气相色谱-负化学源-质谱法测定乌龙茶中拟除虫菊酯和有机氯农药多残留  

Determination of pyrethroids and organochlorine pesticides in oolong tea by gas chromatography-negative chemical ionization-mass spectrometry

作　　者：朱盼[1] 万欢 吕芬[1] 姚敬[1] 龙朝阳[1] 黄伟雄[1] 吴永宁 ZHU Pan;WAN Huan;LV Fen;YAO Jing;LONG Chaoyang;HUANG Weixiong;WU Yongning(Guangdong Provincial Center for Disease Control and Prevention,Guangdong Guangzhou 511430,China;The College of Natural Resources and Environment,South China Agricultural University,Guangdong Guangzhou 510642,China;National Center for Food Safety Risk Assessment,Beijing 100021,China)

机构地区：[1]广东省疾病预防控制中心,广东广州511430 [2]华南农业大学资源环境学院,广东广州510642 [3]国家食品安全风险评估中心,北京100021

出　　处：《中国食品卫生杂志》2021年第4期415-422,共8页Chinese Journal of Food Hygiene

基　　金：广东省自然科学基金(2020A1515010655);广东省医学科研基金(A2017035,C2020010)。

摘　　要：目的建立一种基于液液萃取-固相萃取-气相色谱-负化学源-质谱(GC-NCI-MS)测定乌龙茶中多组分拟除虫菊酯和有机氯类杀虫剂的分析方法。方法茶叶样品粉碎过筛后,经沸水浸泡、丙酮-正己烷液液萃取、Carb-NH2固相萃取柱进化后,用GC-NCI-MS方法进行定性、定量分析。结果18种拟除虫菊酯和9种有机氯类杀虫剂分别在0.006~1.00μg/mL和0.006~0.50μg/mL浓度范围内具有良好的线性关系,相关系数(r)均大于0.996,加标回收率为60.1%~119.8%,相对标准偏差为1.5%~10.4%(n=6),方法检出限和定量限分别为0.5~4.8μg/kg和1.7~16.0μg/kg。结论该方法快速、准确,能满足乌龙茶样品中18种拟除虫菊酯和9种有机氯类杀虫剂残留的快速检测分析要求。Objective To establish a method for the determination of several kinds of pyrethroids and organochlorine pesticides in Chinese oolong tea samples based on liquid-liquid extraction-solid phase extraction-gas chromatography-negative chemical ionization-mass spectrometry(GC-NCI-MS).Methods Oolong tea samples were crushed and screened,soaked in boiling water,extracted with acetone-n-hexane,purified by Carb-NH2 column,and then identified and quantified by GC-NCI-MS.Results All the 18 kinds of pyrethroids and 9 kinds of organochlorine pesticides showed good linear relationships in range of 0.006-1.00μg/mL and 0.006-0.50μg/mL respectively,and the correlation coefficients were above 0.996.The recoveries at different spiked levels for all target compounds in blank matrices were 60.1%-119.8%,and the relative standard deviation(RSD)were 1.5%-10.4%(n=6).The limits of detection and quantification of the method were 0.5-4.8μg/kg and 1.7-16.0μg/kg,respectively.Conclusion The method was suitable for rapid screening and analysis of 18 pyrethroids and 9 organochlorine pesticides in Chinese oolong tea with the advantage of accuracy,rapidity and high sensitivity.

关 键 词：气相色谱-负化学源-质谱 乌龙茶 拟除虫菊酯 有机氯 

分 类 号：R155[医药卫生—营养与食品卫生学]