气相色谱-离子阱-多级质谱法检测鱼体组织中19种有机氯农药

李荣; 何力; 徐进; 吴翠玲

中国水产科学研究院长江水产研究所,农业部淡水鱼类种质监督检验测试中心,湖北,荆州,434000

Varian北京办事处,北京,100070

Determination of 19 Organochlorine Pesticides Residues in Fish Tissues by Gas Chromatography-Ion Trap Mass Spectrometry

摘要: 建立了鱼体组织中19种有机氯农药残留分析的气相色谱-离子阱-多级质谱(GC-IT-MS/MS)方法.试样用V(正己烷):V(丙酮)=1:1溶液提取,凝胶渗透色谱和固相萃取联合净化,浓缩、定容后,上机分析.结果表明,采用EI电离模式,选择不同的监测特征离子,GC-IT-MS/MS法能灵敏测定加标试样中全部目标化合物.添加浓度为5.0 μg·kg~(-1)和10 μg·kg~(-1)时的加标回收率在76.2%～106%之间,相对标准偏差在4.8%～11%范围内;检测限(S/N=3)和定量限(S/N=10)分别为0.03～1.42 μg·kg~(-1)和0.1～4.27 μg·kg~(-1).

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Abstract: A method for the simultaneous determination of 19 organochlorine pesticides(OCPs) in fish tissues was developed by gas chromatography-ion trap mass spectrometry(GC-IT-MS/MS). The samples were extracted by mixture of V(acetone):V(hexane)=1:1, then cleaned-up by gel permeation chromatography(GPC) and solid phase extraction(SPE), followed by analysis using GC-IT-MS/MS. The experimental results demonstrated good sensitivity for 19 target OCPs in spiked samples, by monitoring different precursor ions and product ions in electron ionization(EI) mode. Spiked reference samples are analyzed at concentration levels of 5.0 μg·kg~(-1) and 10 μg·kg~(-1), the average recoveries are range of 76.2%-106%, with a relative standard deviation(RSD) range of 4.8%-11%. Limits of detection(LOD) (S/N=3) are range of 0.03-1.42 μg·kg~(-1). Limits of quantification(LOQ) (S/N=10) are between 0.1 μg·kg~(-1) and 4.27 μg·kg~(-1).

气相色谱-离子阱-多级质谱法检测鱼体组织中19种有机氯农药

中国水产科学研究院长江水产研究所,农业部淡水鱼类种质监督检验测试中心,湖北,荆州,434000

Varian北京办事处,北京,100070

关键词:

Determination of 19 Organochlorine Pesticides Residues in Fish Tissues by Gas Chromatography-Ion Trap Mass Spectrometry

中国水产科学研究院长江水产研究所,农业部淡水鱼类种质监督检验测试中心,湖北,荆州,434000

Varian北京办事处,北京,100070

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