Determination of the active metabolite of moguisteine in human plasma and urine by LC-ESI-MS method and its application in pharmacokinetic study
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摘要
In this study, a sensitive and reproducible electro-spray ionization liquid chromatography-mass spectrometry (LC-ESI-MS) method was established to determine the concentration of M1, the main active metabolite of moguisteine in human plasma and urine. The analysis was performed on a Diamonsil C18(2) column (150 mm 脳 4.6 mm, 5 渭m) with the mobile phase consisting of 0.1%formic acid-acetonitrile (57:43, v/v, pH = 3.0) at a flow rate of 0.8 mL min鈭?. The pseudo-molecular ions [M+H]+ (m/z 312.2 for M1 and 446.3 for glipizide) were selected as the target ions for quantification in the selected ion monitoring (SIM) mode. Plasma samples were analyzed after being processed by acidification with formic acid and protein precipitation with acetonitrile. Urine samples were appropriately diluted with blank urine for analysis. Calibration curve was ranged from 0.02 to 8 渭g mL鈭?. The extraction recovery in plasma was over 90%. Both the inter- and intra-day precision values were less than 7.5%, and the accuracy was in the range from 鈭?.0%to 6.0%. This is the first reported LC-ESI-MS method for analyzing M1 in human plasma and urine. The method was successfully applied to the pharmacokinetic study after oral administration of single-dose and multiple-dose of moguisteine tablets in healthy Chinese subjects.

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