Development fo a column material for chromatographic resolution, using an ion-exchanged adduct of clay-alubumin.

本项目的目的是利用粘土和白蛋白的离子交换加合物，开发一种新的用于光学拆分的柱材料。粘土是一种层状层状硅酸盐，能够在层间空间中插入正离子。白蛋白是一种球状蛋白，在各种化学反应中被用作手性修饰物。我们的目标是将白蛋白的高手性识别能力与粘土的插层性能结合起来。在项目的第一年，我们研究了胶体分散的钠基蒙脱石对白蛋白的吸附行为。结果，人们发现白蛋白的吸附量高达每1克粘土2克。在第二年，我们试图了解粘土具有如此高的吸附能力的原因。用固体核磁共振和X-射线衍射法研究了粘土-白蛋白的固体加合物。在下一步中，我们制备了加合物的高效液相色谱柱。因此，我们成功地在柱上拆分了有机合成中一种有用的手性中间体--安息香。最后，通过改变溶剂组成、pH和温度，确定了拆分的最佳条件。这一结果可能为在不久的将来开发一种新的用于工业规模的光学拆分色谱柱开辟道路。

The present project has been initiated to develop a new column material for optical resolution, using an ion-exchange adduct of clay and albumin. A clay is a layr phyllosilicate capable of intercalating a positive ion in the interlayr spaces. Albumin is one of the globular proteins that have been utilized as a chiral modifier in a variety of chemical reactions. We aimed at combing the high ability of chiral recognition of albumin with the intercalating properties of a clay. In the first year of the project, we investigated the adsorption behaviors of albumin by colloidally dispersed sodium montmorillonite. As a result, it was revelealed that ablumin was adsorbed to an amount as high as 2g per 1g of a clay. In the second year, we attempted to see the reason for such high adsorption ability of a clay. A solid adduct of clay-albumin was investigated with solid state NMR and X-ray diffraction analyzes. In the next step, we prepared a column of the adduct for high performance liquid chromatography. As a result, we suceeded in resolving a useful chiral intermediate in organic synthese, benzoin, on the column. Finally we seaked for the optimum conditions for resolution, varying the solvent compositions, pH and temperature. The present results may open a way to develop a new colum for optical resolution on an industrial scale in a near future.