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| 固相萃取-GC/MS法检测生物检材中的百草枯 | |
| 引用本文： | 刘德伟,杨明,李剑波,刘云志,李永国.固相萃取-GC/MS法检测生物检材中的百草枯[J].中国法医学杂志,2013,28(1):41-43. |
| 作者姓名： | 刘德伟 杨明 李剑波 刘云志 李永国 |
| 作者单位： | 1. 重庆医科大学法医学教研室,重庆400016;重庆市刑事侦查工程技术研究中心,重庆400016;重庆法医验伤所,重庆400016 2. 南充市公安局,四川南充,637000 3. 重庆医科大学法医学教研室,重庆400016;重庆市刑事侦查工程技术研究中心,重庆400016 |
| 摘 要： | 目的采用固相萃取-气相色谱/质谱分析方法检测血液、尿液和脏器组织中的百草枯。方法人血液、尿液和猪肺组织样品经三氯乙酸去除蛋白后,取上清用十二烷基三甲基溴化铵和十二烷基硫酸钠处理过的C18小柱提取,提取物用硼氢化钠在碱性条件下还原,产物用气相色谱/质谱法分析,外标法定量。结果生物检材中百草枯回收率为78%～87%,最低检出限为0.1μg/mL,在0.5～1mg/mL范围内线性关系良好,可对实际案例检材进行定量检测。结论本文固相萃取-气相色谱/质谱分析方法能满足中毒生物检材检验及临床毒物检验需要。 |
| 关 键 词： | 法医毒物分析 百草枯 生物检材 固相萃取 气质联用分析 |
Determination of paraquat in human biological samples using SPE-GC/MS |
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| Liu Dewei,Yang Ming,Li Jianbo,Liu Yunzhi,Li Yongguo.Determination of paraquat in human biological samples using SPE-GC/MS[J].Chinese Journal of Forensic Medicine,2013,28(1):41-43. | |
| Authors: | Liu Dewei Yang Ming Li Jianbo Liu Yunzhi Li Yongguo |
| Institution: | 1,2/1.Department of Forensic,Basic Medicine College,Chongqing Medical University,Chongqing 400016,China;2.Chongqing Municipality Research Center of Criminal Investigation Technology,Chongqing 400016,China;3.Chongqing Institute of Forensic Medicine,Chongqing 400016,China;4.Nanchong Public Security,Sichuan Nanchong 637000,China) |
| Abstract: | Objective A procedure of solid phase extraction and gas chromatography(GC)with mass spectrometry(MS) was established for the determination of paraquat in human biological samples.Methods The biological samples were deproteinated by trichloroacetic acid.the supernate was cleaned up by C18-solid phase extraction cartridge pretreated by dodecyl trimethylammonium bromide and lauryl sodium sulfate,Then,target analyte was reducted by sodium borohydride under alkaline condition and analyzed by GC/MS using external standard method.Results The recoveries were 78%～87% and the limit of detection was 0.1μg/mL.A good linearity was obtained at the concentration of 0.5～1mg/mL and the method could be applied to analyse the forensic cases to quantitation.Conclusion The established SPE-GC/MS method could be in the service of the determination of paraguat in forensic sample and clinical sample. |
| Keywords: | forensic toxicological analysis paraquat biological sample solid phase extraction GC/MS |
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