A. G. Polonevich, S. Leschev, V. A. Bulhakava, L. L. Belyshava
{"title":"高效液相色谱-质谱联用测定蜂蜜中阿米特拉兹的方法的建立与验证","authors":"A. G. Polonevich, S. Leschev, V. A. Bulhakava, L. L. Belyshava","doi":"10.29235/1561-8331-2022-58-4-387-397","DOIUrl":null,"url":null,"abstract":"Method for determination of the insecticide amitraz residual content in honey has been developed and validated. The method is selective, express and easy-to-perform. The technique is based on the extraction of amitraz from alkalized aqueous solutions of honey with n-hexane and quantitative determination by high-performance liquid chromatography with mass spectrometric detection. Validation was performed using three types of honey at three levels of amitraz application 6, 120 and 220 µg/kg. The limit of quantification was 0.9 µg/kg, the calibration curves were linear in the concentration range from 2.5 to 125.0 ng/mL (the corresponding analyte content in honey is from 5.0 to 250.0 µg/kg), relative values of the standard deviations of repeatability and within-laboratory reproducibility did not exceed 3.4 and 5.9 %, respectively, the bias values varied from –8.2 to 5.6 %, the expanded uncertainty estimates of the results ranged from 12 to 16 % (P = 0.95). Instrumental limit of quantification, overall efficiency of the process and robustness were also evaluated during the validation process.","PeriodicalId":20798,"journal":{"name":"Proceedings of the National Academy of Sciences of Belarus, Chemical Series","volume":"12 1","pages":""},"PeriodicalIF":0.0000,"publicationDate":"2022-11-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"1","resultStr":"{\"title\":\"Development and validation of the method for determination of amitraz in honey using high-performance liquid chromatography with mass spectrometric detection\",\"authors\":\"A. G. Polonevich, S. Leschev, V. A. Bulhakava, L. L. Belyshava\",\"doi\":\"10.29235/1561-8331-2022-58-4-387-397\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"Method for determination of the insecticide amitraz residual content in honey has been developed and validated. The method is selective, express and easy-to-perform. The technique is based on the extraction of amitraz from alkalized aqueous solutions of honey with n-hexane and quantitative determination by high-performance liquid chromatography with mass spectrometric detection. Validation was performed using three types of honey at three levels of amitraz application 6, 120 and 220 µg/kg. The limit of quantification was 0.9 µg/kg, the calibration curves were linear in the concentration range from 2.5 to 125.0 ng/mL (the corresponding analyte content in honey is from 5.0 to 250.0 µg/kg), relative values of the standard deviations of repeatability and within-laboratory reproducibility did not exceed 3.4 and 5.9 %, respectively, the bias values varied from –8.2 to 5.6 %, the expanded uncertainty estimates of the results ranged from 12 to 16 % (P = 0.95). Instrumental limit of quantification, overall efficiency of the process and robustness were also evaluated during the validation process.\",\"PeriodicalId\":20798,\"journal\":{\"name\":\"Proceedings of the National Academy of Sciences of Belarus, Chemical Series\",\"volume\":\"12 1\",\"pages\":\"\"},\"PeriodicalIF\":0.0000,\"publicationDate\":\"2022-11-29\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"1\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Proceedings of the National Academy of Sciences of Belarus, Chemical Series\",\"FirstCategoryId\":\"1085\",\"ListUrlMain\":\"https://doi.org/10.29235/1561-8331-2022-58-4-387-397\",\"RegionNum\":0,\"RegionCategory\":null,\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"Q4\",\"JCRName\":\"Chemistry\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Proceedings of the National Academy of Sciences of Belarus, Chemical Series","FirstCategoryId":"1085","ListUrlMain":"https://doi.org/10.29235/1561-8331-2022-58-4-387-397","RegionNum":0,"RegionCategory":null,"ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q4","JCRName":"Chemistry","Score":null,"Total":0}
引用次数: 1
摘要
建立了测定蜂蜜中杀虫剂阿米特唑残留量的方法,并进行了验证。该方法具有选择性强、快速、简便等特点。本技术以正己烷萃取蜂蜜碱化水溶液中的阿米特拉兹为基础,采用高效液相色谱-质谱法进行定量测定。使用三种蜂蜜在阿米特拉兹的三种水平(6、120和220µg/kg)下进行验证。量化的极限是0.9µg /公斤,校准曲线的线性浓度范围从2.5到125.0 ng / mL(相应的蜂蜜是分析物含量从5.0到250.0µg / kg),重复性和相对标准差的值within-laboratory重现性不超过5.9%和3.4,分别偏差值变化从-8.2到5.6%,结果的扩展不确定度的估计范围从12至16% (P = 0.95)。在验证过程中还评估了定量的仪器极限,过程的总体效率和稳健性。
Development and validation of the method for determination of amitraz in honey using high-performance liquid chromatography with mass spectrometric detection
Method for determination of the insecticide amitraz residual content in honey has been developed and validated. The method is selective, express and easy-to-perform. The technique is based on the extraction of amitraz from alkalized aqueous solutions of honey with n-hexane and quantitative determination by high-performance liquid chromatography with mass spectrometric detection. Validation was performed using three types of honey at three levels of amitraz application 6, 120 and 220 µg/kg. The limit of quantification was 0.9 µg/kg, the calibration curves were linear in the concentration range from 2.5 to 125.0 ng/mL (the corresponding analyte content in honey is from 5.0 to 250.0 µg/kg), relative values of the standard deviations of repeatability and within-laboratory reproducibility did not exceed 3.4 and 5.9 %, respectively, the bias values varied from –8.2 to 5.6 %, the expanded uncertainty estimates of the results ranged from 12 to 16 % (P = 0.95). Instrumental limit of quantification, overall efficiency of the process and robustness were also evaluated during the validation process.