%0 Journal Article %T Enantiomeric separation of propranolol by normal phase chiral liquid chromatography coupled with tandem mass spectrometry
正相液相色谱-串联质谱法分离普萘洛尔对映体 %A ZHANG Juanhong %A WANG Rong %A XIE Hua %A MENG Xiandong %A JIA Zhengping %A MA Jun %A ZHANG Junli %A WANG Juan %A
张娟红 %A 王荣 %A 谢华 %A 孟宪栋 %A 贾正平 %A 马骏 %A 张军莉 %A 王娟 %J 色谱 %D 2011 %I %X A rapid and sensitive method was developed and validated using a normal phase liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) for determination of propranolol enantiomers in pharmaceuticals. Sample preparation involved a single extraction step by the addition of methanol. Separation of propranolol enantiomers was achieved on a Chiralcel OD-H chiral column using a mobile phase consisting of n-hexane-ethanol-ammonia (70:30:0.4, v/v/v), and the flow rate was 0.40 mL/min for 20 min. The analyte was monitored by tandem mass spectrometry with electrospray positive ionization in multiple reaction monitoring (MRM) mode, using the transitions of m/z 260.2→116.0. Propranolol enantiomers can be completely separated. The linear range was 2.5~1000 μg/L, and the limit of quantification (LOQ) was 2.5 μg/L. The values for within day and between day precisions and accuracies were well within the generally accepted criteria for analytical methods. The relative standard deviations (RSDs) were less than 2.64%, and the recoveries of the two enantiomers were 99.08%~102.58% and 100.21%~103.16%, respectively. The separation method is accurate, convenient, reliable, efficient, and can be subsequently used for quality control of propranolol enantiomers in pharmaceuticals. %K normal phase liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) %K chiral separation %K determination %K propranolol enantiomers
正相液相色谱-串联质谱 %K 手性分离 %K 测定 %K 普萘洛尔对映体 %U http://www.alljournals.cn/get_abstract_url.aspx?pcid=6E709DC38FA1D09A4B578DD0906875B5B44D4D294832BB8E&cid=6579068328FE643F&jid=4D81E042D77AFEC6881D14759692069C&aid=3DC827A58B9472C7CCE478D77E95A4BE&yid=9377ED8094509821&vid=771469D9D58C34FF&iid=CA4FD0336C81A37A&sid=96C778EE049EE47D&eid=340AC2BF8E7AB4FD&journal_id=1000-8713&journal_name=色谱&referenced_num=0&reference_num=41