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

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1～500 μg/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10 μg/kg,检出限(S/N＞3)为5 μg/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。

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

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.