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目的:建立固相萃取-反相高效液相色谱法测定人血浆中氯硝西泮(clonazepam,CZP)浓度。方法:采用SU-PELCLEAN萃取小柱提取血浆中CZP,以HPLC法测定药物浓度。色谱条件:Shim-Pack VP-ODS(150mm×4.6mm,5μm)分析柱,保护柱为Shim-Pack GVP-ODS柱(10mm×4.6mm,5μm);流动相为乙腈-水(37∶63);流速1.0mL.min-1;检测波长308nm;柱温30℃。结果:CZP与血浆中内源杂质分离良好,tR=9.8min,线性范围19~114μg.L-1(r=0.993,n=6),最低检测限19μg.L-1。固相萃取回收率在90.6%~97.7%之间。结论:该方法灵敏、准确,萃取回收率高,适用于临床氯硝西泮的血药浓度监测。
Objective: To establish a method for the determination of clonazepam (CZP) in human plasma by solid-phase extraction-reverse-phase high performance liquid chromatography. Methods: The CZP in plasma was extracted with SU-PELCLEAN extraction cartridge and the drug concentration was determined by HPLC. The chromatographic conditions were: Shim-Pack VP-ODS (150 mm × 4.6 mm, 5 μm) analytical column with a guard column of Shim-Pack GVP-ODS (10 mm × 4.6 mm, ; Flow rate 1.0mL.min-1; detection wavelength 308nm; column temperature 30 ℃. Results: The separation of endogenous impurities from CZP was good with tR = 9.8 min, linear range 19-114 μg.L-1 (r = 0.993, n = 6) and the lowest detection limit was 19 μg.L-1. Solid phase extraction recoveries ranged from 90.6% to 97.7%. Conclusion: The method is sensitive, accurate and has high extraction recovery rate. It is suitable for the monitoring of clinical clonazepam blood concentration.