色谱

色谱 ›› 2013, Vol. 31 ›› Issue (8): 739-746.DOI: 10.3724/SP.J.1123.2013.01036

• 研究论文 • 上一篇    下一篇

凝胶渗透色谱-固相萃取联合净化气相色谱-质谱联用法测定动物性食品中30种有机氯农药的残留量

杜娟1,2, 吕冰2, 朱盼2,3, 苗虹2, 吴永宁1,2   

  1. 1. 武汉工业学院食品科学与工程学院, 湖北 武汉 430023;
    2. 卫生部食品安全风险评估重点实验室, 国家食品安全风险评估中心, 北京 100021;
    3. 南昌大学食品科学与技术国家重点实验室, 江西 南昌 330031
  • 收稿日期:2013-01-18 修回日期:2013-03-14 出版日期:2013-08-28 发布日期:2013-09-29
  • 通讯作者: 苗虹
  • 基金资助:

    "十二五"国家科技支撑计划项目(2011BAK10B06).

Determination of 30 organochlorine pesticides in animal-originated food products using combined purification by gel permeation chromatography and solid-phase extraction coupled with gas chromatography-mass spectrometry

DU Juan1,2, LÜ Bing2, ZHU Pan2,3, MIAO Hong2, WU Yongning1,2   

  1. 1. College of Food Science and Engineering, Wuhan Polytechnic University, Wuhan 430023, China;
    2. Key Laboratory of Food Safety Risk Assessment, Ministry of Health; China Center for Food Safety Risk Assessment, Beijing 100021, China;
    3. Key Laboratory of Food Science and Technology, Nanchang University, Nanchang 330031, China
  • Received:2013-01-18 Revised:2013-03-14 Online:2013-08-28 Published:2013-09-29
  • Contact: O658

PDF

295

被引次数

27

摘要：

建立了猪肉、鸡肉、鱼肉和虾肉等动物性食品中30种有机氯农药残留的气相色谱-质谱联用检测方法。样品匀浆后,采用乙腈提取,以凝胶渗透色谱和弗罗里硅土固相萃取柱联合进行净化,气相色谱-质谱检测,以同位素内标法定量。30种有机氯农药的响应在5.0~500.0 μg/L范围内呈良好的线性,相关系数在0.996以上,各有机氯农药的检出限在0.2~2.7 μg/kg之间。以猪肉、鸡肉、鱼肉和虾肉作为代表性基质,进行5.0、10.0、20.0 μg/kg 3个水平的加标回收试验,回收率在55.0%~119.1%之间,相对标准偏差在0.4%~15.0%之间。该方法准确可靠,灵敏度高,样品净化效果好,能够满足动物性食品中有机氯农药多残留痕量分析的要求。

关键词: 动物性食品, 多残留, 气相色谱-质谱联用, 有机氯农药

Abstract:

A new analytical method was developed for the determination of 30 organochlorine pesticides (OCPs) in animal-originated food, including pork, chicken, fish and shrimp. The combined purification by gel permeation chromatography (GPC) and solid-phase extraction (SPE) were established by optimizing different fraction collection times. The detection conditions can be achieved by gas chromatography-mass spectrometry (GC-MS) using selective ion monitoring (SIM). Isotopic internal standards were used for the quantitative determination of the 30 OCPs. The sample pretreatment procedure was based on acetonitrile extraction and combined purification of GPC and Florisil SPE cartridge. The experimental results showed that the linear ranges for 30 OCPs were 5.0-500.0 μg/L, the correlation coefficients were better than 0.996, and the method detection limits (MDLs) of the 30 OCPs were 0.2-2.7 μg/kg. The spiked recoveries at three levels of 5.0, 10.0 and 20.0 μg/kg using pork, chicken, fish and shrimp samples as blank matrices were in the range of 55.0%-119.1%, the relative standard deviations (RSDs) were in the range of 0.4%-15.0%. The method has the advantages of wide linear range, high sensitivity and efficient clean-up procedure, and consistent with the demand of pesticide routine analysis.

Key words: animal-originated food, gas chromatography-mass spectrometry (GC-MS), multi-residue, organochlorine pesticides

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