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建立了HPLC-MS法测定人血浆中茴拉西坦代谢产物对甲氧基苯甲酰胺基丁酸(2)的浓度。以N,N-二甲基-3,4-亚甲氧基苯乙胺(3)为内标,采用Thermo C18色谱柱,流动相为30mmol/L乙酸铵溶液(含0.5%甲酸和0.01%三氟乙酸)-乙腈(84:16),HPLC-MS采用ESI+电离源,选择正离子检测模式,检测的离子为m/z 135(2,M+H)和163(3,M+ H)。2在0.058~14.03μg/ml浓度范围内线性良好,回收率在90%以上。18名健康志愿者口服茴拉西坦胶囊0.2g后的药动学参数AUC0→t、AUC0→∞、tmax、Cmax和t1/2分别为(9.21±1.72)μg·h·ml-1、(9.30±1.75)μg·h·ml-1、(0.47±0.11)h、(9.44±2.13)μg/ml和(0.66±0.10)h。
A HPLC-MS method was established for the determination of p-anisamidobutyric acid (2) in the plasma of aniracetam in human plasma. Using N, N-dimethyl-3,4-methyleneoxy-phenethylamine (3) as internal standard and Thermo C18 column, the mobile phase consisted of 30mmol / L ammonium acetate solution 0.01% trifluoroacetic acid) -acetonitrile (84:16). The positive ion detection mode was selected by ESI-MS using HPLC-MS. The detected ions were m / z 135 (2, M + H). 2 in the range of 0.058 ~ 14.03μg / ml linearity was good, the recovery rate was above 90%. The pharmacokinetic parameters AUC0 → t, AUC0 → ∞, tmax, Cmax and t1 / 2 of 9.2 healthy volunteers were 9.21 ± 1.72 μg · h · (9.30 ± 1.75) μg · h · ml-1, (0.47 ± 0.11) h, (9.44 ± 2.13) μg / ml and (0.66 ± 0.10) h.