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目的 建立曲马多血药浓度的高效液相色谱-质谱测定法,用于人体药动学研究。方法 血浆样品用饱和碳酸氢钠碱化,用乙酸乙酯提取。采用AgilentZorbaxSB C18(15 .0mm×2 . 1mm ,5 μm)柱,以甲醇-水(含1%甲酸) =8∶14 (V/V)为流动相,内标为盐酸非洛普,检测离子为m/z 36 4 . 5 (曲马多)、m/z344 . 5 (内标) ,裂解电压为12 0V。测定了2 0名受试者单剂量口服曲马多10 0mg后血药浓度。结果 最低检测限达0 . 5 μg·L-1,线性范围1～5. 0 0 μg·L-1(r =0 . 9996 ,n =5 ) ,日内和日间RSD均<10 % ,方法回收率为94 .2 %～10 .9 7% ,符合生物样品分析要求。结论 本法准确、快速、灵敏,适合曲马多的人体药动学研究。
Objective To establish a high performance liquid chromatography-mass spectrometry method for the determination of tramadol in human plasma. Methods Plasma samples were basified with saturated sodium bicarbonate and extracted with ethyl acetate. The mobile phase consisted of Agilent Zorbax SB C18 (15.0 mm × 2.1 mm, 5 μm) column with methanol-water (containing 1% formic acid) = 8:14 (V / V) M / z 36 4 5 (tramadol), m / z 344.5 (internal standard), the lysis voltage is 12 0V. The plasma concentration of 10 0 mg of tramadol administered orally to 20 subjects was measured. Results The lowest detection limit was 0.5 μg · L-1, with a linear range of 1 -5.0 0 μg · L-1 (r = 0.9996, n = 5) with RSD <10% The recoveries ranged from 94.2% to 10.97%, which met the requirements of biological sample analysis. Conclusion This method is accurate, rapid, sensitive and suitable for human pharmacokinetic study of tramadol.