大豆中二硝基苯胺类除草剂多残留的气相色谱法定量检测及质谱确证  

Determination of Dinitroaniline Multi-residues in Soybean by Gas Chromatography-Mass Spectrometry

作　　者：霍江莲[1] 李军[2] 葛毅强[1] 储晓刚[2] 

机构地区：[1]中国农业大学食品科学与营养工程学院 [2]中国检验检疫科学研究院食品安全研究所,北京100025

出　　处：《分析化学》2006年第U09期63-67,共5页Chinese Journal of Analytical Chemistry

基　　金：国家"十五"食品安全重大专项课题"农药残留检测技术研究"资助项目(No.2001BA804A17-02)

摘　　要：建立以凝胶渗透色谱法（GPC）和固相萃取法（SPE）及气相色谱法（GC）联用技术测定大豆中10种二硝基苯胺类除草剂（氟乐灵、乙氟灵、环丙氟、氯乙氟灵、仲丁灵、异乐灵、二甲戊乐灵、二硝胺、氨基丙氟灵和磺乐灵）多残留检测方法。目标农药经正己烷饱和的乙腈提取，凝胶渗透色谱除去大豆中大部分油脂及色素，再经Florisil柱净化和富集，依次用6mL二氯甲烷和6mL二氯甲烷＋丙酮（99＋1）洗脱。目标农药采用电子捕获检测（GC／ECD），外标法定量，并经质谱（MS）确证。两个添加水平重复6次，回收率分别为74％～105％和59％～105％；相对标准偏差〈20％；检出限为1．8～7．6μg／kg；定量限为6～38μg/kg。A gel permeation chromatography-solid phase extraction-gas chromalography （GPC-SPE-GC） method for simuhaneous determination of 10 dinitroaniline herbicides （trifluralin, ethalfluralin, profluralin, fluchloralin, butralin, isopropalin, pendimethalin, dinitramine, prodiamine, nitralin） in soybean was developed. The herbicides were extracted with acetonitrile （saturated by n-hexane） using uhrasonic washer extractor for 15 minutes from soybean sample. Most of lipids and pigments in co-extractives were removed by gel permeation chromatography. The portion of 14 - 21 min eluat was collected by the gel permeation chromatography （GPC）. The herbicide residues was cleanup on Florisil column using 6 mL dichloromethane and 6 mL dichloromethane ＋ acetone （99 ＋ 1）. When electron capture detector is used as the quantitative detection system, the positive sample was confirmed by GC-MS with SIM mode. Recoveries of 2 fortified levels were 74% - 105%, 59% - 105% respectively, repeated 6 times, RSD 〈 20%. The limit of determination was 1.8 - 7.6 μg/kg, and the limit of quantitation was 6 - 38 μg/kg.

关 键 词：二硝基苯胺类 大豆 气相色谱 气相色谱-质谱 凝胶渗透色谱 固相萃取 

分 类 号：TS214.2[轻工技术与工程—粮食、油脂及植物蛋白工程] O657.63[轻工技术与工程—食品科学与工程]