1550 W\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eNebulizer\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003ePFA Nebulizer\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e100 uL/min\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eArgon gas flow rate\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003eNebulizer gas\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e0.79 L/min\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e\u0026nbsp;\u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003eAuxiliary gas\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e0.80 L/min\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e\u0026nbsp;\u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003eCool gas\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e14 L/min\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eSample uptake rate\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e\u0026nbsp;\u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e0.25 mL/min\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eSelected isotopes(m/z)\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e\u0026nbsp;\u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e11(\u003csup\u003e11\u003c/sup\u003eB)\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003c/tbody\u003e \u003c/colgroup\u003e \u003c/table\u003e\u003c/div\u003e \u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec5\" class=\"Section2\"\u003e \u003ch2\u003e2.3 Sample preparation\u003c/h2\u003e \u003cp\u003eThe study has subjected to microwave-assisted acid digestion to obtain the fully decomposed sample blend and procedure blank solutions. In optimized conditions for the microwave assisted acid digestion, CEM(MARS model) Ultrawave microwave digestion system CEM(MARS6, NC, USA) was used, which is equipped with 15 small digestion vessels in a single reaction chamber. The study has weighed 0.5g of caviar for ICP analysis. Immediately, nitric acid 5mL and Hydrogen peroxide 2mL were added to 0.5 g of sample in vessel. 5 mL of HNO\u003csub\u003e3\u003c/sub\u003e (about 65%) was added to each small digestion vessel. The digestion vessels were inserted into a Teflon outer bath, and 130 mL of deionized water and 2 mL of H\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e2\u003c/sub\u003e were added to the outer bath. The small digestion vessels with caps were heated in a closed microwave reaction chamber. Then, the reaction chamber temperature was maintained at 180\u0026deg;C for 30 min. The study has filled up by distilled water in 50mL volumn flask for analysis. Finally, the study has measured of boric acid in caviar by ICP and ICP-MS.\u003c/p\u003e \u003c/div\u003e"},{"header":"3. Result and discussion","content":"\u003cdiv id=\"Sec7\" class=\"Section2\"\u003e\n \u003ch2\u003e3.1 Optimization of the ICP-OES and ICP-MS method\u003c/h2\u003e\n \u003cp\u003eThe study has determinated for boron by ICP-AES in caviars. Firstly, we found wavelength analysis of boron in caviar by ICP-AES. we have the wavelength that are 182.641, 279.677 and 249.773 nm. The correlation coefficients for all calibration curves were at least 0.999 in microwave wavelength of three. The linearity range of the standard curves was 0.5\u0026ndash;10 \u0026micro;g/mL. The BEC value of boron is measured 0.02 to 0.03ppm by ICP-AES(Fig. \u003cspan class=\"InternalRef\"\u003e1\u003c/span\u003e).\u003c/p\u003e\n \u003cp\u003eWe are selected one of three wavelenght for measure of boron by ICP-AES. The wavelength is 249.773nm for quantitative analysis. The 182.641 and 279.677nm are used for wavelength of qualitative analysis(Fig. \u003cspan class=\"InternalRef\"\u003e2\u003c/span\u003e). It is allowed as a preservative in Europe, such as boric acid and sodium tetraborate. Boric acid and sodium tetraborate have been managing as boric acid in Europe. As well, boric acid has been allowing as boron. The study has purchased boron standard solution in Accustandard. The concentration of boron standard solution is 1000 \u0026micro;g/mL. The study has measured boron in boric acid and sodium tetraborate by ICP-AES. As a result, we confirmed same concentration of boron in standard solution.\u003c/p\u003e\n\u003c/div\u003e\n\u003cdiv id=\"Sec8\" class=\"Section2\"\u003e\n \u003ch2\u003e3.2 Sample preparation\u003c/h2\u003e\n \u003cp\u003eThe study has subjected to microwave-assisted acid digestion to obtain the fully decomposed sample blend and procedure blank solutions. In optimized conditions for the microwave assisted acid digestion, CEM(MARS model) Ultrawave microwave digestion system (CEM(MARS6, NC, USA) was used, which is equipped with 15 small digestion vessels in a single reaction chamber. The study has weighed 0.5g of caviar for ICP analysis. Immediately, nitric acid 5mL and Hydrogen peroxide 2mL were added to 0.5 g of sample in vessel. 5 mL of HNO3 (about 65%) was added to each small digestion vessel. The digestion vessels were inserted into a Teflon outer bath, and 130 mL of deionized water and 2 mL of H\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e2\u003c/sub\u003e were added to the outer bath. The small digestion vessels with caps were heated in a closed microwave reaction chamber. Then, the reaction chamber temperature was maintained at 180\u0026deg;C for 30 min. The study has filled up by distilled water in 50mL volumn flask for analysis. Finally, the study has measured of boric acid in caviar with ICP(Fig. \u003cspan class=\"InternalRef\"\u003e3\u003c/span\u003e).\u003c/p\u003e\n\u003c/div\u003e\n\u003cdiv id=\"Sec9\" class=\"Section2\"\u003e\n \u003ch2\u003e3.3 Method validation\u003c/h2\u003e\n \u003cp\u003eValidation method was conducted by means of the following parameters: linearity, matrix effect, precision and accuracy, LOD \u0026amp; LOQ, Uncertainty of measurement and Inter-lab reproducibility. Linearity was developed with matrix-effect calibration via analyzing sample of caviar. The calibration curve was confirmed from 0.5 \u0026micro;g/mL to 10 \u0026micro;g/mL with a satisfactory correlation coefficient (\u0026gt;\u0026thinsp;0.999).\u003c/p\u003e\n \u003cdiv id=\"Sec10\" class=\"Section3\"\u003e\n \u003ch2\u003e3.3.1 Selectivity \u0026amp; specification\u003c/h2\u003e\n \u003cp\u003eThe Selectivity and specification should be demonstrated by the analysis of representative blank matrix materials from multiple sources. The study has measured the blank sample that is collected for identify selectivity and specification. The study has confirmed no interference so it has acquired selectivity and specification.\u003c/p\u003e\n \u003c/div\u003e\n \u003cdiv id=\"Sec11\" class=\"Section3\"\u003e\n \u003ch2\u003e3.3.2 Linearity\u003c/h2\u003e\n \u003cp\u003eThe accuracy of boron from spiked sample at levels of 0.5\u0026ndash;10.0 \u0026micro;g/mL ranged from 98.9 to 100.6% with RSD between 0.1 and 1.3%. The correlation coefficients for calibration curve was at least 0.999 in sample(Table \u003cspan class=\"InternalRef\"\u003e3\u003c/span\u003e).\u003c/p\u003e\n \u003cdiv class=\"gridtable\"\u003e\u0026nbsp;\u003ctable id=\"Tab3\" border=\"1\"\u003e\n \u003ccaption language=\"En\"\u003e\n \u003cdiv class=\"CaptionNumber\"\u003eTable 3\u003c/div\u003e\n \u003cdiv class=\"CaptionContent\"\u003e\n \u003cp\u003eLinearity of boron by ICP-AES\u003c/p\u003e\n \u003c/div\u003e\n \u003c/caption\u003e\n \u003cthead\u003e\n \u003ctr\u003e\n \u003cth align=\"left\" rowspan=\"2\"\u003e\u0026nbsp;\u003c/th\u003e\n \u003cth align=\"left\" colspan=\"5\"\u003e\n \u003cp\u003eConc.(\u0026micro;g/mL, n\u0026thinsp;=\u0026thinsp;3)\u003c/p\u003e\n \u003c/th\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003cth align=\"left\"\u003e\n \u003cp\u003e0.5\u003c/p\u003e\n \u003c/th\u003e\n \u003cth align=\"left\"\u003e\n \u003cp\u003e1\u003c/p\u003e\n \u003c/th\u003e\n \u003cth align=\"left\"\u003e\n \u003cp\u003e2\u003c/p\u003e\n \u003c/th\u003e\n \u003cth align=\"left\"\u003e\n \u003cp\u003e5\u003c/p\u003e\n \u003c/th\u003e\n \u003cth align=\"left\"\u003e\n \u003cp\u003e10\u003c/p\u003e\n \u003c/th\u003e\n \u003c/tr\u003e\n \u003c/thead\u003e\n \u003ctbody\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e1 day\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e0.49\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e1.00\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e2.00\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e5.05\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e9.97\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e2 day\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e0.49\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e0.98\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e2.02\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e5.01\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e9.99\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e3 day\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e0.50\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e0.98\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e2.01\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e5.01\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e9.99\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eMean\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e0.49\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e0.99\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e2.01\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e5.03\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e9.99\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003ePrecision (%)\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e1.3\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e1.3\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e0.6\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e0.5\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e0.1\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eAccuracy (%)\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e99.0\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e98.9\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e100.5\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e100.6\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e99.9\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003c/tbody\u003e\n \u003c/table\u003e\n \u003c/div\u003e\n \u003c/div\u003e\n \u003cdiv id=\"Sec12\" class=\"Section3\"\u003e\n \u003ch2\u003e3.3.3 Precision and accuracy of Intra-day \u0026amp; inter-day\u003c/h2\u003e\n \u003cp\u003eThe results of the boron precision and accuracy study are summarized in Tables 13 and 14. The spiking levels chosen for the precision and accuracy studies were 0.5, 2.0, and 10.0 ppm in matrices for all analyte. The precision of boron analysis was estimated using the RSD for both intra-day and inter-day. For all test samples, the RSDs of intra-day and inter-day precision ranged from 0.4 to 0.6% and 0.5 to 2.1%. Additionally, the study has confirmed the accuracy of intra-day and inter-day ranged from 99.1 to 100.6% and 96.8 to 100.2% (Table \u003cspan class=\"InternalRef\"\u003e4\u003c/span\u003e, \u003cspan class=\"InternalRef\"\u003e5\u003c/span\u003e).\u003c/p\u003e\n \u003cdiv class=\"gridtable\"\u003e\u0026nbsp;\u003ctable id=\"Tab4\" border=\"1\"\u003e\n \u003ccaption language=\"En\"\u003e\n \u003cdiv class=\"CaptionNumber\"\u003eTable 4\u003c/div\u003e\n \u003cdiv class=\"CaptionContent\"\u003e\n \u003cp\u003ePrecision and accuracy of Intra-day and Intra-day by ICP-AES\u003c/p\u003e\n \u003c/div\u003e\n \u003c/caption\u003e\n \u003cthead\u003e\n \u003ctr\u003e\n \u003cth align=\"left\" rowspan=\"2\"\u003e\u0026nbsp;\u003c/th\u003e\n \u003cth align=\"left\" colspan=\"3\"\u003e\n \u003cp\u003eConc. (\u0026micro;g/mL,n\u0026thinsp;=\u0026thinsp;3)\u003c/p\u003e\n \u003c/th\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003cth align=\"left\"\u003e\n \u003cp\u003e0.5\u003c/p\u003e\n \u003c/th\u003e\n \u003cth align=\"left\"\u003e\n \u003cp\u003e2.0\u003c/p\u003e\n \u003c/th\u003e\n \u003cth align=\"left\"\u003e\n \u003cp\u003e10.0\u003c/p\u003e\n \u003c/th\u003e\n \u003c/tr\u003e\n \u003c/thead\u003e\n \u003ctbody\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003en\u0026thinsp;=\u0026thinsp;1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e0.50\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e2.00\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e10.02\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003en\u0026thinsp;=\u0026thinsp;2\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e0.50\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e2.01\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e10.05\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003en\u0026thinsp;=\u0026thinsp;3\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e0.49\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e2.03\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e10.11\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eMean\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e0.50\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e2.01\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e10.06\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003ePrecision(%)\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e0.6\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e0.6\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e0.4\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eAccuracy(%)\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e99.1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e100.6\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e100.6\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003c/tbody\u003e\n \u003c/table\u003e\n \u003c/div\u003e\n \u003cdiv class=\"gridtable\"\u003e\n \u003cdiv align=\"char\" class=\"colspec\"\u003e\u003cbr\u003e\u003c/div\u003e\u0026nbsp;\u003ctable id=\"Tab5\" border=\"1\"\u003e\n \u003ccaption language=\"En\"\u003e\n \u003cdiv class=\"CaptionNumber\"\u003eTable 5\u003c/div\u003e\n \u003cdiv class=\"CaptionContent\"\u003e\n \u003cp\u003ePrecision and accuracy of Inter-day by ICP-AES\u003c/p\u003e\n \u003c/div\u003e\n \u003c/caption\u003e\n \u003cthead\u003e\n \u003ctr\u003e\n \u003cth align=\"left\" rowspan=\"2\"\u003e\u0026nbsp;\u003c/th\u003e\n \u003cth align=\"left\" colspan=\"3\"\u003e\n \u003cp\u003eConc. (\u0026micro;g/mL,n\u0026thinsp;=\u0026thinsp;3)\u003c/p\u003e\n \u003c/th\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003cth align=\"left\"\u003e\n \u003cp\u003e0.5\u003c/p\u003e\n \u003c/th\u003e\n \u003cth align=\"left\"\u003e\n \u003cp\u003e2.0\u003c/p\u003e\n \u003c/th\u003e\n \u003cth align=\"left\"\u003e\n \u003cp\u003e10.0\u003c/p\u003e\n \u003c/th\u003e\n \u003c/tr\u003e\n \u003c/thead\u003e\n \u003ctbody\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e1 day\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e0.50\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e2.01\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e10.10\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e2 day\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e0.48\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e1.99\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e10.00\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e3 day\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e0.48\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e1.99\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e9.90\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eMean\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e0.48\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e2.00\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e10.02\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003ePrecision(%)\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e2.1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e0.5\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e0.6\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eAccuracy(%)\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e96.8\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e100.0\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e100.2\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003c/tbody\u003e\n \u003c/table\u003e\n \u003c/div\u003e\n \u003c/div\u003e\n \u003cdiv id=\"Sec13\" class=\"Section3\"\u003e\n \u003ch2\u003e3.3.4 LOD \u0026amp; LOQ\u003c/h2\u003e\n \u003cp\u003eThe study has used ICP-AES in order to calculate LOD and LOQ. As well, the study has checked S/N ratio of boron in matrix. The study has calculated MDL using Environmental Protection Agency (EPA) method for detection of MDL (40 CFR Part 136. APPENDEX B, revision 1.11). For ICP-AES, the LOD and LOQ of boron were 0.03 \u0026micro;g/mL and 0.1 \u0026micro;g/mL.\u003c/p\u003e\n \u003c/div\u003e\n \u003cdiv id=\"Sec14\" class=\"Section3\"\u003e\n \u003ch2\u003e3.3.5 Result of recovery\u003c/h2\u003e\n \u003cp\u003eThe recoveries of boron from spiked samples at levels of 0.5, 2 and 10.0 \u0026micro;g/mL ranged from 98.0 to 102.0% with RSDs between 0.1 and 0.4%(Table \u003cspan class=\"InternalRef\"\u003e6\u003c/span\u003e).\u003c/p\u003e\n \u003cdiv class=\"gridtable\"\u003e\u0026nbsp;\u003ctable id=\"Tab6\" border=\"1\"\u003e\n \u003ccaption language=\"En\"\u003e\n \u003cdiv class=\"CaptionNumber\"\u003eTable 6\u003c/div\u003e\n \u003cdiv class=\"CaptionContent\"\u003e\n \u003cp\u003eThe result of recovery for boric acid\u003c/p\u003e\n \u003c/div\u003e\n \u003c/caption\u003e\n \u003cthead\u003e\n \u003ctr\u003e\n \u003cth align=\"left\" rowspan=\"2\"\u003e\n \u003cp\u003eConc.(\u0026micro;g/mL)\u003c/p\u003e\n \u003c/th\u003e\n \u003cth align=\"left\" colspan=\"3\"\u003e\n \u003cp\u003eDetected value(\u0026micro;g/mL)\u003c/p\u003e\n \u003c/th\u003e\n \u003cth align=\"left\" rowspan=\"2\"\u003e\n \u003cp\u003eMean\u003c/p\u003e\n \u003c/th\u003e\n \u003cth align=\"left\" rowspan=\"2\"\u003e\n \u003cp\u003eCV(%)\u003c/p\u003e\n \u003c/th\u003e\n \u003cth align=\"left\" rowspan=\"2\"\u003e\n \u003cp\u003eRecovery(%)\u003c/p\u003e\n \u003c/th\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003cth align=\"left\"\u003e\n \u003cp\u003en\u0026thinsp;=\u0026thinsp;1\u003c/p\u003e\n \u003c/th\u003e\n \u003cth align=\"left\"\u003e\n \u003cp\u003en\u0026thinsp;=\u0026thinsp;2\u003c/p\u003e\n \u003c/th\u003e\n \u003cth align=\"left\"\u003e\n \u003cp\u003en\u0026thinsp;=\u0026thinsp;3\u003c/p\u003e\n \u003c/th\u003e\n \u003c/tr\u003e\n \u003c/thead\u003e\n \u003ctbody\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e0.5\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e0.48\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e0.50\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e0.50\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e0.49\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e0.1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e98.0\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e2.0\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e2.03\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e2.03\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e2.05\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e2.04\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e0.4\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e102.0\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e10.0\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e10.19\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e10.15\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e10.12\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e10.15\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e0.3\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e101.5\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003c/tbody\u003e\n \u003c/table\u003e\n \u003c/div\u003e\n \u003c/div\u003e\n \u003cdiv id=\"Sec15\" class=\"Section3\"\u003e\n \u003ch2\u003e3.3.6 Meauremetn of uncertainty\u003c/h2\u003e\n \u003cp\u003eTo assess the suitability of the analytical method for use in the laboratory, the uncertainty measurement of boron in caviar spiked with 203.1 mg/kg boron was estimated using the ICP-AES. The uncertainty in the measurements was identified and used as parameters to determine the combined standard uncertainty based on GUM (guide to the expression of uncertainty in measurement) and the Draft EURACHEM/CITAC Guide(EURACHEM., 2000, ISO., 2002). The final U, for a level of confidence of approximately 95% and considering a coverage factor of 2, was found to be 203.1\u0026thinsp;\u0026plusmn;\u0026thinsp;10.8 (mg/kg) for the ICP-AES method (Table \u003cspan class=\"InternalRef\"\u003e7\u003c/span\u003e).\u003c/p\u003e\n \u003cdiv class=\"gridtable\"\u003e\u0026nbsp;\u003ctable id=\"Tab7\" border=\"1\"\u003e\n \u003ccaption language=\"En\"\u003e\n \u003cdiv class=\"CaptionNumber\"\u003eTable 7\u003c/div\u003e\n \u003cdiv class=\"CaptionContent\"\u003e\n \u003cp\u003eExpanded uncertainty\u003csup\u003ea\u003c/sup\u003e of boron level using ICP-AES and 203.1 mg/kg in caviar\u003c/p\u003e\n \u003c/div\u003e\n \u003c/caption\u003e\n \u003cthead\u003e\n \u003ctr\u003e\n \u003cth align=\"left\"\u003e\n \u003cp\u003eParameters of Uncertainty\u003c/p\u003e\n \u003c/th\u003e\n \u003cth align=\"left\"\u003e\n \u003cp\u003eResult\u003c/p\u003e\n \u003c/th\u003e\n \u003cth align=\"left\"\u003e\n \u003cp\u003eUnit\u003c/p\u003e\n \u003c/th\u003e\n \u003c/tr\u003e\n \u003c/thead\u003e\n \u003ctbody\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eCertified Concentration\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e203.1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003emg/kg\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eThe result of uncertainty\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e203.1\u0026thinsp;\u0026plusmn;\u0026thinsp;10.8\u003c/p\u003e\n \u003cp\u003e(k\u0026thinsp;=\u0026thinsp;2, 95% confidence level)\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003emg/kg\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eExpanded uncertainty(U)\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e10.82\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003emg/kg\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eCoverage factor(k)\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e2\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003edimensionless unit\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003edegrees of freedom,(veff)\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e19\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003edimensionless unit\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eCombined Standard Uncertainty (u\u003csub\u003ec\u003c/sub\u003e)\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e5.41\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003emg/kg\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eCombined relative Standard Uncertainty\u003c/p\u003e\n \u003cp\u003e(u\u003csub\u003er\u003c/sub\u003e/r)\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e0.027\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003edimensionless unit\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003c/tbody\u003e\n \u003c/table\u003e\n \u003c/div\u003e\n \u003c/div\u003e\n\u003c/div\u003e\n\u003cdiv id=\"Sec16\" class=\"Section2\"\u003e\n \u003ch2\u003e3.4 Result of sample analysis\u003c/h2\u003e\n \u003cp\u003eThe method developed in this study was used to monitor the presence of boric acid and sodium tetraborate residue levels in caviars including various roe samples in domestic and foreign markets. A total of 104 real samples of caviars and various roe were collected from grocery markets in South Korea (39), and the Europe (65). Of the 104 analyzed samples, 33 contained 46.0\u0026thinsp;~\u0026thinsp;3942.2 mg/kg boric acid. Boric acid and sodium tetraborate were not found in any of the samples such as caviar, salted pollack roe and Flying Fish Roe. The boric acid concentrations were under the legal limit of 4000 mg/kg as specified in EU (Table \u003cspan class=\"InternalRef\"\u003e8\u003c/span\u003e).\u003c/p\u003e\n \u003cdiv class=\"gridtable\"\u003e\u0026nbsp;\u0026nbsp;\u003ctable id=\"Tab8\" border=\"1\"\u003e\n \u003ccaption language=\"En\"\u003e\n \u003cdiv class=\"CaptionNumber\"\u003eTable 8\u003c/div\u003e\n \u003cdiv class=\"CaptionContent\"\u003e\n \u003cp\u003eThe determination of boric acid by ICP-AES in caviars. * As boric acid : Boric acid conc.(mg/kg)\u0026thinsp;=\u0026thinsp;Boron x Mw(Boric acid)\u0026thinsp;\u0026divide;\u0026thinsp;MW(Boron), N.D : Not detection\u003c/p\u003e\n \u003c/div\u003e\n \u003c/caption\u003e\n \u003cthead\u003e\n \u003ctr\u003e\n \u003cth align=\"left\"\u003e\n \u003cp\u003eMethod of collection\u003c/p\u003e\n \u003c/th\u003e\n \u003cth align=\"left\"\u003e\n \u003cp\u003eName of\u003c/p\u003e\n \u003cp\u003esample\u003c/p\u003e\n \u003c/th\u003e\n \u003cth align=\"left\"\u003e\n \u003cp\u003eThe number\u003c/p\u003e\n \u003cp\u003eof sample\u003c/p\u003e\n \u003c/th\u003e\n \u003cth align=\"left\"\u003e\n \u003cp\u003eThe number\u003c/p\u003e\n \u003cp\u003eof detection\u003c/p\u003e\n \u003c/th\u003e\n \u003cth align=\"left\"\u003e\n \u003cp\u003eRange\u003c/p\u003e\n \u003cp\u003e(mg/kg)\u003c/p\u003e\n \u003c/th\u003e\n \u003cth align=\"left\"\u003e\n \u003cp\u003eType of food\u003c/p\u003e\n \u003c/th\u003e\n \u003c/tr\u003e\n \u003c/thead\u003e\n \u003ctbody\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\" rowspan=\"2\"\u003e\n \u003cp\u003eDomestic market in Korea\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eCaviar\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e7\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e2\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e3106.2\u003c/p\u003e\n \u003cp\u003e~\u0026thinsp;3549.2\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\u0026nbsp;\u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eVarious roe\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e32\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e0\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eND\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eHerring Roe, Lumpfish Roe, Soused roe, noodles, Flying Fish Roe, etc.\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\" rowspan=\"2\"\u003e\n \u003cp\u003eForeign market in Europe\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eCaviar\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e31\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e31\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e46.0\u003c/p\u003e\n \u003cp\u003e~ \u0026nbsp;3942.2\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\u0026nbsp;\u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eVarious roe\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e24\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e0\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eND\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eHerring Roe,\u003c/p\u003e\n \u003cp\u003eLumpfish Roe,\u003c/p\u003e\n \u003cp\u003eSalmon Roe,\u003c/p\u003e\n \u003cp\u003eTrout roe,\u003c/p\u003e\n \u003cp\u003eFlying Fish Roe etc.\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003c/tbody\u003e\n \u003c/table\u003e\n \u003c/div\u003e\n\u003c/div\u003e\n\u003cp\u003e* As boric acid : Boric acid conc.(mg/kg) = Boron x Mw(Boric acid) \u0026divide; MW(Boron), N.D : Not detection\u0026nbsp;\u003c/p\u003e"},{"header":"4. Conclusions","content":"\u003cp\u003eThe study has determinated for boron by ICP-AES in caviars. Firstly, we found wavelength analysis of boron in caviar by ICP-AES. we have the wavelength that are 182.641, 279.677 and 249.773 nm. The correlation coefficients for all calibration curves were at least 0.999 in microwave wavelength of three. The linearity range of the standard curves was 0.5\u0026ndash;10 \u0026micro;g/mL. The BEC value of boron is measured 0.02 to 0.03ppm by ICP-AES.\u003c/p\u003e \u003cp\u003eThe study has purchased boron standard solution in Accustandard. The concentration of boron standard solution is 1000\u0026micro;g/mL. The study has measured boron in boric acid and sodium tetraborate by ICP-AES. To assess the suitability of the analytical method for use in the laboratory, the uncertainty measurement of boron in caviar spiked with 203.1\u0026thinsp;\u0026plusmn;\u0026thinsp;10.8 mg/kg boron was estimated using the ICP-AES. The study has subjected to microwave-assisted acid digestion to obtain the fully decomposed sample blend and procedure blank solutions.\u003c/p\u003e \u003cp\u003eA total of 104 real samples of caviars and various roe were collected from grocery markets in South Korea (39), and the Europe (65). Of the 104 analyzed samples, 33 contained 46.0\u0026thinsp;~\u0026thinsp;3942.2 mg/kg boric acid. Boric acid and sodium tetraborate were not found in any of the samples such as caviar, salted pollack roe and Flying Fish Roe. The boric acid concentrations were under the legal limit of 4000 mg/kg as specified in EU (Table\u0026nbsp;17).\u003c/p\u003e"},{"header":"Declarations","content":"\u003ch2\u003eAuthor Contribution\u003c/h2\u003e\u003cp\u003ehe authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.\u003c/p\u003e\u003ch2\u003eAcknowledgements\u003c/h2\u003e \u003cp\u003eThis research was supported by a grant(14162MFDS971) the Ministry of Food and Drug Safety in 2014.\u003c/p\u003e"},{"header":"References","content":"\u003col\u003e\n \u003cli\u003eAOAC Official Method 969.26 AOAC. (2005). Boric Acid in Caviar Spectrophotometric Method.\u003c/li\u003e\n \u003cli\u003eAOAC Official Method 970.34 AOAC. (2005).\u0026nbsp;Boric Acid in Caviar Titrimetric Method.\u003c/li\u003e\n \u003cli\u003eAOAC Official Method 972.19 AOAC. (2005).\u0026nbsp;Boric Acid in Food Atomic Absorption Spectro photometric Method.\u003c/li\u003e\n \u003cli\u003eAOAC Official Method 975.26 AOAC. (2005).\u0026nbsp;Boric Acid in Food Emission Spectroscopic Method.\u003c/li\u003e\n \u003cli\u003eCODEX ALIMENTARIUS.(2021). General Standard for Food Additives(GSFA).\u003c/li\u003e\n \u003cli\u003eEU Official Journal of the European Union.(2011). COMMISSION REGULATION (EU) No 1129/2011 of 11 November 2011 L 295 p 115.\u0026nbsp;\u003c/li\u003e\n \u003cli\u003eEURACHEM. (2000). Quantifying uncertainty in analytical measurement (2nd ed). London: Eurachem.\u003c/li\u003e\n \u003cli\u003eEU Food Standards Agency(2012),\u0026nbsp;Current EU approved additives and their E Numbers.\u003c/li\u003e\n \u003cli\u003eFDA food additive list and color additive list.(2022). FDA (http://www.fda.gov) CFR eCFR(http://www.ecfr.gov/cgi-bin/).\u003c/li\u003e\n \u003cli\u003eFMO Food and Agriculture Organization. (2006). FAO JECFA Monographs Combined compendium of food additive specifications.\u003c/li\u003e\n \u003cli\u003eFoster, G.L., H\u0026ouml;nisch, B., Paris, G., Dwyer, G.S., Rae, J.W.B., Elliott, T., J\u0026eacute;r\u0026ocirc;me Gaillardet, J., Gary Hemming, N., Louvat, P., Vengosh, A. (2013). Interlaboratory comparison of boron isotope analyses of boric acid, seawater and marine CaCO3 by MC-ICPMS and NTIMS. \u003cem\u003eChemical Geology\u003c/em\u003e, 358, 1-14.\u003c/li\u003e\n \u003cli\u003eISO. (2002). Guide to the expression of uncertainty in measurements. International Organization for Standardization (ISO), Geneva Switzerland.\u003c/li\u003e\n \u003cli\u003eKunimasa, S., Tasaki, M., Yamada, H., Morimoto, S., Togal, M.(2012).\u0026nbsp;Development of a Quantitative Analysis Method for Unreacted Boric Acid in Polarizing Plates. \u003cem\u003eSumitomo Gagaku R\u0026amp;D Report\u003c/em\u003e, 1-12.\u003c/li\u003e\n \u003cli\u003eKFDA The Guideline of Drug Excipients. (2007): Ministry of Food and Drug Safety, Osong, Korea.\u0026nbsp;\u003c/li\u003e\n \u003cli\u003eKorean Food Code. (2023). 8. General test methods, Ministry of Food and Drug Safety, Osong, Korea.\u003c/li\u003e\n \u003cli\u003eKorean Food Additives Code. (2021). III.\u0026nbsp;Standards and Specification for Food Contact Surface Sanitizing Solutions, Ministry of Food and Drug Safety, Osong, Korea.\u003c/li\u003e\n \u003cli\u003eMHLW Ministry of Health, Labour and welfare.(2023). 4. The Japan Food Chemical \u0026nbsp;Research Foundation Standards for Use of Food Additives.\u003c/li\u003e\n \u003cli\u003eSee, A.S., Salleh, A. B., Bakar, F.A., Yusof, N. A., Abdulamir, A.S., Heng, L.Y. (2010). Risk and Health Effect of Boric Acid. \u003cem\u003eAmerican Journal of Applied Sciences\u003c/em\u003e, 7(5), 620-627.\u003c/li\u003e\n \u003cli\u003eSiti-Mizura, S., Tee, E.S., Ooi, H.E. (1991). Determination of Boric Acid in Foods: Comparative Study of Three Methods. \u003cem\u003eJ Sci Food Agric\u003c/em\u003e, 55, 261-268.\u0026nbsp;\u003c/li\u003e\n \u003cli\u003eVan Staden, J.F., M.(Mutshutshu) Tsanwani, M. ( 2002).\u0026nbsp;Determination of boron as boric acid in eye lotions using a sequential injection system. \u003cem\u003eTalanta\u003c/em\u003e, 58, 1103-1108.\u003c/li\u003e\n \u003cli\u003eYoshida, M., Watabiki, T., Ishida, N.(1989). Spectrophotometric determination of boric acid by the curcumin method. \u003cem\u003eThe Japanese Journal of Legal Medicine,\u003c/em\u003e 43(6), 490-496.\u003c/li\u003e\n \u003cli\u003eZeon, L.M., Wang, H.Y., Guo, Y. L.(2010). Fast quantitative analysis of boric acid by gas chromatography-mass spectrometry coupled with a simple and selective derivatization reaction using triethanolamine. \u003cem\u003eJ Am Soc Mass Spectrum,\u003c/em\u003e 21, 482-485.\u003c/li\u003e\n\u003c/ol\u003e"}],"fulltextSource":"","fullText":"","funders":[],"hasAdminPriorityOnWorkflow":false,"hasManuscriptDocX":true,"hasOptedInToPreprint":true,"hasPassedJournalQc":"","hasAnyPriority":false,"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":"Boric acid, ICP-MS, Method validation, Caviars","lastPublishedDoi":"10.21203/rs.3.rs-4211245/v1","lastPublishedDoiUrl":"https://doi.org/10.21203/rs.3.rs-4211245/v1","license":{"name":"CC BY 4.0","url":"https://creativecommons.org/licenses/by/4.0/"},"manuscriptAbstract":"\u003cp\u003e. Boric acid is authorized as food additive in EU. However, it is not authorized for use in Korea. The analytical method of boric acid in foods has not been reported in Korea. In this study, an analytical method has been developed and validated for the determination of boric acid in caviars. We established the analytical assay for boric acid in caviars by Inductively Coupled Plasma Mass Spectrometry(ICP-MS). Caviar samples were digested in closed vessels made of PTFE in an Automatic Microwave Digestion System. We also performed a method validation including linearity, inter-day, intra-day, precision, accuracy, Limit of detection (LOD) and Limit of Quantitation(LOQ) and recovery. The calibration curve was obtained from 0.2 µg/mL to 10 µg/mL with a satisfactory correlation coefficient of 0.99. The LOD and LOQ were 0.04 µg/mL and 0.16 µg/mL. The recoveries of boric acid from spiked samples at levels of 0.5, 2 and 10 µg/mL ranged from 91.8 to 98.3% with relative standard deviation(RSD) between 0.4 and 2.4 %.\u003c/p\u003e","manuscriptTitle":"Determination of Boric acid by ICP-AES and ICP-MS in Caviars and Processed food","msid":"","msnumber":"","nonDraftVersions":[{"code":1,"date":"2024-04-16 10:20:42","doi":"10.21203/rs.3.rs-4211245/v1","editorialEvents":[{"type":"communityComments","content":0}],"status":"published","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}}],"origin":"","ownerIdentity":"ff02ad9b-c3e3-495f-93a9-501e9f94c51b","owner":[],"postedDate":"April 16th, 2024","published":true,"recentEditorialEvents":[],"rejectedJournal":[],"revision":"","amendment":"","status":"posted","subjectAreas":[],"tags":[],"updatedAt":"2024-04-29T19:29:11+00:00","versionOfRecord":[],"versionCreatedAt":"2024-04-16 10:20:42","video":"","vorDoi":"","vorDoiUrl":"","workflowStages":[]},"version":"v1","identity":"rs-4211245","journalConfig":"researchsquare"},"__N_SSP":true},"page":"/article/[identity]/[[...version]]","query":{"redirect":"/article/rs-4211245","identity":"rs-4211245","version":["v1"]},"buildId":"qtupq5eGEP_6zYnWcrvyt","isFallback":false,"isExperimentalCompile":false,"dynamicIds":[84888],"gssp":true,"scriptLoader":[]}