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目的:建立LC-MS/MS法同时检测卡巴拉汀及其代谢物NAP226-90血药浓度。方法:血浆经甲基叔丁基醚-二氯甲烷提取预处理,用Phenomenex-curocil PFP(250 mm×4.6 mm,5μm)色谱柱,0.1%甲酸0.05%甲酸铵溶液-0.1%甲酸0.05%甲酸铵甲醇为流动相,梯度洗脱分离,ESI正离子化三重四极杆质谱MRM测定,检测反应离子对:卡巴拉汀m/z 251.0→206.0、NAP226-90m/z 166.0→121.0、内标(美托洛尔)m/z 268.4→74.3。结果:卡巴拉汀及NAP226-90血药浓度在0.2~30 ng·m L~(-1)范围内均线性关系良好,定量下限均为0.2 ng·m L~(-1),经方法学验证符合生物样品测定要求。结论:建立的LC-MS/MS方法可用于重酒石酸卡巴拉汀胶囊人体药动学研究。
Objective: To establish a LC-MS / MS method for the simultaneous determination of rivastigmine and its metabolite NAP226-90 in plasma. Methods: The plasma was pretreated with methyl t-butyl ether-methylene chloride and the residue was chromatographed on a Phenomenex-curocil PFP (250 mm × 4.6 mm, 5 μm) column with 0.1% formic acid 0.05% ammonium formate solution - 0.1% formic acid 0.05% formic acid Ammonium methanolate as mobile phase, gradient elution and ESI positive ionized triple quadrupole mass spectrometry (MRM) were used to detect the reactive ion pairs: rivastigmine m / z 251.0 → 206.0, NAP226-90m / z 166.0 → 121.0, Metoprolol) m / z 268.4 → 74.3. Results: The linear relationship between rivastigmine and NAP226-90 in the range of 0.2-30 ng · m L -1 was good, and the lower limit of quantitation was 0.2 ng · m L -1. Validation meets biological sample determination requirements. Conclusion: The established LC-MS / MS method can be applied to the pharmacokinetics of rivastigrednibatidine capsules.