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Simultaneous determination of the metabolites of the herbicide metazachlor in agricultural crops by LC–MS/MS
Applied Biological Chemistry ( IF 2.3 ) Pub Date : 2020-06-13 , DOI: 10.1186/s13765-020-00513-1
Ji-Su Park , Han Sol Lee , Sung Min Cho , Su Jung Lee , Hye-Sun Shin , Jae-Han Shim , Sang Soon Yun , Yong-hyun Jung , Jae-ho Oh

To manage the safety of the herbicide metazachlor, analytical methods are required for the determination of metazachlor metabolites in agricultural crops. Herein, a liquid chromatography–tandem mass spectrometry (LC–MS/MS) method was developed for the simultaneous determination of metazachlor metabolites (479M04, 479M08, and 479M16) in various agricultural commodities. After extraction using acetonitrile and adjusting the pH to 3, the samples were purified using a hydrophilic–lipophilic balance cartridge. The matrix-matched calibration curves (0.002–0.2 μg/mL) were linear (r2 > 0.99). For validation, recovery tests were carried out at three fortification levels (limit of quantification (LOQ), 10 LOQ, and 50 LOQ) in various agricultural samples. The recoveries of 479M04, 479M08, and 479M16 were 79.6–113.0, 76.9–97.7, and 79.1–102.1%, respectively, with relative standard deviation values of less than 17.0%. Furthermore, inter-laboratory testing was conducted to validate the method. All the values corresponded to the criteria of both the CODEX (CAC/GL 40-1993, 2003) and Ministry of Food and Drug Safety guidelines. Therefore, the proposed LC–MS/MS method can be used as an analytical method for the determination of metazachlor.

中文翻译:

LC-MS / MS同时测定农作物中除草剂间草胺的代谢物

为了管理除草剂灭草胺的安全性,需要使用分析方法测定农作物中的灭草胺代谢产物。在此,开发了一种液相色谱-串联质谱(LC-MS / MS)方法,用于同时测定各种农产品中的甲草胺代谢物(479M04、479M08和479M16)。用乙腈萃取并调节pH至3后,使用亲水亲脂平衡柱纯化样品。基质匹配的校准曲线(0.002-0.2μg/ mL)是线性的(r2> 0.99)。为了验证有效性,对各种农业样品在三个设防水平(定量限(LOQ),10 LOQ和50 LOQ)下进行了回收率测试。479M04、479M08和479M16的回收率为79.6–113.0、76.9–97.7和79.1–102.1%,相对标准偏差小于17.0%。此外,进行了实验室间测试以验证该方法。所有值均符合CODEX(CAC / GL 40-1993,2003)和食品和药品安全部准则的标准。因此,建议的LC-MS / MS方法可以用作测定甲草胺的分析方法。
更新日期:2020-06-13
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