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目的:建立灵敏的液相色谱-串联质谱法测定人血浆中替扎尼定的浓度。方法:血浆样品碱化后经乙醚液-液萃取,以甲醇-10 mmo·lL-1醋酸铵-甲酸(55∶45∶0.1,v/v/v)为流动相,采用Zorbax SB C18柱(150 mm×4.6 mm,5μm)分离,通过电喷雾电离源,以选择反应监测(SRM)方式进行正离子检测,用于定量分析的离子反应分别为m/z254→44(替扎尼定)和m/z243→210(内标,石杉碱甲)。结果:测定血浆中替扎尼定方法的线性范围为10.0～5000 pg·mL-1,定量下限可达10.0 pg·mL-1。日内、日间精密度(RSD)均小于10.0%,准确度(RE)在±3.6%以内。结论:本方法灵敏度高,血浆用量少,适用于替扎尼定制剂的人体药物动力学研究。
Objective: To establish a sensitive liquid chromatography-tandem mass spectrometry for the determination of tizanidine concentration in human plasma. Methods: The plasma samples were alkalized and extracted with ether-liquid. The mobile phase was methanol-10 mmo · L 1 -ammonium acetate-formic acid (55:45:0.1, v / v / v) 150 mm × 4.6 mm, 5 μm). The positive ion was detected by electrospray ionization (ESI) and selective reaction monitoring (SRM). The ion reactions for quantitative analysis were m / z 254 → 44 m / z 243 → 210 (internal standard, huperzine A). Results: The linear range of tizanidine in plasma was 10.0-5000 pg · mL-1 and the lower limit of quantitation was 10.0 pg · mL-1. Day and day precision (RSD) were less than 10.0%, accuracy (RE) within ± 3.6%. Conclusion: The method has high sensitivity and less plasma dosage, which is suitable for human pharmacokinetic study of tizanidine.