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气质联用选择离子一次测定食品中32种农药和除草剂 被引量:6

Determination of 32 weedicides and pesticides in foods by gas chromatography-mass spectrometry and selected ion monitoring
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摘要 目的:建立一种测定食品中有机磷、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、氨基甲酸酯和除草剂等32种农药残留。结果:所有32种农药均在37 m in内流出,分离良好,农药标准的线性范围在0.05-1.0μg/m l,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%,方法最低检出限为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、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32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, 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 confiIm the pesticides. Results:The calibration curves of 32 pesticides were linear( correlation coefficient r 〉0. 99) within the range of 0.05 - 1.0 μg/ml. The recoveries were 90% 96%, 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. 005 mg/kg. Conclusion: The method is suitable for determining pesticides in foods with satisfactory sensitivity, accuracy and precision.
出处 《中国卫生检验杂志》 CAS 2009年第5期1029-1031,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)
关键词 食品 农药 气相色谱-质谱分析 选择离子监测方式 Foods Pesticides Gas chromatography-mass spectrometry(GC -MS) Selected ion monitoring(SIM)
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参考文献4

  • 1GB/T5009.145-2003.植物性食品中有机磷和氨基甲酸酯农药多种残留的测定[S].
  • 2GB/T19426-2006.蜂蜜、果汁和果酒中497种农药及相关化学品残留量的测定[S].
  • 3Gregory E Mercer,Jeffrey A. A multiresidue pesticide monitoring procedure using gas chromatography/mass spectrometry and selected ion monitoring for the determination of pesticides containing nitrogen, sulfur, and/or oxygen in fruits and vegetables [ J ]. AOAC, 87 ( 5 ) : 1224 - 1236.
  • 4Michelangelo Anastassiaoles, Steven J Lehotay, Darinka Stajnbaher, et al. Fast and easy mnltiresidue method employing acetonitrile extraction/partitioning and " dispersine - phase exlraction" for the determination of pesticide residues in produce [ J ]. AOAC, 86 ( 2 ) :412 - 431.

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