摘要
目的建立一种同时测定人血浆中氯哌丁、氯苯那敏和伪麻黄碱的LC-MS,并用于含上述组分的复方酚咖伪麻胶囊人体药动学研究。方法以苯海拉明为内标,血样经乙酸乙酯提取后,采用LC-MS进行测定。色谱柱为Shim-packODS柱(150mm×2.0mm,5μm);流动相为含0.5‰冰醋酸和0.5mmol.L-1醋酸铵的水溶液及甲醇;检测离子为m/z330.1(氯哌丁)、m/z275.0(氯苯那敏)、m/z166.0(伪麻黄碱)及m/z256.15(内标);裂解电压为25V。结果氯哌丁、氯苯那敏和伪麻黄碱的线性范围分别为0.5~50.0,0.2~25.0和6.25~400.0ng.mL-1;最低可定量浓度分别为0.5,6.25和0.2ng.mL-1;日内、日间RSD小于10%,方法回收率均大于85%。结论该方法简便,快速,重复性好,灵敏度高,可用于含氯哌丁、伪麻黄碱和氯苯那敏的复方制剂临床药动学研究。
OBJECTIVE To establish an LC-MS tot simultaneous determine the concentration of cloperastine,chlorpheniramine and psedoephedrine in human plasma and to apply this method to the pharmacokinetic and bioavailability study of above components after oral administration of a compound preparation. METHODS Using diphenhydramin hydrochloric as internal standard, plasma was extracted with ethyl acetate and separated by a C18 column with the mobile phase of methanol-water ( including 0.5‰ acetic acid and 0.5 mmol·L^-1 ammoniium acetate). I,C-MS was performed in the selected ion monitoring mode using target ions was at m/z 330.1 for cloperastine, m/z 275. 0 for chlorpheniramine, m/z 166. 0 for psedoephedrine and m/z 256. 15 for diphenhydramin hydrochloric( IS ). The fragmentor voltage was 25 V. RESULTS The linear range of cloperastine, chlorpheniramine and psedoephedrine in human plasma were 0.5 - 50.0,0.2 - 25.0 and 6.25 - 400.0 ng·mL^-1, respectively. The limit of determination were 0.5, 6.25 and 0.2 ng·mL^-1 , respectively. The recoveries of methodology were all more than 85%. The inter-day and intra-day RSI) were all less then 10%. CONCLUSION This method has good sensitivity and precision. It is shown to be suitable for pharmacokinetics studies of different compound preparations containing low dosage of cloperastine,chlorpheniramine,psedoephedrine.
出处
《中国现代应用药学》
CAS
CSCD
北大核心
2009年第2期106-108,共3页
Chinese Journal of Modern Applied Pharmacy