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分散固相萃取-超高效液相色谱-串联质谱法测定水果、蔬菜、牛奶、植物油和动物肌肉中的61种有机磷农药残留量

[Determination of 61 organophosphorous pesticide residues in fruits, vegetables, milk, vegetable oils and animal muscles by dispersive solid-phase extraction and ultra performance liquid chromatography-tandem mass spectrometry].

作者信息

Ye Ruihong, Su Jianfeng

机构信息

Fuqing Branch of Fujian Normal University, Fuqing 350300, China.

出版信息

Se Pu. 2011 Jul;29(7):618-23.

PMID:22097787
Abstract

A dispersive solid-phase extraction coupled with ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed for the determination of 61 organophosphorous pesticide residues in fruits, vegetables, milk, vegetable oils and animal muscles. The fruit, vegetable and milk samples were extracted with acetonitrile and separated with salting out method; vegetable oil samples were dissolved by n-hexane, and extracted with acetonitrile; animal muscle samples were extracted with acetonitrile-water assisted by n-hexane and separated with salting out method. And then the supernatants were purified using dispersive solid-phase extraction (C18 and primary secondary amine powder) prior to the UPLC-MS/MS analysis. The analytes were indentified in positive electrospray ionization (ESI+) and multiple reaction monitoring (MRM) mode. The matrix-matched external standard calibration curves were used for quantitative analysis. Under the optimal conditions, the detection limits (S/N > or = 10) of the method were 0.01 mg/kg. The recoveries were 62.8%-107%, and the relative standard deviations (RSDs) were in the range of 4.2%-19%. The method has the advantages of easy, fast, and more sensitive, and can meet the requirement of the determination of organophosphorous pesticide residues in the foods.

摘要

建立了一种分散固相萃取结合超高效液相色谱 - 串联质谱(UPLC - MS/MS)法,用于测定水果、蔬菜、牛奶、植物油和动物肌肉中的61种有机磷农药残留。水果、蔬菜和牛奶样品用乙腈提取,采用盐析法分离;植物油样品用正己烷溶解,再用乙腈提取;动物肌肉样品用乙腈 - 水在正己烷辅助下提取,并用盐析法分离。然后,在进行UPLC - MS/MS分析之前,上清液采用分散固相萃取(C18和伯仲胺粉末)进行净化。在正电喷雾电离(ESI +)和多反应监测(MRM)模式下对分析物进行鉴定。采用基质匹配外标校准曲线进行定量分析。在最佳条件下,该方法的检测限(S/N≥10)为0.01 mg/kg。回收率为62.8% - 107%,相对标准偏差(RSD)在4.2% - 19%范围内。该方法具有简便、快速、灵敏度高的优点,能够满足食品中有机磷农药残留测定的要求。

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