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全血中17种农药同时测定的固相萃取气相色谱质谱法 被引量:3

Determination method for 17 pesticides in common in whole blood by gas chromatogvaphy coupled to mass spectrometry with solid-phase extraction sample cleanup
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摘要 目的 建立同时检测全血中17种常见农药的固相萃取净化气相色谱-质谱(SPE-GC-MS)检测方法.方法 全血样品用乙腈提取,Oasis HLB固相萃取柱净化,用气相色谱进行分离,选择离子扫描监测(SIM)的质谱扫描模式下定量分析.结果 全血中17种农药添加浓度在1.0~5.0 mg/L之间,加标回收率为41.3%~102.1%,大部分农药的相对标准偏差<10%,17种农药在0.5~5.0 mg/L浓度范围线性关系良好,相关系数为0.9945 ~0.9994,定量检出限为0.05~0.09 mg/L.结论 该方法能够将全血中17种农药进行良好的分离测定,有较高的灵敏度、准确度和精密度,可满足中毒血样中多种农药的定性及定量检测分析的要求. Objective To establish a method for simultaneous determination of 17 common pesticides in whole blood by solid phase extraction-gas chromatography-mass spectrometry (SPE-GC-MS).Methods Whole blood samples were treated by extraction with acetonitrile,and the obtained extract was cleaned up using an Oasis HLB SPE cartridge; pesticides were separated by GC and quantitatively analyzed by MS with selected ion monitoring.Results The concentrations of 17 pesticides in whole blood were 1.0-5.0 mg/L,and the recovery rate was 41.3-102.1%,with a relative standard deviation of less than 10% in most pesticides.The 17 pesticides showed a good linear relationship between concentration and peak area within 0.5-5.0 mg/L,with a correlation coefficient of 0.9945-0.9994.The limit of detection and limit of quantification were 0.02-0.05 mg/L and 0.05-0.09 mg/L,respectively.Conclusion With this method,17 pesticides in whole blood can be well separated and determined.This method has high sensitivity,accuracy,and precision and can be used for identification and quantification of muhiple pesticides in blood samples.
出处 《中华劳动卫生职业病杂志》 CAS CSCD 北大核心 2013年第9期709-712,共4页 Chinese Journal of Industrial Hygiene and Occupational Diseases
关键词 血液 农药 色谱法 气相 Blood Pesticides Chromatography, gas
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