摘要
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 pseudoephedrine hydrochloride （PSE） in human plasma by LC - MS/MS. METHODS The method of using liquid/liquid extraction from alkalized plasma conbined with back - extraction from the upper organic phase with 10% acetic acid. The mobile phase consisted of methanol/10 mmol·L^-1 ammonium acetate in water, pH4 （80 ： 20） and plasma samples were performed on a reversed - phase Diamonsil C18 column with a flow rate of 0.5 ml·min^-1 and analyzed by LC - MS/MS using positive eleetrospay ionization （ ESI＊ ）. Multiple reaction monitoring using the preeursor→pmduct ion combinations of m/z 166→148 and m/z 300→191 were used to quantify the PSE and the codeine phosphate （internal standard, IS）, respectively. RESULTS The assay exhibited a linear range of 5. 065 - 1.013 × 10^3 ng·ml^-1 for PSE and gave a mean correlation coefficient of 0.9986. The lower limit of quantification was 1.0 ng·ml^-1. The intra - and inter - batch precision were lower than 11.7%. The extraction recovery of each analyte and IS was 81.1% - 100.4%. CONCLUSION The method for determination the concentration of PSE in human plasma was proved to be applied to study the pharmacokinetics of PSE in human plasma.
出处
《华西药学杂志》
CAS
CSCD
北大核心
2010年第1期100-102,共3页
West China Journal of Pharmaceutical Sciences
