凝胶渗透色谱净化-气相色谱/串联质谱分析蘑菇中的36种农药残留  

Determination of 36 Pesticide Residues in Mushroom by Gel Permeation Chromatography and Gas Chromatography-Tandem Mass Spectrometry

作　　者：于胜良[1] 杨桂朋[1] 付萌 

机构地区：[1]中国海洋大学海洋化学理论与工程技术教育部重点实验室,山东青岛266003 [2]上海诺安农产品检测服务有限公司青岛分公司,山东青岛266012

出　　处：《色谱》2007年第4期581-585,共5页Chinese Journal of Chromatography

基　　金：教育部科学技术研究重点项目(No.105105);教育部新世纪优秀人才支持计划(No.NCET-04-0643);山东省"泰山学者"建设工程专项经费资助

摘　　要：建立了用凝胶渗透色谱净化-气相色谱/串联质谱分析蘑菇中36种农药残留的方法。蘑菇中的待测农药组分在30℃条件下用乙酸乙酯提取,高速匀浆后通过凝胶渗透色谱净化;选用填料为中性多孔的聚苯乙烯二乙烯基苯微球体的S-X3玻璃柱（22g,19cm×2cm）作为凝胶渗透色谱净化柱,流动相为乙酸乙酯-环己烷（体积比为1∶1）溶液,流速5mL/min;收集第7-15min流出的液体用气相色谱-三重四极杆串联质谱仪测定。在0.01-1.0mg/L的质量浓度范围内,各种农药标准溶液的线性相关系数均大于0.99。在样品中添加36种农药（添加水平为0.01,0.05,0.10mg/kg）的混合标准溶液,平均回收率为72.6%-117.1%,相对标准偏差为2.0%-10.8%（n=5）,最低检出限为0.1-0.7μg/kg,最低定量限为0.2-2μg/kg。A gel permeation chromatographic method was developed for the extraction of 36 pesticides from mushroom prior to gas chromatography with a triple quadrupole mass spectrometric determination. The extraction was based on homogenization with ethyl acetate using a high speed homogenizer. A gel permeation chromatographic clean-up process with ethyl acetate-cyclohexane （ 1： 1, v/v） as mobile phase was applied to the extracts to separate the lowmolecular mass pesticides from the high molecular mass compounds in the mushroom. The 7 - 15 min eluate fraction was collected for subsequent analysis. The target compounds were quan- tified in the final extract by gas chromatography using a triple quadrupole mass spectrometer with multiple reaction monitoring （MRM）. In the linear range （0.01 - 1.0 mg/L） of each pesti- cide, the correlation coefficient was higher than 0.99. The average recoveries （spiked at the levels of 0.01,0.05, 0. l0 mg/kg） were from 72.6% to ll7.1% with the relative standard devi- ations from 2.0% to 10. 8% （ n = 5 ）. The limits of detection （ LOD ） for these pesticides were from 0. 1 to 0.7 μg/kg and the limits of quantification （LOQ） were from 0.2 to 2 μg/kg.

关 键 词：凝胶渗透色谱 气相色谱/串联质谱 农药 残留检测 蘑菇 

分 类 号：O658[理学—分析化学]