摘要
采用一种连续中压硅胶柱层析分离高纯度表没食子儿茶素没食子酸酯(EGCG)及表儿茶素没食子酸酯(ECG),原料为含量高于98%的茶多酚。连续中压柱层析分离工艺条件为:160~280μm硅胶为填充料,1200mm×80mm的自制不锈钢中压层析柱,洗脱液为乙酸乙酯-石油醚-甲酸(体积比6∶4∶1),洗脱流速为30mL/min,负载量为35g/kg(以硅胶计,下同),可以得到纯度大于98%的EGCG产品(平均回收率为85.5%)和98%的ECG产品(平均回收率均为80.3%)。回收的洗脱剂先校正pH值,再经薄层层析校正后可重复使用。使用后的层析柱用乙酸乙酯再生,石油醚为平衡剂平衡,平衡后的层析柱可重复使用。
A method is described for successive purification of epigallocatechin gallate (EGCG) and epicatechin gallate (ECG) by medium-pressure silica gel column chromatography. The raw material was 98 % tea polyphenols. The operating conditions of the chromatographic steps were investigated and optimized, using 1 200 mm × 80 mm stainless steel column as chromatographic column. The optimum condition was as followed: 160-280μm silica gel as filling material, ethyl acetate-petroleum ether-formic acid 6 : 4 : 1 as eluting solvent, flowing rate 30 mL/min, loading amount 35 g/kg silica gel. The average yields of 98 % EGCG and 98 % ECG were 85.5 % and 80.3 %, respectively. A reclaimed eluting solvent can be used repeatedly,it's pH value is first adjusted, and concentration ratio is then adjusted by TLC method. The chromatographic column which was regenerated by ethyl acetate, and equilibrated with petroleum, can be used repeatedly.
出处
《林产化学与工业》
EI
CAS
CSCD
2007年第2期100-104,共5页
Chemistry and Industry of Forest Products