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

引用本文: 杜娟, 吕冰, 朱盼, 苗虹, 吴永宁. 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[J]. 色谱, 2013, 31(8): 739-746. doi: 10.3724/SP.J.1123.2013.01036 shu

Citation: DU Juan, LÜ Bing, ZHU Pan, MIAO Hong, WU Yongning. 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[J]. Chinese Journal of Chromatography, 2013, 31(8): 739-746. doi: 10.3724/SP.J.1123.2013.01036 shu

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,

通讯作者: 苗虹

基金项目:
"十二五"国家科技支撑计划项目(2011BAK10B06). (2011BAK10B06)

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:

English

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

1.
1. College of Food Science and Engineering, Wuhan Polytechnic University, Wuhan 430023, China;

Corresponding author: 苗虹

Received Date: 18 January 2013
Fund Project:
"十二五"国家科技支撑计划项目(2011BAK10B06).

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:

gas chromatography-mass spectrometry (GC-MS)
/ organochlorine pesticides
/ multi-residue
/ animal-originated food

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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

通讯作者: 苗虹

English

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

Corresponding author: 苗虹

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中国化学会秘书处

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

通讯作者: 苗虹

English

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

Corresponding author: 苗虹

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

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CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

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