气相色谱-质谱法分析蜂蜜中多种有机氯农药残留  

Multiresidue determination of organochlorine pesticides in honey by gas chromatography-mass spectrometry

作　　者：林竹光[1] 金珍[1] 马玉[1] 陈美瑜[1] 谭君[1] 范玉兰[1] 陈招斌[1] 涂逢樟[2] 

机构地区：[1]厦门大学化学化工学院化学系现代分析科学教育部重点实验室,厦门361005 [2]龙岩学院化学与材料工程系,龙岩364000

出　　处：《分析试验室》2006年第6期12-17,共6页Chinese Journal of Analysis Laboratory

摘　　要：建立了气相色谱-电子轰击离子化-质谱法（GC-EI-MS）同时分析蜂蜜试样中12种有机氯农药残留的分析方法.蜂蜜试样用V（正己烷）：V（乙酸乙酯）=5：1混合提取剂超声提取和Florisil硅藻土层析柱净化后,以PCB 103为内标物,采用GC-EI-MS的选择离子监测方式（SIM）分析,同时探讨了一些有机氯农药EI-MS特征离子的结构与断裂机理.当空白试样的加标浓度为10、50、200μg/kg时,加标回收率为80%～112%,相对标准偏差为0.4%～9.8%,方法检出限为0.2～4.0μg/kg,其中8种农药的MDL＜1.0μg/kg,线性范围为10～500μg/kg,相关系数皆大于0.996,此方法已用于蜂蜜试样中多种痕量有机氯农药残留的分析.An analytical multiresidue method for the simultaneous determination of 12 organochlorines pesticides in honey was developed. Pesticides were extracted from honey with hexane/ethyl acetate （5/1, V/V）, in an ultrasonic bath and cleaned up on a Florisil column, then were determined by using a gas chromatography-mass spectrometry operated in electron ionization mode and quantified in selective ion monitoring mode, and with PCB103 as internal standard. Meanwhile, fracture mechanism of some organochlorines electronic ionization mass spectrometry were evaluated. Recovery studies were performed at 10, 50 and 200 μg/kg fortification levels for each pesticide, and the recoveries ranged from 80% to 112% with a relative standard deviation between 0.4% and 9.8% for the different pesticides. The detection limit of the method was less than 1.0 μg/kg for the most of pesticides. The developed method was linear over the range assayed, 10 ～500 μg/L, with correlation coefficients 〉 0.996. Finally, the developed analytical method has been successfully applied to the determination of pesticides in several honey samples.

关 键 词：气相色谱-质谱 蜂蜜 有机氯农药 农药残留 

分 类 号：O657[理学—分析化学]