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[液相色谱-串联质谱法测定农产品中农药多残留方法的验证研究]

[Validation study on a multi-residue method for determination of pesticides in agricultural products by LC-MS/MS].

作者信息

Ueno Eiji, Watanabe Minae, Umemura Yuko, Inoue Tomomi, Ikai Yoshitomo

机构信息

Aichi Prefectural Institute of Public Health.

出版信息

Shokuhin Eiseigaku Zasshi. 2014;55(6):290-6. doi: 10.3358/shokueishi.55.290.

Abstract

A multi-residue method for 122 pesticides in agricultural products was validated in accordance with Japanese guidelines for residual agricultural chemicals in food. The sample was extracted with acetonitrile. Co-extractives were removed by GPC-graphitized carbon column SPE, followed by silica gel/PSA cartridge column SPE. The pesticides in the test solution were determined by LC-MS/MS using scheduled MRM in combination with polarity switching. Validation tests were performed on spinach, brown rice, soybean, orange and tomato fortified at 0.01 and 0.1 μg/g. The pesticides at each level were analyzed in two samples per day on five different days. In conclusion, among 122 pesticides tested for each level, 121 pesticides (but not disulfoton) were found to meet all of the guideline criteria.

摘要

按照日本食品中残留农业化学品指南,对一种用于测定农产品中122种农药的多残留方法进行了验证。样品用乙腈提取。共提取物通过凝胶渗透色谱-石墨化碳柱固相萃取去除,然后通过硅胶/PSA柱固相萃取。测试溶液中的农药通过液相色谱-串联质谱联用,采用定时多反应监测结合极性切换进行测定。在菠菜、糙米、大豆、橙子和番茄中添加浓度为0.01和0.1μg/g进行验证试验。每个水平的农药在五个不同的日子里每天分析两个样品。总之,在每个水平测试的122种农药中,发现121种农药(但不包括乙拌磷)符合所有指南标准。

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