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Optimization, extraction, and purification of three bioactive compounds from Entada phaseoloides by high-speed countercurrent chromatography
Biomedical Chromatography ( IF 1.8 ) Pub Date : 2021-08-23 , DOI: 10.1002/bmc.5232
Yan Zhou 1 , Hu Shan 2 , Haitao Lü 1
Affiliation  

The objective of this paper was to develop a preparative method for the separation and purification of phaseoloidin, entadamide A, and entadamide A-β-D-glucopyranoside from the crude extract of Entada phaseoloides by high-speed countercurrent chromatography (HSCCC) for the first time. Optimized by orthogonal experiments, the extraction conditions were extraction temperature of 65°C, solid-to-liquid ratio of 1:15 (g/mL), ethanol concentration of 40%, and extraction time of 2.5 h. Using n-butanol-acetic acid-water (4:1:5, v/v/v) as the two-phase solvent system, 38.79 mg phaseoloidin (the purity was 99.3% with a recovery of 98.1%), 34.85 mg entadamide A (the purity was 96.4% with a recovery of 98.5%), and 33.97 mg entadamide A-β-D-glucopyranoside (the purity was 98.6% with a recovery of 97.7%) were obtained from 500 mg crude extract by HSCCC in head-to-tail elution mode. The retention ratio of stationary phase was 51.0%. According to the antioxidant activity assays, phaseoloidin, entadamide A, and entadamide A-β-D-glucopyranoside had certain scavenging abilities on 1,1-diphenyl-2-picrylhydrazyl free radicals and hydroxyl free radicals.

中文翻译:

高速逆流色谱法优化、提取和纯化 Entada phaseoloides 中的三种生物活性化合物

本论文的目的是建立一种制备方法,首次采用高速逆流色谱法(HSCCC)白菜豆粗提物中分离纯化白豆苷、恩他酰胺A和恩他酰胺A- β - D-吡喃葡萄糖苷。时间。通过正交实验优化提取条件为提取温度65℃、料液比1:15(g/mL)、乙醇浓度40%、提取时间2.5 h。以丁醇-乙酸-水(4:1:5, v/v/v)为两相溶剂体系,38.79 mg菜豆苷(纯度为99.3%,回收率为98.1%),34.85 mg entadamide A(纯度为 96.4%,回收率为 98.5%)和 33.97 mg entadamide A-采用HSCCC从500 mg粗提物中以头对尾洗脱方式获得β - D-吡喃葡萄糖苷(纯度为98.6%,回收率为97.7%)。固定相的保留率为51.0%。抗氧化活性测定表明,菜豆素、恩他酰胺A和恩他酰胺A- β - D-吡喃葡萄糖苷对1,1-二苯基-2-苦基肼自由基和羟基自由基具有一定的清除能力。
更新日期:2021-08-23
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