食品科学 ›› 2009, Vol. 30 ›› Issue (22): 331-334.doi: 10.7506/spkx1002-6300-200922079

• 分析检测 • 上一篇    下一篇

高效液相色谱-串联质谱法测定进出口食品中十三吗啉残留

高文惠1,艾连峰2   

  1. 1. 河北科技大学生物科学与工程学院 2. 河北出入境检验检疫局
  • 收稿日期:2008-11-28 修回日期:2009-04-21 出版日期:2009-11-15 发布日期:2010-12-29
  • 通讯作者: 高文惠 E-mail:wenhuigao@126.com
  • 基金资助:

    河北省自然科学基金项目(B2008000669);河北省教育厅课题(Z2005202);
    河北科技大学杰出青年基金项目(2006JC-14)

Use of HPLC Coupled with Tandem MS for Determination of Tridemorph Residues in Import and Export Foods

GAO Wen-hui1,AI Lian-feng2   

  1. 1. College of Biological Science and Engineering, Hebei University of Science and Technology, Shijiazhuang 050018, China;
    2. Hebei Entry and Exit Inspection and Quarantine Bureau, Shijiazhuang 050071, China
  • Received:2008-11-28 Revised:2009-04-21 Online:2009-11-15 Published:2010-12-29
  • Contact: GAO Wen-hui E-mail:wenhuigao@126.com

摘要:

建立一种快速、灵敏的测定进出口食品中十三吗啉残留量的高效液相色谱- 串联质谱(LC-MS-MS)方法,并已在选定的多种基质的检测中证明是有效的。采用乙酸乙酯对样品中十三吗啉残留进行提取。提取液经ENVI-Carb/LC-NH2 柱固相萃取(花生采用GPC 净化)净化后,用液相色谱- 串联质谱联用仪检测,外标法定量。实验结果表明,该方法的线性范围为2.5~100ng/ml,线性相关系数为0.9995,检测限为2.5ng/ml,在添加浓度10~100ng/g 范围内,十三吗啉的平均回收率在80.2%~101.8% 之间,相对标准偏差在5.71%~10.50% 之间(n=6)。实验证明该方法具有操作简便、快速、结果准确、检测限低等特点,能够满足日本肯定列表及欧盟等发达国家的限量检测要求。

关键词: 十三吗啉, 杀菌剂, 残留, 高效液相色谱-串联质谱法

Abstract:

A rapid and sensitive high performance liquid chromatography-electrospray ionization-tandem mass spectrometry (HPLC-ESI-MS-MS) method for the determination of tridemorph residues in import and export foods was developed and validated in foods of various matrix. The tridemorph residues in samples were extracted with ethyl acetate and purified with solid extraction using ENVI-Carb/LC-NH2 column (peanut with GPC). The purified liquid was detected using HPLC-MS-MS and quantified using external standard method. Linear range of tridemorph was between 2.5 - 100 ng/ml with the correlation coefficients 0.9995 and the detection limit 2.5 ng/ml. The recoveries for all samples with tridemorph ranging 10-100 ng/g were between 80.2% and 101.8%. The relative standard deviations(R.S.D.s) were between 5.71%-10.50% (n=6). The results show that the method was convenient, rapid, accurate and of low detection limit, and could satisfy the request of Japan and Europe.

Key words: tridemorph, fungicide, residue, high performance liquid chromatography-tandem mass spectrometry

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