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目的:建立LC-MS/MS法测定人血浆中泮托拉唑的浓度。方法:人血浆样本以乙腈沉淀蛋白后,选用Zorbax SB-C18Narrow-Bore色谱柱(150 mm×2.1 mm,5μm),以甲醇-10 mmol.L-1乙酸铵(65∶35)为流动相,流速为0.40 mL.min-1;选用API3200型三重四极杆串联质谱仪的多重反应监测(MRM)扫描方式进行监测,电喷雾离子化源,正离子方式,选择监测离子反应分别为m/z 384.1→m/z 200.2(泮托拉唑)和m/z 370.1→m/z 252.0(内标兰索拉唑)。结果:泮托拉唑和兰索拉唑的保留时间分别为1.75 min和2.36 min;血浆中泮托拉唑的线性范围为0.0100～6.00 mg.L-1(r>0.99),定量下限为0.0100 mg.L-1;日内、日间相对标准差(RSD)均小于5%;相对偏差(RE)均在±4%的范围以内;平均提取回收率为(97.2±5.4)%;稳定性试验中,在各种贮存条件下血浆中泮托拉唑均较稳定。结论:该方法快速、灵敏、准确、专属性强、重现性好,适用于人血浆中泮托拉唑浓度的测定,可应用于泮托拉唑钠肠溶片的人体生物等效性研究。
Objective: To establish a method for the determination of the concentration of pantoprazole in human plasma by LC-MS / MS. METHODS: Human plasma samples were precipitated with acetonitrile. Zorbax SB-C18Narrow-Bore column (150 mm × 2.1 mm, 5 μm) and methanol-10 mmol·L-1 ammonium acetate (65:35) The flow rate was 0.40 mL · min-1. Multiplex reaction monitoring (MRM) scanning was performed with API3200 triple quadrupole mass spectrometer. The electrospray ionization source, positive ion mode and selective ion monitoring were m / z 384.1 → m / z 200.2 (pantoprazole) and m / z 370.1 → m / z 252.0 (internal standard Lansoprazole). Results: The retention time of pantoprazole and lansoprazole was 1.75 min and 2.36 min, respectively. The linear range of plasma pantoprazole was 0.0100 ~ 6.00 mg.L-1 (r> 0.99), and the lower limit of quantification was 0.0100 mg.L-1. The relative standard deviations (RSDs) were less than 5%, the relative deviations (REs) were all within ± 4%, and the average recovery was (97.2 ± 5.4)%. The stability test , The plasma pantoprazole is more stable under various storage conditions. Conclusion: The method is rapid, sensitive, accurate, specific and reproducible. It is suitable for the determination of pantoprazole concentration in human plasma and can be applied to the bioequivalence study of pantoprazole sodium enteric-coated tablets .