青霉胺对映体的毛细管电泳手性分离及应用研究
毛细管电泳,,毛细管电泳,,手性分离,青霉胺,摘要,关键词,1引言,2实验部分,3结果与讨论,References
摘 要建立了一种青霉胺对映体的毛细管电泳手性分离方法。采用2,4-二硝基氯苯作为青霉胺的衍生试剂,以磺化β环糊精(SβCD)作为手性选择剂,50 mmol/L pH 9.5的硼砂缓冲溶液作为电泳缓冲液,在14 min 内实现了青霉胺对映体的毛细管电泳手性拆分,分离度达3.7。本文还考察了在大量D青霉胺存在下, 测定微量L青霉胺的可能性。当D青霉胺中,L青霉胺的含量在0.3%~2.0%范围内时,其浓度与吸光度之间呈现良好的线性关系(r=0.9995), 对D青霉胺药片进行光学纯度分析,获得了满意的结果。
关键词 毛细管电泳, 手性分离,青霉胺
Enantioseparation of Penicillamine by Capillary Electrophoresis
He Min, Zhao Shulin*, Chen Jie
(College of Chemistry and Chemical Engineering,Guangxi Normal University,Guilin 541004)
Abstract A method is presented for the chiral separation of penicillamine enantiomers. The penicillamine enantiomers were derivatized with 1chloro2,4dinitrobenzene and separated by capillary electrophoresis. The βcyclodextrin (βCD), methylcyclodextrin (MβCD), hydroxypropylβCD (HβCD) and sulfatedβCD (SβCD), as chiral selector, were examinedfor the enantionmeric separation of penicillamine, the concentration of chiral selector, some other experimental factors have also been optimized, such as concentration of borate buffer, pH of electrolyte and applied voltage. Optimal separation was obtained at pH 9.5, 50 mmol/L borate solution containing 25 mmol/L SβCD, as well as 20 kV applied voltage and 20℃ capillary temperature. Determination was followed by ultraviolet absorptiometric measurements at 202 nm. The derivatives of penicillamine enantiomers were resolved completely in 14 minutes, giving a resolution reached up to 3.7. The linear range, the recovery and the repeatability of Lpenicillamine in the presence of large Dpenicillamine were tested and a satisfactory result was obtained. The developed method has been employed for optical purity analysis of Dpenicillamine drug, and allowed the determination of 0.3% Lpenicillamine in Dpenicillamine with well peak identification. ......
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