气相色谱-质谱选择离子测定食品中33种农药和除草剂  

Determination of 33 weedicides and pesticides in foods by gas chromatography-mass spectrometry and selected ion monitoring

作　　者：于维森[1] 郝文[1] 段海平[1] 楼树青 

机构地区：[1]山东省青岛市疾病预防控制中心,山东青岛266033

出　　处：《中国卫生检验杂志》2009年第3期475-477,共3页Chinese Journal of Health Laboratory Technology

基　　金：国家"十一五"科技支撑计划项目-重大活动中食品安全保障技术研究与示范(2006BAK02A27);青岛市科技局立项课题(06-3-2-2NSH)

摘　　要：目的：建立一种测定食品中有机磷、拟除虫菊酯、有机氯、氨基甲酸酯和除草剂农药残留的气相色谱质谱方法。方法：本法采用丙酮、二氯甲烷提取,40℃水浴旋转蒸发近干,以Envi-Carb柱和Sep-Pak-NH2柱净化,以气相色谱-质谱选择离子监测方式分析检测有机磷、有机氯、拟除虫菊酯、氨基甲酸酯和除草剂等33种农药残留。结果：所有33种农药均在34 min内流出,分离良好,农药标准的线性范围在0.01～1.0μg/ml,相关系数r均在0.99以上,低、高二种浓度加标回收率均在89%～98%之间,相对标准偏差均小于10%,方法最低检出限在0.001～0.005 mg/kg（S/N=3）。结论：方法选择性强,适合于食品中有机磷、有机氯、拟除虫菊酯、氨基甲酸酯和除草剂农药残留的测定,且准确度好,精密度高,可快速一次检测33种农药,达到残留量检测中所要求的检测浓度水平。Objective：To establish a method for determination of 33 organophosphorus,pyrethroid,organochlorine,carbamate and weedicide pesticides in foods by gas chromatography-mass spectrometry（GC-MS） and selected ion monitoring（SIM）.Methods：The pesticides were extracted with acetone and dichloromethane.The extract was warmed with water at 80℃,circumrotated and evaporated until it was nearly dry.Then it was cleaned up by Envi-Carb column and Sep-Pak-NH2 column.The analysis was performed by GC-MS and SIM.Retention time and specific ions were used to confirm the pesticides.Results：The calibration curves of 33 pesticides were linear（correlation coefficient r〉0.99） within the range of 0.01～1.0 μg/ml.The recoveries were 89%～98%,the relative standard deviations（RSD） of the method was 〈10% for each case,and the limit of determination（LOD）,defined in terms of 3 times baseline noise was 0.001～0.005 mg/kg.Conclusion：The method is suitable for determining pesticides in foods with satisfactory sensitivity,accurcy and precision.

关 键 词：食品 农药 气相色谱-质谱分析 选择离子监测方式 

分 类 号：O657.63[理学—分析化学]