Su Jung Lee, Jung Mi Lee, Gui-Hyun Jang, Hyun-Kyung Kim, 지영 김
{"title":"LC-MS/MS同时分析农产品中36种磺酰脲类除草剂残留的研究进展","authors":"Su Jung Lee, Jung Mi Lee, Gui-Hyun Jang, Hyun-Kyung Kim, 지영 김","doi":"10.5338/kjea.2023.42.2.17","DOIUrl":null,"url":null,"abstract":"Sulfonylurea herbicides are widely used in agriculture because they have a long residual period and high selectivity. An analytical method was developed using QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) technique for simultaneous determination of sulfonylurea herbicide residues in agricultural products by liquid chromatography tandem mass spectrometry and for establishment MRL (Maximum Residue Limit) of those herbicides in Korea. Extraction was performed using acetonitrile containing 0.1% formic acid with MgSO 4 (anhydrous magnesium sulfate) and NaCl (sodium chloride) and the extract was cleaned up using MgSO 4 and C 18 (octadecyl). The matrix-matched calibration curves were composed of 7 concentration levels from 0.001 to 0.25 mg/kg and their coefficients of determination (R 2 ) exceeded 0.99. The recoveries of three spiking levels (LOQ, 10LOQ, 50LOQ, n =5) were in the range of 71.7-114.9% with relative standard deviations of less than 20.0% for all the five agriculture products. All validation values met criteria of the European Union SANTE/11312/2021 guidelines and Food and Drug Safety Evaluation guidelines. Therefore, the proposed analytical method was accurate, effective, and sensitive for sulfonylurea herbicide residues determination in agricultural commodities.","PeriodicalId":17872,"journal":{"name":"Korean Journal of Environmental Agriculture","volume":null,"pages":null},"PeriodicalIF":0.0000,"publicationDate":"2023-06-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Development of the Simultaneous Analysis of 36 Sulfonylurea Herbicide Residues in Agricultural Products Using LC-MS/MS\",\"authors\":\"Su Jung Lee, Jung Mi Lee, Gui-Hyun Jang, Hyun-Kyung Kim, 지영 김\",\"doi\":\"10.5338/kjea.2023.42.2.17\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"Sulfonylurea herbicides are widely used in agriculture because they have a long residual period and high selectivity. An analytical method was developed using QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) technique for simultaneous determination of sulfonylurea herbicide residues in agricultural products by liquid chromatography tandem mass spectrometry and for establishment MRL (Maximum Residue Limit) of those herbicides in Korea. Extraction was performed using acetonitrile containing 0.1% formic acid with MgSO 4 (anhydrous magnesium sulfate) and NaCl (sodium chloride) and the extract was cleaned up using MgSO 4 and C 18 (octadecyl). The matrix-matched calibration curves were composed of 7 concentration levels from 0.001 to 0.25 mg/kg and their coefficients of determination (R 2 ) exceeded 0.99. The recoveries of three spiking levels (LOQ, 10LOQ, 50LOQ, n =5) were in the range of 71.7-114.9% with relative standard deviations of less than 20.0% for all the five agriculture products. All validation values met criteria of the European Union SANTE/11312/2021 guidelines and Food and Drug Safety Evaluation guidelines. Therefore, the proposed analytical method was accurate, effective, and sensitive for sulfonylurea herbicide residues determination in agricultural commodities.\",\"PeriodicalId\":17872,\"journal\":{\"name\":\"Korean Journal of Environmental Agriculture\",\"volume\":null,\"pages\":null},\"PeriodicalIF\":0.0000,\"publicationDate\":\"2023-06-30\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Korean Journal of Environmental Agriculture\",\"FirstCategoryId\":\"1085\",\"ListUrlMain\":\"https://doi.org/10.5338/kjea.2023.42.2.17\",\"RegionNum\":0,\"RegionCategory\":null,\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"\",\"JCRName\":\"\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Korean Journal of Environmental Agriculture","FirstCategoryId":"1085","ListUrlMain":"https://doi.org/10.5338/kjea.2023.42.2.17","RegionNum":0,"RegionCategory":null,"ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"","JCRName":"","Score":null,"Total":0}
引用次数: 0
摘要
磺酰脲类除草剂因其残留期长、选择性高而广泛应用于农业。采用QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe)技术建立了液相色谱串联质谱法同时测定农产品中磺酰脲类除草剂残留的分析方法,并建立了国内磺酰脲类除草剂的最大残留限量(MRL)。用含0.1%甲酸的乙腈、mgso4(无水硫酸镁)和NaCl(氯化钠)进行萃取,用mgso4和c18(十八烷基)对萃取物进行净化。基质匹配校准曲线由0.001 ~ 0.25 mg/kg 7个浓度水平组成,其测定系数(r2)均大于0.99。3个添加水平(LOQ、10LOQ、50LOQ, n =5)的加样回收率在71.7 ~ 114.9%之间,相对标准偏差均小于20.0%。所有验证值均符合欧盟SANTE/11312/2021指南和食品药品安全评价指南的标准。因此,该分析方法准确、有效、灵敏,可用于农产品中磺酰脲类除草剂残留的检测。
Development of the Simultaneous Analysis of 36 Sulfonylurea Herbicide Residues in Agricultural Products Using LC-MS/MS
Sulfonylurea herbicides are widely used in agriculture because they have a long residual period and high selectivity. An analytical method was developed using QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) technique for simultaneous determination of sulfonylurea herbicide residues in agricultural products by liquid chromatography tandem mass spectrometry and for establishment MRL (Maximum Residue Limit) of those herbicides in Korea. Extraction was performed using acetonitrile containing 0.1% formic acid with MgSO 4 (anhydrous magnesium sulfate) and NaCl (sodium chloride) and the extract was cleaned up using MgSO 4 and C 18 (octadecyl). The matrix-matched calibration curves were composed of 7 concentration levels from 0.001 to 0.25 mg/kg and their coefficients of determination (R 2 ) exceeded 0.99. The recoveries of three spiking levels (LOQ, 10LOQ, 50LOQ, n =5) were in the range of 71.7-114.9% with relative standard deviations of less than 20.0% for all the five agriculture products. All validation values met criteria of the European Union SANTE/11312/2021 guidelines and Food and Drug Safety Evaluation guidelines. Therefore, the proposed analytical method was accurate, effective, and sensitive for sulfonylurea herbicide residues determination in agricultural commodities.