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目的:建立同时测定人血浆中地西泮、奥沙西泮、咪达唑仑和1′-羟基咪哒唑仑浓度的固相萃取-高效液相测定方法,并将其应用于临床中地西泮、咪达唑仑及其代谢产物血药浓度的测定。方法:以卡马西平为内标,血浆样品经Cleanert C18固相萃取柱净化处理。色谱柱为WondaSil C18柱(150 mm×4.6 mm,5μm),流动相为乙腈-水=55∶45,柱温:30℃,流速:1.2mL·min-1,检测波长:308 nm,进样量:30μL。结果:地西泮、奥沙西泮、咪达唑仑和1’-羟基咪哒唑仑标准曲线范围分别为0.5~20,0.2~10,0.5~40,0.5~20 mg·L~(-1),最低定量限分别为0.5,0.2,0.5,0.5 mg·L~(-1),方法回收率分别为88.32%~93.77%,86.14%~91.80%,87.55%~92.53%,88.69%~92.30%,日内、日间精密度均小于7%。结论:该方法简便快速,灵敏准确,测定结果可靠,适用于地西泮、咪达唑仑及其代谢产物血药浓度的检测。
OBJECTIVE: To establish a method for the simultaneous determination of diazepam, oxazepam, midazolam and 1’-hydroxymidazolam in human plasma by solid-phase extraction and high performance liquid chromatography Determination of plasma concentration of diazepam, midazolam and their metabolites. Methods: Carbamazepine was used as internal standard. The plasma samples were cleaned up with Cleanert C18 solid phase extraction column. The column was a Wonda Sil C18 column (150 mm × 4.6 mm, 5 μm). The mobile phase was acetonitrile-water = 55:45, the column temperature was 30 ℃, the flow rate was 1.2 mL · min -1, the detection wavelength was 308 nm, Amount: 30 μL. Results: The calibration curves of diazepam, oxazepam, midazolam and 1’-hydroxymidazolam ranged from 0.5 to 20, from 0.2 to 10, from 0.5 to 40 and from 0.5 to 20 mg · L ~ (-1) 1, the lowest limit of quantitation was 0.5, 0.2, 0.5 and 0.5 mg · L -1, respectively. The recoveries were 88.32% ~ 93.77%, 86.14% ~ 91.80%, 87.55% ~ 92.53%, 88.69% 92.30%, day, day precision less than 7%. Conclusion: The method is simple, rapid and sensitive, accurate and reliable. It is suitable for the determination of plasma concentration of diazepam, midazolam and its metabolites.