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气相色谱-负化学电离质谱法测定食用植物油中5种酰基吡唑类农药残留量

[Determination of five acylpyrazole pesticide residues in edible vegetable oils using gas chromatography-negative chemical ionization-mass spectrometry].

作者信息

Shen Weijian, Wu Bin, Wang Hong, Wang Xiaoyan, Yu Keyao, Lu Huiyuan, Hu Guoshen, Li Jingjing

机构信息

Animal, Plant and Food Inspection Center, Nanjing Customs, Nanjing 210019, China.

出版信息

Se Pu. 2019 Jan 8;37(1):27-31. doi: 10.3724/SP.J.1123.2018.10009.

DOI:10.3724/SP.J.1123.2018.10009
PMID:30693706
Abstract

A method was established for the determination of five acylpyrazole pesticide residues in edible vegetable oils using gas chromatography-negative chemical ionization-mass spectrometry (GC-NCI-MS). The pesticides were extracted from a sample with acetonitrile under freezing conditions. A simple cleanup step known as QuEChERS was then conducted. After being identified by GC-NCI-MS, the extracts were quantified using an external standard method that employs a matrix correction standard curve. The linearity of the method was good between 20 and 1000 μg/L, and all limits of quantification were less than 2 μg/kg. Recoveries of all pesticides were in the range of 82.7%-112.4% at the three spiked levels of 0.01, 0.02, and 0.05 mg/kg, and all relative standard deviations were not more than 12.3%. Therefore, this method can be used to determine the residues of acylpyrazole pesticides in edible vegetable oils.

摘要

建立了一种使用气相色谱 - 负化学电离 - 质谱法(GC-NCI-MS)测定食用植物油中5种酰基吡唑类农药残留量的方法。在冷冻条件下,用乙腈从样品中提取农药。然后进行一种称为QuEChERS的简单净化步骤。提取物经GC-NCI-MS鉴定后,采用外标法并使用基质校正标准曲线进行定量。该方法在20至1000μg/L之间线性良好,所有定量限均小于2μg/kg。在0.01、0.02和0.05mg/kg的三个加标水平下,所有农药的回收率在82.7% - 112.4%范围内,所有相对标准偏差均不超过12.3%。因此,该方法可用于测定食用植物油中酰基吡唑类农药的残留量。

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