PMID- 21574396 OWN - NLM STAT- MEDLINE DCOM- 20120628 LR - 20190923 IS - 1000-8713 (Print) IS - 1000-8713 (Linking) VI - 29 IP - 1 DP - 2011 Jan TI - [Enantiomeric separation of propranolol by normal phase chiral liquid chromatography coupled, with tandem mass spectrometry]. PG - 26-30 AB - 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 microg/L, and the limit of quantification (LOQ) was 2.5 microg/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. FAU - Zhang, Juanhong AU - Zhang J AD - Base for Clinical Pharmacology, Lanzhou General Hospital of Lanzhou Military Region, Lanzhou 730050, China. FAU - Wang, Rong AU - Wang R FAU - Xie, Hua AU - Xie H FAU - Meng, Xiandong AU - Meng X FAU - Jia, Zhengping AU - Jia Z FAU - Ma, Jun AU - Ma J FAU - Zhang, Junli AU - Zhang J FAU - Wang, Juan AU - Wang J LA - chi PT - English Abstract PT - Journal Article PT - Research Support, U.S. Gov't, Non-P.H.S. PL - China TA - Se Pu JT - Se pu = Chinese journal of chromatography JID - 9424804 RN - 9Y8NXQ24VQ (Propranolol) SB - IM MH - Chromatography, Liquid/*methods MH - Propranolol/*chemistry MH - Stereoisomerism MH - Tandem Mass Spectrometry/*methods EDAT- 2011/05/18 06:00 MHDA- 2012/06/29 06:00 CRDT- 2011/05/18 06:00 PHST- 2011/05/18 06:00 [entrez] PHST- 2011/05/18 06:00 [pubmed] PHST- 2012/06/29 06:00 [medline] AID - 10.3724/sp.j.1123.2011.00026 [doi] PST - ppublish SO - Se Pu. 2011 Jan;29(1):26-30. doi: 10.3724/sp.j.1123.2011.00026.