LC-MS法测定曲马多在人体中的血药浓度

目的建立LC-MS法测定曲马多在血浆中的浓度。方法血浆样品经过饱和NaHCO3溶液碱化后,用乙酸乙酯萃取;流动相为甲醇-10 mmol/L(含0.5%甲酸)的醋酸铵水溶液(60︰40,v/v),流速为1.0 ml/min,采用电喷雾离子化(ESI),以选择性离子检测(SIM)方式进行检测。结果曲马多的线性范围在5.075～609.0 ng/ml,最低定量限为5.075 ng/ml,方法提取回收率为82.7%～85.9%,相对回收率为97.9%～102.0%,日内日间RSD均<10%。结论本方法准确,灵敏,重现性好,可用于曲马多血药浓度的检测及药动学的相关研究。

Determination of Concentration of Tramadol in Human Plasma by HPLC-MS/MS

Objective To establish an HPLC-MS/MS method for the determination of concentration of tramadol in human plasma.Methods Plasma samples were alkalized with saturative CH3COOC2H5.The mobile phase was ammonium acetate buffer(40∶60,v/v) containing 0.5% formic acid-methanol-10 mmol/L,the flow rate was 1.0 ml/min.The samples were subsequently analyzed by mass spectrometry with an ESI source and then quantified by selected reaction monitoring mode(SIM).Results The linear calibration curves of tramadol were in the range of 5.075-609.0 ng/ml,and the lowest determination limit was 5.075 ng/ml.The extraction recoveries of tramadol were 82.7%-85.9%,the relative recoveries of tramadol were 97.9%-102.0%,and RSDs of within-day and between-day were lower than 10%.Conclusion This method is sensitive and reproducible,and the results are reliable and accurate.