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目的建立高效液相色谱-串联质谱法(HPLC-MS/MS)测定汗液中美托洛尔(metoprolol,MET)及其代谢产物α-羟化美托洛尔(α-hydro-metoprolol,α-MET)的质量浓度。方法采用Finnigan液相色谱仪串联LXQ离子阱质谱仪检测,流动相为乙腈-甲醇-体积分数0.1%甲酸水溶液(体积比20∶20∶60),采用SRM模式,正离子模式监测。采用内标法计算待测样品的质量浓度,内标物为盐酸普萘洛尔(proprandoIhydroc.hloride,PRO)。结果MET在载药量0.5~50ng内、α-MET在载药量2.5~50ng内线性关系良好;MET(α-MET)低、中、高三个质量浓度的回收率分别为89.9%(89.5%)、103.5%(83.6%)和92.5%(87.3%);汗液中MET检出时间为服药后1~18h,α-MET检出时间为服药后2~16h。结论本方法适用于同时测定汗液中美托洛尔及其代谢产物的含量,可为药物的体外监测提供参考。
Objective To establish a HPLC-MS / MS method for the determination of metoprolol (MET) and its metabolite α-hydro-metoprolol (α- MET) mass concentration. Methods Finnigan liquid chromatography tandem LXQ ion trap mass spectrometry was used. The mobile phase consisted of acetonitrile - methanol - 0.1% formic acid solution (20:20:20 by volume) and monitored by SRM mode and positive mode. The internal standard method was used to calculate the mass concentration of the sample to be tested. The internal standard was proprandol hydrochloride (PRO). Results MET had a good linearity within the range of 0.5-50ng. The recoveries of MET (α-MET) were 89.9% (89.5% ), 103.5% (83.6%) and 92.5% (87.3%) respectively. The detection time of MET in sweat was 1 ~ 18h after taking the medicine and the detection time of α-MET was 2 ~ 16h after taking the medicine. Conclusion This method is suitable for the simultaneous determination of metoprolol and its metabolites in sweat, which can provide reference for the in vitro monitoring of drugs.