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目的采用LC-MS/MS法测定人血浆中盐酸伪麻黄碱的血药浓度。方法血浆样品经液-液萃取,结合液-液反相萃取的方法处理,采用DiamonsilTM C18柱(150mm×4.6mm,5μm),以甲醇-10mmol·L-1醋酸铵(冰醋酸调pH4)(20∶80)为流动相,LC-MS/MS用正离子电喷雾离子源(ESI+)、离子选择通道为盐酸伪麻黄碱(m/z166→148)、磷酸可待因内标(m/z300→191)。结果盐酸伪麻黄碱血药浓度5.065～1.013×103ng·ml-1与检测信号具有良好的线性关系(r=0.9986),最低定量浓度为1ng·ml-1。低、次低、中、高浓度的盐酸伪麻黄碱的萃取回收率分别为86.86%±5.8%、95.24%±4.31%、96.91%±1.75%、92.60%±7.79%;内标的萃取回收率为86.24%±3.86%。盐酸伪麻黄碱的日内、日间RSD均小于11.7%。结论所建方法适用于盐酸伪麻黄碱的生物等效性及药物动力学的研究。
Objective To determine the plasma concentration of pseudoephedrine hydrochloride in human plasma by LC-MS / MS. Methods The plasma samples were treated with liquid-liquid extraction combined with liquid-liquid reverse phase extraction. The samples were separated on a DiamonsilTM C18 column (150mm × 4.6mm, 5μm) with methanol-10mmol·L-1 ammonium acetate 20:80) was used as the mobile phase. Positive ion electrospray ionization (ESI +) was used for LC-MS / MS. The ion channel was pseudoephedrine hydrochloride (m / z 166 → 148) ). Results The plasma concentration of pseudoephedrine hydrochloride was 5.065-1.013 × 103 ng · ml-1 with a good linear relationship (r = 0.9986) and the lowest concentration was 1 ng · ml-1. The recoveries of low, middle, low and medium concentrations of pseudoephedrine hydrochloride were 86.86% ± 5.8%, 95.24% ± 4.31%, 96.91% ± 1.75% and 92.60% ± 7.79%, respectively. The internal standard extraction recoveries were 86.24% ± 3.86%. Intra-day and inter-day RSD of pseudoephedrine hydrochloride were less than 11.7%. Conclusion The proposed method is suitable for the study of bioequivalence and pharmacokinetics of pseudoephedrine hydrochloride.