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首页> 外文期刊>Biotechnology Progress >Combining synthetic and analytical strategies for preparative HPLC enantioseparation of monastrol racemic mixture
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Combining synthetic and analytical strategies for preparative HPLC enantioseparation of monastrol racemic mixture

机译：合成和分析策略相结合，用于制备HPLC拆分对映体的对映异构体

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Large-scale resolution of racemic monastrol has been carried out by normal-phase mode HPLC on an amylose-based chiral stationary phase. Because monastrol solubility, in media of proper compositions for normal-mode HPLC separations (in terms of retention factors and selectivity), was significantly low and impractical for preparative scopes, racemic monastrol was transformed into the corresponding O-tert-butyldimethylsilyl derivative. The tert-butyldimethylsilyl group was chosen as a suitable derivatizing agent because it induced approximatively a six-times higher solubility and allowed for an almost quantitative recovery of pure monastrol from the derivatization-deprotection sequence. The competitive isotherms of the O-tert-butyldimethylsilyl compounds, measured through frontal analysis, were fitted to competitive Langmuir and four-parameter bi-Langmuir models. The equilibrium dispersive model of chromatography was used for modeling the nonlinear separation of the racemate and to optimize the experimental conditions for collection of highly concentrated fractions of pure (R,S)-O-tert-butyldimethylsilyl compounds, from which significant amounts of the corresponding enantiomers of monastrol (about 100 mg of each enantiomer with 30 runs on an analytical-scale column) were obtained by quantitative back-derivatization.
机译：已通过正相模式HPLC在直链淀粉基手性固定相上进行了外消旋菊酯的大规模拆分。由于在适当组成的正常模式HPLC分离介质（就保留因子和选择性而言）中，蒙纳那尔溶解度非常低，在制备范围内不切实际，因此外消旋蒙纳斯丁转化为相应的O-叔丁基二甲基甲硅烷基衍生物。选择叔丁基二甲基甲硅烷基作为合适的衍生试剂，因为它诱导的溶解度大约高六倍，并允许从衍生-脱保护序列中几乎定量回收纯的菊香酚。通过正面分析测得的O-叔丁基二甲基甲硅烷基化合物的竞争等温线适用于竞争性Langmuir模型和四参数bi-Langmuir模型。使用色谱的平衡分散模型对外消旋物的非线性分离进行建模，并优化实验条件，以收集纯净的（R，S）-O-叔丁基二甲基甲硅烷基化合物的高浓度馏分，其中大量相应的通过定量反衍生得到monastrol的对映体（每种对映体约100 mg，在分析规模的色谱柱上进行30次电泳）。

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