色谱2011，Vol.29Issue(1)：26-30,5.DOI:10.3724/SP.J.1123.2011.00026
正相液相色谱-串联质谱法分离普萘洛尔对映体
Enantiomeric separation of propranolol by normal phase chiral liquid chromatography coupled with tandem mass spectrometry
摘要
Abstract
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 - l 000 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.关键词
正相液相色谱-串联质谱/手性分离/测定/普萘洛尔对映体分类
化学化工引用本文复制引用
张娟红,王荣,谢华,孟宪栋,贾正平,马骏,张军莉,王娟..正相液相色谱-串联质谱法分离普萘洛尔对映体[J].色谱,2011,29(1):26-30,5.基金项目
国家自然科学基金项目(No. 20775089)和甘肃省科技支撑计划项目(No. 1011FKCA144). （No. 20775089）
