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使用七(2,3-二乙酰基-6-硫酸根)-β-环糊精通过毛细管电泳法测定利奈唑胺对映体杂质

Determination of enantiomeric impurity of linezolid by capillary electrophoresis using heptakis-(2,3-diacetyl-6-sulfato)-beta-cyclodextrin.

作者信息

Michalska Katarzyna, Pajchel Genowefa, Tyski Stefan

机构信息

Department of Antibiotics and Microbiology, National Medicines Institute, Chełmska 30/34, 00-725 Warsaw, Poland.

出版信息

J Chromatogr A. 2008 Feb 8;1180(1-2):179-86. doi: 10.1016/j.chroma.2007.11.110. Epub 2007 Dec 8.

Abstract

A method for the enantioseparation of linezolid, the first compound of a truly new class of antibiotics-the oxazolidinones, was developed. The elaborated method of linezolid enantiomers separation was successfully performed using an anionic single-isomer cyclodextrin-heptakis-(2,3-diacetyl-6-sulfato)-beta-cyclodextrin (HDAS-beta-CD) as a resolving agent with the help of the charged resolving agent migration model (CHARM model). The best results were obtained with 27.5mM HDAS-beta-CD dissolved in 50mM borate buffer, pH 9.0, 15 degrees C, normal polarity. The facile strategies for the reversal of the enantiomers elution order are also described. Afterwards, the optimized method was validated in terms of sensitivity, linearity, accuracy and precision.

摘要

开发了一种对利奈唑胺进行对映体拆分的方法,利奈唑胺是一类全新的抗生素——恶唑烷酮类中的首个化合物。使用阴离子单异构体环糊精——七(2,3 - 二乙酰基 - 6 - 硫酸根)-β-环糊精(HDAS-β-CD)作为拆分剂,借助带电拆分剂迁移模型(CHARM模型),成功实现了利奈唑胺对映体的精细拆分方法。将27.5mM的HDAS-β-CD溶解于50mM硼酸盐缓冲液(pH 9.0)中,在15℃、正常极性条件下可获得最佳结果。文中还描述了使对映体洗脱顺序反转的简便策略。之后,对优化后的方法在灵敏度、线性、准确度和精密度方面进行了验证。

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