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目的:建立同时测定术后患者应用曲马多后的曲马多和活性代谢物O-脱甲基曲马多(M1)血药浓度的方法。方法:血浆样品50μl以乙腈溶液150μl(含内标氟康唑)沉淀蛋白处理后,采用液-质联用(LC-MS/MS)法进样测定,色谱柱为Zorbax SB-C18,流动相为0.1%甲酸-5 mmol/L乙酸铵溶液-0.1%甲酸乙腈溶液(梯度洗脱);用于定量分析的离子反应m/z分别为曲马多264.2→58.6、M1250.0→58.6、氟康唑307→220。结果:2种待分析物血药浓度均在5~1 000 ng/ml范围内线性关系良好,日内、日间RSD均<10%;方法回收率分别为92.26%~100.01%、88.45%~100.60%。结论:本方法准确、快速、灵敏,可用于曲马多和M1的血药浓度测定及药动学研究。
Objective: To establish a method for the simultaneous determination of tramadol and the active metabolite O-demethyltramadol (M1) in patients after tramadol administration. Methods: 50μl of plasma samples were treated with 150μl of acetonitrile solution (containing fluconazole as precipitated protein) and determined by liquid chromatography-mass spectrometry (LC-MS / MS). The chromatographic column was Zorbax SB-C18 with mobile phase 0.1% formic acid-5 mmol / L ammonium acetate solution-0.1% formic acid in acetonitrile (gradient elution); the ion reaction m / z for quantitative analysis was tramadol 264.2 → 58.6, M1250.0 → 58.6, Conazole 307 → 220. Results: The two analytes had good linearity in the range of 5-1 000 ng / ml with daily RSD <10%, and the recoveries were 92.26% -100.01% and 88.45% -100.60 %. Conclusion: The method is accurate, rapid and sensitive and can be used for the determination of plasma concentration and pharmacokinetics of tramadol and M1.