同位素内标稀释气相色谱-质谱联用法测定果蔬中的滴滴涕含量  

Determination of DDT in Fruits and Vegetables by Gas Chromatography-Mass Spectrometry

作　　者：李美华[1] 杨维成[1] 盛立彦 吕靖[1] 潘洁[1] 孙雯[1] 罗勇[1] 

机构地区：[1]上海化工研究院,上海200062

出　　处：《分析科学学报》2016年第1期67-70,共4页Journal of Analytical Science

基　　金：国家科技支撑计划(No.2015BAK45B01);上海化学试剂产业技术创新战略联盟能力提升项目(No.14DZ0511800)

摘　　要：建立了果蔬中滴滴涕（DDT）的气相色谱-质谱联用的测定方法。样品用乙腈提取,采用Florisil固相萃取柱净化,以HP-5ms色谱柱（30m×0.25mm×0.25μm）分离,在选择离子模式（SIM）下,以自行研制的p,p′-DDT-D8为内标进行定性定量分析。线性范围为1~1 000μg/L,检出限为0.02~0.05μg/kg,加标回收率为88.67%~101.73%,相对标准偏差（RSD）为1.6%~3.8%（n=5）。该方法为果蔬中滴滴涕的检测提供了一种可靠实用的方法。In this paper,a method for the determination of DDT and its isomers in fruits and vegetables was established by gas chromatography-mass spectrometry with self-prepared D8-DDT as the internal standard.Samples were extracted with acetonitrile and purified by Florisil column,and the chromatographic separation was carried out using a HP-5ms column（30m×0.25mm×0.25μm）.The mass spectrometer was operated using SIM mode.The detection limits were 0.02-0.05μg/kg and the linear range was obtained from 1to 1 000μg/L.The recoveries were between 88.67%and 101.73%,and RSDs values were between 1.6%and 3.8%（n=5）.This method was proved to be accurate and sensitive for the determination of DDT residue in fruit and vegetables.

关 键 词：气相色谱-质谱联用 同位素标记内标 滴滴涕 果蔬 

分 类 号：O657.63[理学—分析化学]