色谱

色谱

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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

郭德华, 伊雄海*, 曲栗   

  1. 上海出入境检验检疫局, 上海 200135
  • 收稿日期:2011-05-03 修回日期:2011-06-17 出版日期:2011-10-28 发布日期:2011-10-13
  • 通讯作者: 伊雄海,博士,工程师,研究方向为食品安全.
  • 基金资助:
    上海技术标准专项基金项目(10DZ050410)、上海技术贸易措施应对专项基金项目(09TBT006)和国家质量监督检验检疫总局项目(2011IK232).

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

GUO Dehua, YI Xionghai*, QU Li   

  1. Shanghai Entry-Exit Inspection and Quarantine Bureau, Shanghai 200135, China
  • Received:2011-05-03 Revised:2011-06-17 Online:2011-10-28 Published:2011-10-13

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484

被引次数

1

摘要： 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。

关键词: 3,4-二氯苯胺, 利谷隆, 肉, 肉制品, 液相色谱-串联质谱

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 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/N＞10) 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.

Key words: 3,4-dichloroaniline, linuron, meat, meat products, liquid chromatography-tandem mass spectrometry(LC-MS/MS)