生物试样中巴比妥类药物固相提取柱上衍生化GC/MS分析

Determination of barbiturates from biological tissues by solid-phase extraction,on-column derivatization GC/MS analysis

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。

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.