水相中无溶剂α-硫辛酸的制备

Preparation of α-lipoic Acid without Solvent in Water

无溶剂残余的α-硫辛酸作为原料药越来越得到药学界的重视。通过三种纯化方法的筛选,成功的在水相中应用柱层析的方法,制备了无溶剂残余的α-硫辛酸,回收率达到90%以上。经气相色谱(GC-FID)检测可能涉及到的七种有机溶剂,均在仪器的最小检出浓度以下;经高效液相色谱(HPLC-UV)检测,其含量≥99.5%,其中主要杂质1,2,3-三噻环己烷-4-戊酸已除去,而且产品的外观也大为改善。

It gets more and more important to α-lipoic acid without organic solvent as the raw materials medicine. A new method for preparation of α-lipoic acid without solvent was developed by column chromatography screening of three kinds of purification methods. The recoveries of α-lipoic acid were more than 90 %. Seven kinds of organic solvent that might involve were measured by GC-FID. Each of it was not found in instrument. Measured by HPLC-UV, the content of α-lipoic acid was not less than 99, 5 %. And its main by-product was not found through HPLC. After purification, α-lipoic acid without solvent was good looking in appearance.