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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。
OBJECTIVE To establish a method for the determination of benzodiazepines in human whole blood using solid-phase extraction micellar electrokinetic capillary chromatography. Methods Whole blood was extracted with Oasis cartridges. Clenbuterol was used as an internal standard. Uncoated capillaries (75μmID × 50.2cm, effective separation length of 40cm) were used. The buffer was 30mmol / L DSDS → 15mmol / L borax → 15mmol / L phosphate (pH 8.2) → 18% methanol. Injection conditions: pressure injection 0.5psi × 10s, separation voltage of 25kV, column temperature 25 ℃, detection wavelength of 230nm. Results The separation efficiency of this method was high. The minimum detectable concentration of 9 benzodiazepines was 5 ~ 50ng / ml. The linear range of plasma concentration was 0.02 ~ 1.6μg / ml. The intra- and inter-day precision was < 12%. Conclusion This method is simple, efficient and reliable.