文献类型：期刊文献

英文题名：Refining androstenedione and bisnorcholenaldehyde from mother liquor of phytosterol fermentation using macroporous resin column chromatography followed by crystallization

作者：Xu, Shi-Dong[1];Ning, Fang-Hong[1];Jiang, Bang-he[1];Xu, Huan-Xin[1];Liu, Zuo-Zhen[1]

机构：[1]East China Univ Sci & Technol, State Key Lab Bioreactor Engn, Box 348,130 Meilong Rd, Shanghai 200237, Peoples R China

年份：2018

卷号：1079

起止页码：9

外文期刊名：JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES

收录：;EI(收录号：20180604767752);WOS:【SCI-EXPANDED(收录号:WOS:000427343800002)】；

基金：The authors gratefully acknowledge the financial support by the program for Shanghai Science and Technology Committee (No. 1402H248400)

语种：英文

外文关键词：Androstenedione; Bisnorcholenaldehyde; Macroporous resin; Chromatography; Crystallization

摘要：Androstenedione is an androgen and intermediate in the biosynthesis of most adrenocortical, anabolic, sex and synthetic steroids, such as canrenone, eplerenone, norethindrone and spironolactone. Bisnorcholenaldehyde is an important intermediate in the synthesis of progesterone. This study established an androstenedione and bisnorcholenaldehyde separation method that used a macroporous adsorption resin and an ethanol-water mixture as eluent. The adsorption properties of 12 non-polar or weakly polar macroporous adsorption resins were compared, and three resins exhibited a high adsorption capacity and high desorption rate for both androstenedione and bisnorcholenaldehyde. The three resins were then compared using column chromatography, and one resin was selected and parameters (flow rate, resin size, ethanol concentration and volume) of chromatography were optimized to obtain high purity and recovery. Chromatography eluate was concentrated, dissolved in suitable solvent and crystallized at an optimal temperature to obtain a high purity of both androstenedione and bisnorcholenaldehyde from the same starting material: The levels of androstenedione and bisnorcholenaldehyde in the raw material were 39.78% and 19.15%, respectively. After preparative separation and enrichment by resin column chromatography and crystallization, the purity of androstenedione and bisnorcholenaldehyde was 94.3% and 98.6%, respectively, with their recovery yields of 66.8% and 57.9%, respectively. In addition, the resin maintained over 90% separation efficiency for 5 cycles of adsorption. These results indicated that the combination of macroporous resin chromatography followed by crystallization provide a simple, effective, environmentally friendly and low-cost method for the simultaneous purification of androstenedione and bisnorcholenaldehyde.