摘要:
目的 建立人血浆中伪麻黄碱浓度的LC-MS/MS测定方法,并用该法研究西替伪麻缓释片在健康人体内的药动学。 方法 采用LC-MS/MS测定人血浆中不同时间点伪麻黄碱的浓度,以盐酸金刚烷胺为内标,血浆样品用乙腈沉淀蛋白,色谱柱为Agilent Zorbax SB-C18 (150 mm×2.1 mm, 3.5 μm),流动相为甲醇-0.1%甲酸水溶液(40∶60),流速0.3 ml/min,柱温30 ℃。 结果 伪麻黄碱的线性范围为2.5~1 000.0 ng/ml (r=0.995 2),最低定量检测浓度达2.5 ng/ml(S/N>10),提取回收率>78％,日内和日间RSD<15%。 结论 本法操作简单,选择性好,灵敏度高,适用于伪麻黄碱的药动学研究。
Abstract:
Objective To establish a LC-MS/MS method for the determination of pseudoephedrine concentration in plasma, and to investigate the pharmacokinetics of sustained release tablets of cetirizine hydrochloride and pseudoephedrine hydrochloride in Chinese healthy volunteers. Methods The plasma concentrations of pseudoephedrine were determined by LC-MS/MS method in the volunteers at different time points. Amantadine hydrochloride was used as internal standard. After precipitation of the plasma proteins with acetonitrile, the analytes were separated on an agilent zorbax SB-C18 reversed-phase column with methanol -0.1% formic acid (40:60, v/v) and detected by electrospray ionization (ESI) mass spectrometry in positive multiple reaction monitoring (MRM) mode. The flow rate was 0.3 ml/min. Column temperature was maintained at 30 ℃. Results The calibration curves with good linearities (r=0.995 2 for plasma sample) were obtained in the range of 2.5~1 000.0 ng/ml for pseudoephedrine. The lower limit of quantification (LLOQ) was 2.5 ng/ml. Recoveries were around 78% for the extraction from human plasma, and good precision and accuracy were achieved. The intra-day and inter-day RSD were less than 15.0%. Conclution This method was simple, selective and sensitive. It's suitable for the pharmacokinetic research of pseudoephedrine in human plasma.
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