食品中42种有机磷、拟除虫菊酯、有机氯、氨基甲酸酯和除草剂的气相色谱-质谱选择离子测定  

Determination of 42 organophosphorus,pyrethroid,organochlorine,carbamate and weedicide pesticides in foods by gas chromatography-mass spectrometry and selected ion monitoring

作　　者：于维森[1] 郝文[1] 于红卫[1] 曲青[1] 

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》2008年第11期2272-2274,2411,共4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42种农药残留。结果：所有42种农药均在38min内流出，分离良好，农药标准的线性范围在0．001～1．0μg／ml，相关系数r均在0．99以上，低、高2种浓度加标回收率均在89％～94％之间，相对标准偏差均小于10％，方法最低检出限在0．001～0．005mg／kg（S／N=3）。结论：方法选择性强，适合于食品中有机磷、拟除虫菊酯、有机氯、氨基甲酸酯和除草剂农药残留的测定，且准确度好，精密度高，可快速一次检测42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 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 diehloromethane. The extract was warmed with water at 80℃, cireumrotated and evaporated until it was nearly dry. Then it was cleaned - up by Envi - Carb column and Sep - Pak - NH2 column. The a- nalysis was performed by GC - MS and SIM. Retention time and specific ions were used to confirm the pesticides. Results： The calibration curves of 42 pesticides were linear（ correlation coefficient r 〉 0. 99 ） within the range of 0. 001 - 1.0μg/ml. The recov- eries were 89% - 94%, the relative standard deviations （RSD） of the method was 〈 10% for each case, and the limit of determi- nation （ 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]