加速溶剂萃取/气相色谱-负化学电离质谱法对广东凉茶冲剂中有机氯杀虫剂残留的测定  

Determination of Organochlorine Pesticide Residues in Chinese Herbal Tea Granule by Accelerated Solvent Extraction Combined with Gas Chromatography-Negative Chemical Ionization-Mass Spectrometry

作　　者：邓洁薇[1] 李娜[1] 杨运云[1] 

机构地区：[1]中国广州分析测试中心广东省分析测试技术公共实验室,广东广州510070

出　　处：《分析测试学报》2011年第9期1001-1005,共5页Journal of Instrumental Analysis

基　　金：广东省科技计划重点项目(2010A030100013)

摘　　要：建立了加速溶剂萃取/气相色谱-负化学电离质谱法(ASE/GC-NCI-MS)测定广东凉茶颗粒冲剂中有机氯杀虫剂(OCPs)含量的方法。采用ASE萃取冲剂中的OCPs,萃取溶剂为正己烷-二氯甲烷(1∶1),萃取温度100℃,萃取压力10 MPa,萃取时间10 min×3。萃取液经SPE净化,浓缩定容后,经色谱柱DB-1MS(30 m×0.25 mm×0.1μm)分离,采用GC-NCI-MS测定其中OCPs的含量。25种OCPs的线性范围为1～500pg,相关系数(r)均大于0.999,方法的检出限为1.0～34.4 pg/g,定量下限为3.4～114.6 pg/g,回收率为86%～105%。将该方法用于分析不同厂家和批次的凉茶颗粒冲剂样品,25种OCPs均未检出。该方法快速、灵敏,是广东凉茶中有机氯杀虫剂残留检测的有效手段。A method was developed for the determination of organochlorine pesticide residues in Chinese herbal tea granule by accelerated solvent extraction combined with gas chromatography-negative chemical ionization-mass spectrometry（ASE/GC-NCI-MS）.The samples were extracted with ASE for 10 min×3 times using hexane-dichloromethane（1 ∶ 1） as solvent at temperature of 100 ℃ and pressure of 10 MPa.The extracts were purified by solid phase extraction using a SampliQ Silica column,concentrated with a gentle stream of nitrogen,and then separated on a DB-1MS column（30 m×0.25 mm× 0.1 μm）.The quantitative analysis of 25 organochlorine pesticides was carried out by GC-NCI-MS under selected ion monitoring mode.The calibration curves of 25 organochlorine pesticides were linear in the range of 1-500 pg,with correlation coefficients more than 0.999.The limits of detection and limits of quantitation were in the ranges of 1.0-34.4 pg/g and 3.4-114.6 pg/g,respectively.The spiked recoveries ranged from 86% to 105%.The method was applied in the determination of the Chinese herbal tea granule samples with different batches from different manufactures,and none of the 25 organochlorine pesticides was detected.The method was sensitive and efficient,and could meet the requirement for the quality control of organochlorine pesticide residues in Chinese herbal tea granule.

关 键 词：广东凉茶 有机氯 气相色谱负化学电离质谱 加速溶剂萃取 残留 

分 类 号：O657.63[理学—分析化学] S482.3[理学—化学]