色谱

色谱

• 研究论文 • 上一篇    下一篇

快速溶剂萃取-气相色谱法同时测定含脂羊毛中的28种有机氯拟除虫菊酯杀虫剂的残留量

樊苑牧,黄绍棠,俞雪钧,顾晓俊,裘亚钧,湛嘉,陈树兵,贺小雨,陈俊,王时杰,李亚萍,李忠榜   

  1. Ningbo Entry-Exit Inspection and Quarantine Bureau, Ningbo 315012, China
  • 收稿日期:2008-10-27 修回日期:2008-10-27 出版日期:2008-10-27 发布日期:1983-09-25
  • 通讯作者: 樊苑牧
  • 基金资助:
    国家质检总局科研项目(2006IK021)和宁波市科研项目(2005C100095).

Determination of 28 organochlorine and synthetic pyrethroid pesticides in greasy wool using accelerated solvent extraction technique and gas chromatography

FAN Yuanmu, HUANG Shaotang, YU Xuejun, GU Xiaojun, QIU Yajun, ZHAN Jia, CHEN Shubing, HE Xiaoyu, CHEN Jun, WANG Shijie, LI Yaping, LI Zhongbang   

  1. Ningbo Entry-Exit Inspection and Quarantine Bureau, Ningbo 315012, China
  • Received:2008-10-27 Revised:2008-10-27 Online:2008-10-27 Published:1983-09-25
  • Contact: FAN Yuanmu

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621

被引次数

22

摘要： 建立了快速溶剂萃取-气相色谱法同时测定含脂羊毛中28种有机氯、拟除虫菊酯杀虫剂残留量的方法。在80 ℃、10.34 MPa条件下用正己烷饱和的乙腈快速提取样品,提取物经冷冻除脂、浓缩、固相萃取净化处理后直接用气相色谱分析。结果表明:16种有机氯杀虫剂在0.005～1.0 mg/L范围内,9种拟除虫菊酯杀虫剂及三氯杀螨醇、三氯杀螨砜在0.01～2.0 mg/L范围内,氟氯苯菊酯在0.02～4.0 mg/L范围内,其峰面积与质量浓度呈良好的线性关系。28种有机氯、拟除虫菊酯杀虫剂的平均回收率为67.2%～107.7%,相对标准偏差为2.6%～29.0%。结果表明：该方法具有操作简便、快速方便、灵敏度高等特点,完全可满足含脂羊毛中28种有机氯拟除虫菊酯杀虫剂残留量初筛检测的要求。

关键词: 含脂羊毛 , 快速溶剂萃取法, 拟除虫菊酯杀虫剂, 气相色谱法-电子捕获检测, 气相色谱-质谱, 有机氯杀虫剂

Abstract: A method for the simultaneous determination of 28 organochlorine and synthetic pyrethroid pesticides in greasy wool was developed by accelerated solvent extraction (ASE) coupled with gas chromatography-electron capture detection (GC-ECD). The organochlorine and synthetic pyrethroid pesticides in greasy wool were extracted with acetonitrile saturated with n-hexane at 80 ℃, 10.34 MPa by ASE. The extract was pretreated by a series of procedures such as freezing-lipid filtration, concentration and purification by solid-phase extraction prior to the determination with GC-ECD. The linear ranges were 0.005-1.0 mg/L for 16 organochlorines, 0.02-4.0 mg/L for flumethrin and 0.01-2.0 mg/L for the others. There were good linear relationships between the peak area and concentration in the linear ranges. The average recoveries of 28 organochlorine and synthetic pyrethroid pesticides were 67.2%-107.7%, and the relative standard deviations were 2.6%-29.0%. The method is simple, sensitive and suitable for preliminary screening of organochlorine and synthetic pyrethroid pesticides in greasy wool.

Key words: gas chromatography-electron capture detection (GC-ECD), gas chromatography-mass spectrometry (GC-MS), greasy wool , organochlorine pesticides (OCs), synthetic pyrethroid pesticides (SPs), accelerated solvent extraction (ASE)