全血中苯骈二氮杂类药物的胶束电动色谱法分析

目的建立用固相萃取胶束电动毛细管色谱法测定人体全血中苯骈二氮杂艹卓类药物的方法。方法全血以Oasis小柱提取,以克仑特罗为内标,采用未涂层毛细管(75μmID×50.2cm,有效分离长度为40cm),缓冲液为30mmol/LSDS→15mmol/L硼砂→15mmol/L磷酸盐(pH8.2)→18%甲醇。进样条件:压力进样0.5psi×10s,分离电压为25kV,柱温25℃,检测波长为230nm。结果本法分离效率高,9种苯骈二氮杂艹卓类药物的最低检测浓度为5～50ng/ml;血药浓度的线性范围为0.02～1.6μg/ml,日内、日间精密度<12%。结论本法简便、高效、可靠。

Determination of benzodiazepines in human whole blood by micellar electrokinetic capillary chromatography

Objective To develop a method for simultaneous determination of benzodiazepines in human whole blood by SPE-Micellar electrokinetic capillary chromatography.Methods With the Clenbuterol as internal standard,Oasis column was used to extract the drugs from whole blood.The separation was performed on a fused-silica capillary of 75μm ID×50.2cm(40cm of effect length).The running buffers were sequentially used as 15mmol/L phosphates→15mmol/L sodium borate(pH8.2)→30 mmol/L SDS,and 18% methanol served as an organic modifier.Sample solution was injected with pressure mode,and the running voltage was 25kV.The detection wavelength was set at 230nm.Results The linear ranges of the calibration curves were from 0.02 to 1.6μg/ml,and the limits of detection ranged between 5 ng/ml and 50 ng/ml.The within-day and between-day precision was less than 12%.Conclusion The method developed for determination of benzodiazepines in human whole blood is effective,simple and reliable,with which 9 benzodiazepines may be simultaneously separated.