高压制备液相色谱法制备没食子儿茶素没食子酸酯高纯单体化合物

Preparation of high purity gallocatechin gallate by high pressure preparative liquid chromatography

建立了没食子儿茶素没食子酸酯(GCG)高纯单体化合物的制备方法。以表没食子儿茶素没食子酸酯(EGCG)原料,料液在120℃高温转化45 min,再经高压制备液相色谱分离纯化,GCG馏分经旋转蒸发、冷冻干燥和减压真空干燥后产品纯度为99.51%,经过3次循环转化-高压制备液相色谱分离纯化,GCG的总产率大于70%。该方法操作简单、制备量大、收率高、产物纯度高,可用于没食子儿茶素没食子酸酯(GCG)标准物质的研制。

A sample method was developed in this paper for preparation of high purity compound gallocatechin gallate（GCG）. Epigallocatechin gallate（EGCG） was used as raw material and the reaction was converted in closed vassal at 120 ℃ for 45 min, the mixture was separated by high pressure preparative liquid chromatography, the collected GCG peaks were sequentially concentrated by rotary evaporation, freeze drying and vacuum drying. The purity of GCG final product was 99.51%, and the total recovery was greater than 70% for 3 replicate cycles. The method was easily operated, and had the characters of high recovery, high purity and high preparation amount. The presented method can be used for gallocatechin gallate（GCG） reference material preparation.