【摘要】 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。更多还原

【Abstract】 OBJECTIVE:To establish the method for simultaneous determination of tramadol and active metabolite O-demethyl tramadol(M1)in the plasma of postoperative patients treated with tramadol. METHODS:Tramadol and M1 in plasma were determined simultaneously by LC-MS/MS after the plasma sample 50 μl was precipitated with acetonitrile 150 μl containing fluconazol.The determination was performed on Zorbax SB-C18 with mobile phase consisted of 0.1% formic acid-5 mmol/L ammonium acetate solution-0.1% formic acid acetonitrile solution(gradient elution);m/z was 264.2→58.6 for tramadol,250.0→58.6 for M1 and 307→220 for fluconazol. RESULTS:The linear range of tramadol and M1 both were 5-1 000 ng/ml;RSDs of intra-day and inter-day were lower than 10%;method recoveries were 92.26%-100.01% and 88.45%-100.60%. CONCLUSIONS:The method is accurate,rapid and sensitive,and can be used for the determination of plasma concentration of tramadol and M1 and pharmacokinetic study.更多还原