摘要
目的:建立气相色谱—选择离子质谱法(GC -MS/SIM )测定人体血液中麻黄碱(ephedrine ,E)、伪麻黄碱(pseu doephedrine ,PE)的浓度,以此进行麻黄汤药代动力学研究。方法:用GC MS/SIM法,HP 5弹性石英毛细管(2 5m×0 .2mmID) ,载气He ,柱流量1.0ml/min ,无分流进样,柱初温80℃,1min后以15℃/min升至2 0 0℃,再以2 0℃/min升至2 40℃,保持5min ,选择离子(SIM ,m /z =15 4,2 65 ) ,进样量1μl。结果:E、PE分别在5ng/ml～10 0 0ng/ml,2 .5ng/ml～5 0 0ng/ml范围内与峰面积比值呈良好的线性关系(r =0 .9988,r =0 .9994) ,最低检测浓度分别为2ng/ml ,1ng/ml(S/N =3 )。加样回收率分别为10 7.5 %～96.2 % ,10 2 .5 %～93 .9%。两者日内、日间精密度的RSD <10 %。血浆样品60天内稳定性RSD <10 %。用本法测定了12名志愿者口服麻黄汤后血浆中药物浓度经时变化过程,并对其药动学参数进行估算。结论:本法稳定、准确,灵敏度高,适于E、PE的动力学研究。
Objective: To develop a GC-MS/SIM method for the determination of ephedrine and pseudoephdrine and study the pharmacokinetics of the two detected components in human plasma. Methods: Gas chromatography-mass spectrometry with selected ion monitoring (GC-MS/SIM) was used. Chromatography/mass spectrometry conditions were: capillary column HP-5(25m×0.2mmID), Helium as carrier gas, with 1.0ml/min runoff, non-split injection , column initial temperature 80℃,after 1 min rising to 200 ℃ at the rate 10℃/min, and then rising to 240℃ at the rate of 20℃/min and holding for 5 minutes. Choosing SIM (m/z=154,265) and injection volume(1μl). Results: The calibration curves of E were linear in the range from 5 ng/ml to 1000 ng/ml (r=0.9985) and 2.5 ng/ml to 500 ng/ml (r=0.9994),the lowest detectable concentrations were 2ng/ml, 1 ng/ml (S/N=3), the recoveries added samples were from 107.5% to 96.2%, and from 102.5% to 93.9% for ephedrine and pseudoephedrine , respectively. The RSDs of interday and intraday were all less than 10%. The ephedrine and pseudoephedrine in tissue solution were steady within 60 days. The difference of the proportion main pharmacokinetics between ephedrine and pseudoephedrine parameters is significant. Conclusion: This method is precise and reliable to study ephedrine and pseudoephedrine in human plasma.
出处
《中药药理与临床》
CAS
CSCD
北大核心
2005年第1期1-3,共3页
Pharmacology and Clinics of Chinese Materia Medica
基金
国家自然科学基金重点资助项目 (No :30 0 30 1 50 )
