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生物试样中巴比妥类药物固相提取柱上衍生化GC/MS分析
引用本文:李玉兰,徐建中,刘耀. 生物试样中巴比妥类药物固相提取柱上衍生化GC/MS分析[J]. 中国法医学杂志, 1998, 0(3)
作者姓名:李玉兰  徐建中  刘耀
作者单位:公安部物证鉴定中心!北京,100038,公安部物证鉴定中心!北京,100038,公安部物证鉴定中心!北京,100038
摘    要:建立生物试样中常见巴比妥类药物的固相提取和柱上衍生化GC/MS分析法。将预制的血或肝分别在pH6.0和pH2.2的条件下过预活化的GDX-403吸附小柱,再用缓冲浪和蒸馏水各4ml顺序洗柱。最后用4ml丙酮/氯仿(1:1)溶剂洗脱样品,离心弃除水相,80℃挥至近干,用50μl乙醇定溶、取净化的样品2~4μl挥至近干,加20μl0.2molTMAH衍生化试剂,直接进样0.5μl,柱上衍生化GC/MS(GC)分析。在试验条件下,当血和肝分别添加2.0μg和5.0μg混合药物,回收率≥80%,相对标准差(RSD)优于±10%,检测限优于5ng(信/噪比≥2)。该法能有效地排除类脂物和组胺的干扰,可用于治疗量级药物分析和婴幼儿中毒案检验。

关 键 词:固相提取  生物试样  巴比妥类  柱上衍生化GC/MS分析

Determination of barbiturates from biological tissues by solid-phase extraction,on-column derivatization GC/MS analysis
MS analysis/Li Yulan,et al.. Determination of barbiturates from biological tissues by solid-phase extraction,on-column derivatization GC/MS analysis[J]. Chinese Journal of Forensic Medicine, 1998, 0(3)
Authors:MS analysis/Li Yulan  et al.
Affiliation:MS analysis/Li Yulan,et al. /
Abstract:A method of SPE and on-column derivatization has been esteblished for analysis of barbiturates from biological tissues, GC/MS analysis. Speciments were prepared by adding 2. 0μg and 5. 0μg of barbiturates in blood and livers respectively, and then was purfied by GDX-403 column at pH 6. 0 and pH2. 2 (for livers), was finally analyzed by on-column derivatization. This method has a detection limits≤45ng. Accuracy precision was ±10 %. Recovery was ≥80 %. This method is sensitive, reliable and was used in cases work succesfully.
Keywords:Biological tissues Barbiturates SPE on-column Derivatization GC/MS analysis
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