羟基化多壁碳纳米管分散固相萃取/气相色谱-质谱测定茶叶中有机氯农药和拟除虫菊酯类农药残留  

Determination of Organochlorine and Pyrethroid Pesticides in Tea by Gas Chromatography-Mass Spectrometry Using Hydroxylated Multi-walled Carbon Nanotubes as Dispersive Solid-phase Extraction Sorbent

作　　者：荣杰峰 韦航 黄伙水 李亦军 许美珠 

机构地区：[1]泉州出入境检验检疫局,福建泉州362000

出　　处：《分析测试学报》2016年第1期8-15,共8页Journal of Instrumental Analysis

基　　金：福建检验检疫局科技计划项目(FK2013-26);国家质检总局项目(2015IK032);安溪县科技计划项目(N[2015]0065)

摘　　要：建立了羟基化多壁碳纳米管作为吸附剂的改进Qu ECh ERS方法,联合气相色谱-质谱联用法快速检测茶叶中24种有机氯农药和拟除虫菊酯类农药残留量。茶叶样品中的农药残留经正己烷-丙酮（2∶1）提取,以羟基化多壁碳纳米管（MWCNTs-OH）和N-丙基乙二胺键合固相吸附剂（PSA）吸附提取液中的杂质,提取液离心后过滤,经气相色谱-电子轰击源质谱法测定,外标法定量。研究了不同吸附剂种类、提取溶剂、吸附剂用量对提取净化效率的影响。在优化实验条件下,目标物质在0.01~0.50 mg/kg范围内线性关系良好。空白茶叶样品在低、中、高3个加标水平下的平均回收率为78.6%~109.6%,相对标准偏差（n=5）为2.1%~9.3%;方法的定量下限为0.002~0.050 mg/kg。该方法操作简单、快速、灵敏、成本低,能满足茶叶中常见有机氯和拟除虫菊酯类农药残留的检测要求,特别适合在小型实验室和企业中推广使用。Using modified multi-walled carbon nanotubes as sorbent in modified QuEChERS method, a rapid determination method of 24 organoehlorine and pyrethroid pesticides in tea by gas ehromatogra- phy - mass spectrometry was developed. Pestieides residues in tea were extracted with a hexane - ac- etone（2 ： 1 ） mixture, and cleaned up with hydroxylated multi-walled carbon nanotubes （MWCNTs - OH） and primary - secondary amine （PSA） as dispersive solid-phase extraction sorbent. After cen- trifugation and filtration, the target compounds were analyzed by gas chromatography - mass spec- trometry, and quantified by the external standard method. Effects of different sorbents and extraction solvents, amount of hydroxylated multi-walled carbon nanotubes on the determination of organoehlo- rine and pyrethroid pesticides residues were investigated. Under the optimal conditions, the ealihra- tion curves were linear in the range of 0.01 -0. 50 mg/kg. Tests of recoveries were made by the ad- dition of mixed standards to blank tea sample at three concentration levels, and the recoveries were in the range of 78.6% - 109.6% with relative standard deviations （ RSDs, n = 5） of 2. 1% - 9. 3% . The quantitation limits of method were in the range of 0. 002 - 0. 050 mg/kg. The method is simple, rapid, sensitive and cheap, and could meet the requirements for the detection of organoehlorine and pyrethroid pesticides in teas, partieularly suitable for the applieation in small laboratories and enter- prises.

关 键 词：羟基化多壁碳纳米管 分散固相萃取 气相色谱-质谱 茶叶 有机氯农药 拟除虫菊酯类农药 

分 类 号：O657.63[理学—分析化学] F767.2[理学—化学]