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用半制备高效液相色谱法制备少量的阿苯达唑亚砜单一对映体
引用本文:翟宗德,张虹,师彦平,陈立仁,张红丽,李永民.用半制备高效液相色谱法制备少量的阿苯达唑亚砜单一对映体[J].分析化学,2005,33(1):109-112.
作者姓名:翟宗德  张虹  师彦平  陈立仁  张红丽  李永民
作者单位:中国科学院兰州化学物理研究所,兰州,730000;中国科学院研究生院,北京,100039;兰州医学院第一附属医院,兰州,730000;中国科学院兰州化学物理研究所,兰州,730000
基金项目:科技部基础性研究项目;中国科学院"百人计划"
摘    要:涂敷直链淀粉-三(3,5-二甲基苯基氨基甲酸酯)(ADMPC)于自制的球形氨丙基硅胶上,制备了手性固定相。用高效液相色谱法(HPLC)在正相条件下,用该固定相在分析柱上直接拆分了广谱驱虫药物阿苯达唑亚砜外消旋体(Albendazole Sulfoxide,ABZSO)。然后,将分析色谱方法扩展到了半制备色谱,进行该药物的半制备分离,考察了不同进样量对半制备色谱的参数的影响。在最大进样量下,83h制备了各约1g的阿苯达唑亚砜的两种单一对映体。( )ABZSO的产率大于98.0%,纯度大于99.9%;(-)ABZSO的产率大于94.0%,纯度大于99.0%。

关 键 词:手性拆分  半制备色谱  阿苯达唑亚砜  直链淀粉-三(3  5-二甲基苯基氨基甲酸酯)

Use of Semipreparative High Performance Liquid Chromatography to Obtain Small Quantities of the Albendazole Sulfoxide Enantiomers
Zhai Zongde , Zhang Hong ,Shi Yanping ,Chen Liren ,Zhang Hongli ,Li Yongmin.Use of Semipreparative High Performance Liquid Chromatography to Obtain Small Quantities of the Albendazole Sulfoxide Enantiomers[J].Chinese Journal of Analytical Chemistry,2005,33(1):109-112.
Authors:Zhai Zongde  Zhang Hong  Shi Yanping  Chen Liren  Zhang Hongli    Li Yongmin
Institution:Zhai Zongde 1,2 Zhang Hong 3,Shi Yanping 1,Chen Liren *1,Zhang Hongli 1,2,Li Yongmin 1 1
Abstract:A chiral stationary phase (CSP) was prepared by coating amylose tris ( 3,5 dimethyl phenyl carbamate ) (ADMPC) onto aminopropylated spherical silica gel. Broad spectrum anthelmintic agent albendazole sulfoxide (ABZSO) was directly resolved on analytical ADMPC CSP column by normal phase high performance liquid chromatography (HPLC). Then, the analytical methods were scaled up to semipreparative loading to obtain small quantities of both ABZSO enantiomers. Especially, different loading amounts were investigated for their effect on various parameters of semipreparative HPLC. Using the maximum loading, about 1 g of each enantiomer were obtained in 83 h. A purity of >99.9% and a yield of >98.0% was obtained for (+)ABZSO enantiomer; and a purity of >99.0% and a yield of >94.0% was obtained for (-)ABZSO enantiomer.
Keywords:Enantiomer separation  semipreparative high performance liquid chromatography  albendazole sulfoxide  amylose tris(3  5  dimethylphenyl carbamate)
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