加速溶剂萃取凝胶渗透色谱-固相萃取净化气相色谱-质谱法测定茶叶中残留的33种农药.pdfVIP

2008 年 1 月 Vol. 26 No. 1 色谱 January 2008 Chinese Journal 01 Chromatography 22 -28 加速溶剂萃取/凝胶渗透色谱固相萃取净化/气相色谱 质谱法测定茶叶中残留的 33 种农药 胡贝贞， 宋伟华， 1M 丽萍， 邵铁锋 (细〉飞出入城价!阶粉咬时，浙江绍兴 3120üO) 摘要:建立了茶叶中有机磷、有机氯、拟除虫菊醋类共 33 种农药残留的分析方法。样品以丙酬-二氯甲炕(体积比 为 1: 1) 为提取剂经加速溶剂方法萃取，提取液用凝胶渗透色谱净化除去大部分的色素、脂类和蜡质，再用 Carb­ NH 小柱和 Florisil 小柱净化。采用气相色谱法分析、外标法定量、气相色i普·质谱法(GC-MS) 定性。加标水平为 2 ü.05 mg/kg时，大部分农药的回收率为 70% -120% ，相对标准偏差小于20% 。方法的检测限为O. 005 - O. 05 mg/kg (以 10 倍信噪比计)。该方法的提取效率高，准确灵敏，目前已应用于出口茶叶中农药残留的日常检测。大量实际 样品的检测结果表明，此方法适于出口茶叶中农药残留检测实际工作的需要。 关键词:加速溶剂萃取;凝胶渗透色谱z 固相萃取;气相色谱·质谱;农药;茶叶;残留测定 中图分类号:0658 文献标识码:A 文章编号: 1000-8713 (2008) 01-0022-07 栏目类别:研究论文 Determination of 33 pesticides in tea by accelerated solvent extraction-gel permeation and solid帽phase extraction purification -gas chromatography-mass spectrometry HU Beizhen , SONG Weihua , XIE Liping , SHAO Tiefeng (Shao:ring E叽try-r:it Inspection α nd Qaαranti怔e Buγeau 、 Shao.x:i ng 312000 、 China) Abstract: A method has been developed for the determination of 33 pesticide residues in tea , including organophosphorous , organochlorine and pyrethroìd pesticides. The target analytes were extracted with the solution of acetone/dichloromethane (1: 1 , v/v) using accelerated sol- vent extraction (ASE) and then purified using gel permeation chromatography (GPC) to elimi- nate most of the coextracts , such as pigments , lipids and waxes. They were further purified using Carb-NH2 and Florisil solid-phase extraction (SPE) cartridges prior to the id