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[采用液相色谱-串联质谱法测定肉类及肉制品中利谷隆及其代谢物3,4-二氯苯胺残留量]

[Determination of linuron and its metabolite 3,4-dichloroaniline residues in meat and meat products using liquid chromatography-tandem mass spectrometry].

作者信息

Guo Dehua, Yi Xionghai, Qu Li

机构信息

Shanghai Entry-Exit Inspection and Quarantine Bureau, Shanghai 200135, China.

出版信息

Se Pu. 2011 Oct;29(10):967-73.

Abstract

A method of liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed for the determination of linuron and its metabolite 3, 4-dichloroaniline residues in pork, liver, kidney, casings, canned steam pork and sausage. The sample was extracted with a mixture of acetone-acetonitrile (5: 95, v/v). Most of the lipids in the extract were eliminated by freezing-lipid filtration. After Florisil solid phase extraction cleanup, the linuron and its metabolite residues were determined by LC-MS/MS, and quantified by internal standard meth-od. In the range of 1 - 500 microg/L, both linuron and 3,4-dichloroaniline showed good linearity with the correlation coefficients (r) more than 0. 998. The limit of quantification (S/N > 10) was 10 microg/kg, and the limit of detection (S/N > 3) was 5 microg/kg for each analyte. The recoveries of linuron and 3,4-dichloroaniline in meat and meat products at three spiked levels were in the ranges of 88.3% - 101.2% and 91.6% - 101. 6%, and the relative standard deviations were in the ranges of 4. 8% - 13. 7% and 4. 7% - 11. 8%, respectively. The results demonstrated that the proposed method can meet the requirements for the determination of linuron and 3,4-dichloroaniline in meat and meat products.

摘要

建立了一种液相色谱-串联质谱法(LC-MS/MS),用于测定猪肉、肝脏、肾脏、肠衣、罐装蒸猪肉和香肠中利谷隆及其代谢物3,4-二氯苯胺的残留量。样品用丙酮-乙腈混合液(5:95,v/v)提取。提取物中的大部分脂质通过冷冻-脂质过滤去除。经弗罗里硅土固相萃取净化后,采用LC-MS/MS测定利谷隆及其代谢物残留量,并以内标法进行定量。在1 - 500μg/L范围内,利谷隆和3,4-二氯苯胺均呈现良好的线性,相关系数(r)大于0.998。各分析物的定量限(S/N>10)为10μg/kg,检测限(S/N>3)为5μg/kg。利谷隆和3,4-二氯苯胺在肉类和肉制品中3个加标水平下的回收率分别为88.3% - 101.2%和91.6% - 101.6%,相对标准偏差分别为4.8% - 13.7%和4.7% - 11.8%。结果表明,该方法能够满足肉类和肉制品中利谷隆和3,4-二氯苯胺残留量测定的要求。

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