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采用 LC-MS/MS 同时测定咖喱叶中的乐果及其代谢物氧乐果,并进行风险评估。

Simultaneous determination of dimethoate and its metabolite omethoate in curry leaf using LC-MS/MS and risk assessment.

机构信息

Pesticide Residue and Food Quality Analysis Laboratory, Department of Agricultural Entomology, University of Agricultural Sciences, Raichur, Karnataka, 584 104, India.

Pesticide Toxicology Laboratory, Department of Agricultural Entomology, Tamil Nadu Agricultural University, Coimbatore, Tamil Nadu, 641 003, India.

出版信息

J Sep Sci. 2022 Jun;45(11):1831-1838. doi: 10.1002/jssc.202100696. Epub 2022 Apr 9.

DOI:10.1002/jssc.202100696
PMID:35315569
Abstract

This study presents the method development, validation, and simultaneous determination of dimethoate and its metabolite omethoate in curry leaf. Samples were extracted following modified quick, easy, cheap, effective, rugged, and safe extraction protocol and analyzed using liquid chromatography-tandem mass spectrometry. The limit of quantification in the matrix was 0.005 μg g for dimethoate and omethoate. Extraction using acetonitrile recorded the average recoveries in the range of 82.25 to 112.97% for dimethoate and 85.57 to 107.22% for omethoate at 0.005, 0.025 and 0.050 μg g fortification levels and relative standard deviation less than 5%. Similarly, the relative standard deviation values for intraday (Repeatability) and interday (Reproducibility) tests were less than 15%. Dissipation kinetics of dimethoate 30% emulsifiable concentrate at 200 and 400 g a.i h recorded initial deposits of 5.20 and 10.05 μg g and 0.33 and 0.48 μg g for dimethoate and omethoate, respectively, and half-life of 3.07 and 3.34 days. The estimated hazard index value found more than one at a day after dimethoate application. It is not safe for consumer health to use curry leaves in the initial days after application.

摘要

本研究介绍了在咖喱叶中同时测定乐果及其代谢物氧乐果的方法开发、验证和定量。样品采用改良的快速、简便、廉价、有效、耐用、安全提取方案提取,并用液相色谱-串联质谱法进行分析。在基质中,乐果和氧乐果的定量限均为 0.005μg g。乙腈提取法在 0.005、0.025 和 0.050μg g 加标水平下,乐果和氧乐果的平均回收率分别在 82.25%至 112.97%和 85.57%至 107.22%之间,相对标准偏差均小于 5%。同样,日内(重复性)和日间(再现性)测试的相对标准偏差值均小于 15%。在 200 和 400g a.i. h 下,30%乐果乳油的消解动力学研究记录了初始沉积量分别为 5.20 和 10.05μg g 和 0.33 和 0.48μg g 的乐果和氧乐果,半衰期分别为 3.07 和 3.34 天。乐果施药后一天,估计的危害指数值超过了 1。施药后最初几天食用咖喱叶对消费者健康不安全。

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