色谱

色谱

• 研究论文 • 上一篇    下一篇

双气相色谱-双脉冲火焰光度法高通量检测动物性食品中有机磷农药残留及其代谢产物

杨立新1,2,3, 李荷丽1, 苗虹1*, 曾凡刚2,李瑞丰1, 陈惠京1, 赵云峰1, 吴永宁1   

  1. 1. 中国疾病预防控制中心营养与食品安全所化学污染与健康安全重点实验室, 北京 100021; 2. 中国人民大学环境与资源学院, 北京 100872; 3. 河北省疾病预防控制中心, 河北 石家庄 050021
  • 收稿日期:2011-04-07 修回日期:2011-05-23 出版日期:2011-10-28 发布日期:2011-10-13
  • 通讯作者: 苗虹,研究员,研究方向为食品安全
  • 基金资助:

    卫生部卫生科研专项(No. 200902009)和“十一五”国家科技支撑计划课题(Nos. 2007BAC27B02, 2006BAK02A20)

High throuput analysis of organophosphorus pesticide residues and their metabolites in animal original foods by dual gas chromatography-dual pulse flame photometric detection

YANG Lixin1,2,3, LI Heli1, MIAO Hong1*, ZENG Fangang2, LI Ruifeng1, CHEN Huijing1, ZHAO Yunfeng1, WU Yongning1   

  1. 1. Key Laboratory of Chemical Safety and Health, National Institute of Nutrition and Food Safety, Chinese Centre for Disease Control and Prevention, Beijing 100021, China; 2. School of Environment and Nature Resources, Renmin University of China, Beijing 100872, China; 3. Hebei Centre for Disease Control and Prevention, Shijiazhuang 050021, China
  • Received:2011-04-07 Revised:2011-05-23 Online:2011-10-28 Published:2011-10-13

PDF

468

被引次数

18

摘要： 建立了动物性食品中包括代谢产物在内的54种有机磷农药残留及其代谢产物的双气相色谱-双脉冲火焰光度检测器(GC-PFPD)检测方法。动物组织样品经丙酮提取后以二氯甲烷进行液-液萃取,经凝胶渗透色谱净化后采用配有双脉冲火焰光度检测器的气相色谱仪测定。采用外标法定量,有机磷农药的响应与其浓度在线性范围内均呈良好的线性关系,相关系数在0.9905～0.9999之间。分别在空白鸡肉、羊肉、牛肉和猪肉样品中添加低、中和高3个加标水平的标准品进行了回收试验,回收率在50.5%～128.1%之间,相对标准偏差(n=6)在1.1%～25.5%之间,证明该方法的精密度和准确度良好。各有机磷农药的检出限在0.001～0.170 mg/kg之间,定量限在0.002～0.455 mg/kg之间。对从市场采集的动物组织样品进行了测定,检出敌敌畏、乙拌磷亚砜等有机磷农药残留。本方法灵敏度高、特异性强,且能同时检测有机磷农药多残留及其代谢产物,能够更加真实地反映动物性食品中有机磷农药的残留水平。

关键词: 代谢产物, 动物性食品, 凝胶渗透色谱净化, 双气相色谱-双脉冲火焰光度检测, 有机磷农药

Abstract: A method was established for quantitative determination of 45 organophosphorus pesticide residues and their metablites in animal original foods by dual gas spectrometry – dual pulse flame photometric detection. Homogenized samples were extracted with acetone and methylene chloride, and cleaned up by GPC. The response of each analyte showed a good linearity with its concentration with the linearity correlation not less than 0.99. The recovery experiments were performed by blank sample spiked at the low, medium and high fortification levels. The recoveries for beef, mutton, pork, chicken were in the range of 50.5 % ~ 128.1 % with the relative standard deviations (RSD, n=6) of 1.1 % ~ 24.4 %. The limits of detection for the analytes were in the range of 0.001 ~ 0.170 mg/kg, and the limits of quantification were in the range of 0.002 ~ 0.455 mg/kg. Animal original food samples collected from market such as meat, liver and kidney were analyzed, and residues of dichlorovis and disulfoton-sulfoxide were detected in some of those samples.

Key words: Animal original foods, Dual gas chromatography &ndash, Gel permeation chromatography cleanup, Metabolites, dual pulse flame photometric detection, Organophosphorus pesticides