液相色谱-串联质谱法测定肉及肉制品中利谷隆及其代谢产物3,4-二氯苯胺残留

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

建立了液相色谱-串联质谱分析多种肉及肉制品中利谷隆及其代谢产物3,4-二氯苯胺残留的方法。样品用丙酮-乙腈(5∶95,v/v)提取,冷冻去脂,经弗罗里硅土固相萃取柱净化后进行液相色谱-串联质谱检测,采用内标法定量。利谷隆及3,4-二氯苯胺在1～500μg/L范围内呈良好的线性关系,相关系数(r)均大于0.998,方法的定量限(信噪比(S/N)>10)为10μg/kg,检出限(S/N>3)为5μg/kg。在各种肉及肉制品基质中添加低、中、高3种不同水平的利谷隆及3,4-二氯苯胺,其回收率范围分别为88.3%～101.2%和91.6%～101.6%,相对标准偏差(RSD)分别为4.8%～13.7%和4.7%～11.8%。结果表明所建立的方法可以满足肉及肉制品中利谷隆和3,4-二氯苯胺残留量的检测需要。

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 method.In the range of 1-500 μg/L,both linuron and 3,4-dichloroaniline showed good linearity with the correlation coefficients（r） more than 0.998.The limit of quantification（S/N10） was 10 μg/kg,and the limit of detection（S/N〉3） was 5 μg/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.