Semipreparative Enantiomer Separation of Propranolol Hydrochloride by High-Performance Liquid Chromatography Using Cellulose tris(3,5-Dimethylphenylcarbamate) Chiral Stationary Phase

CORC > 兰州化学物理研究所 > 中国科学院兰州化学物理研究所 > 中科院西北特色植物资源化学重点实验室/甘肃省天然药物重点实验室

	Semipreparative Enantiomer Separation of Propranolol Hydrochloride by High-Performance Liquid Chromatography Using Cellulose tris(3,5-Dimethylphenylcarbamate) Chiral Stationary Phase
	Jiang SX(蒋生祥); Liu X(刘霞); Liu X(刘霞)
刊名	Journal of Chromatographic Science
	2008
卷号	46 期号:9 页码:767-771
ISSN号	0021-9665
通讯作者	刘霞
中文摘要	In this paper, we describe the direct semipreparative resolution of racemic (rac)-propranolol hydrochloride by high-performance liquid chromatography using cellulose tris(3,5-dimethylphenylcarbamate) as chiral stationary phase and mobile phase systems containing petroleum ether and 2-propanol with the use of basic additives. At analytical scale, the retention factor of both enantiomers is less than 5 with the separation factor 1.95 and the resolution 2.4. Then, the analytical method is scaled up to semipreparative loading to obtain small amounts of both propranolol hydrochloride enantiomers. Petroleum ether, rather than n-hexane, is used to effectively reduce the production cost of (R)- and (S)-propranolol. To increase the throughput, overlapping injections are used, allowing an injection to be made every 6.5 min instead of every 12 min. At semipreparative scale, approximately 19 mg/h enantiomers are isolated. The first fraction [(R)-(+)-propranolol hydrochloride] is isolated with a purity of > 99.6%(e.e.) and > 97.0% yield, and the second [(S)-(–)-propranolol hydrochloride] is isolated with a purity of > 99.3% (e.e.) and > 95.0% yield. In addition, optical rotations of both propranolol hydrochloride enantiomers isolated are investigated.
学科主题	分析化学与药物化学
收录类别	SCI
资助信息	the National Natural Science Foundation of China (NSFC, NO. 20475058 and NO. 20527005).
语种	英语
公开日期	2012-10-11
内容类型	期刊论文
源URL	[http://210.77.64.217/handle/362003/1389]
专题	兰州化学物理研究所_中科院西北特色植物资源化学重点实验室/甘肃省天然药物重点实验室
通讯作者	Liu X(刘霞); Liu X(刘霞)
推荐引用方式 GB/T 7714	Jiang SX,Liu X,Liu X. Semipreparative Enantiomer Separation of Propranolol Hydrochloride by High-Performance Liquid Chromatography Using Cellulose tris(3,5-Dimethylphenylcarbamate) Chiral Stationary Phase[J]. Journal of Chromatographic Science,2008,46(9):767-771.
APA	蒋生祥,刘霞,&刘霞.(2008).Semipreparative Enantiomer Separation of Propranolol Hydrochloride by High-Performance Liquid Chromatography Using Cellulose tris(3,5-Dimethylphenylcarbamate) Chiral Stationary Phase.Journal of Chromatographic Science,46(9),767-771.
MLA	蒋生祥,et al."Semipreparative Enantiomer Separation of Propranolol Hydrochloride by High-Performance Liquid Chromatography Using Cellulose tris(3,5-Dimethylphenylcarbamate) Chiral Stationary Phase".Journal of Chromatographic Science 46.9(2008):767-771.