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

Use of Semipreparative High Performance Liquid Chromatography to Obtain Small Quantities of the Albendazole Sulfoxide Enantiomers

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(AlbendazoleSulfoxide, 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%。

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.