To develop a simple and rapid purification method of rohitukine from the stem bark of Dysoxylum binectariferum. A L9 （34） orthogonal test was designed to optimize the extraction condition. Rohitukine in the plant e...To develop a simple and rapid purification method of rohitukine from the stem bark of Dysoxylum binectariferum. A L9 （34） orthogonal test was designed to optimize the extraction condition. Rohitukine in the plant extract was purified by using solvent-solvent partition and cation exchange resion （CER）. Five different types of packing materials, including XAD-2 resin, polyamide, Sephadex LH-20, ODS and CER, were compared and CER showed the best capacity for rohitukine separation. The purification procedure was optimized as follows： the plant material powder was extracted with 70% ethanol （v/m = 60） by ultrasonic agitation for 60 min, then the 70% ethanol extract was dissolved in aqueous solution （pH 1, adjusted with 0.5 mol/L HCl） and extracted with equal volume of n-butanol. The aqueous layer was retained and the pH was adjusted to 10 with 25% aqueous ammonia and a solventsolvent partition was performed with equal volume of n-butanol. The obtained n-butanol extract was dissolved in aqueous solution （pH 1, adjusted with 0.5 mol/L HCl）, and purified by a CER column eluting with H2O and 70% ethanol （pH 10, adjusted with 25% aqueous ammonia）, successively. Rohitukine existed in 70% ethanol eluate, with a purity up to 53.3%. The method developed in this study provides a simple and rapid approach for the preparation of rohitukine from the stem bark ofD. binectariferum.展开更多
不同的大孔树脂对花青素的吸附能力不同,本试验依据花青素的特征,大孔树脂的特性,筛选出DM301、ADS-17、HPD-417 3种不同型号的大孔树脂,以吸附率α和解吸率β为评价指标,选择两种大孔树脂进行组合,对黑豆皮花青素粗提物进行吸附与解吸...不同的大孔树脂对花青素的吸附能力不同,本试验依据花青素的特征,大孔树脂的特性,筛选出DM301、ADS-17、HPD-417 3种不同型号的大孔树脂,以吸附率α和解吸率β为评价指标,选择两种大孔树脂进行组合,对黑豆皮花青素粗提物进行吸附与解吸试验,采用UPLC-MS对纯化物进行检测。结果表明:最佳的树脂比例组合是DM301:HPD-417为4∶1(质量比),乙醇溶液体积分数65%,解吸液p H 3.5,动态吸附上样流速0.5 m L/min,洗脱液流速1.5 m L/min是最佳的选择,纯化的花青素主要成分为矢车菊素-3-O-葡萄糖苷。展开更多
基金Scientific Research Foundation for the Returned Overseas Chinese Scholars by Ministry of Education of China (Grant No.[2004]527).
文摘To develop a simple and rapid purification method of rohitukine from the stem bark of Dysoxylum binectariferum. A L9 （34） orthogonal test was designed to optimize the extraction condition. Rohitukine in the plant extract was purified by using solvent-solvent partition and cation exchange resion （CER）. Five different types of packing materials, including XAD-2 resin, polyamide, Sephadex LH-20, ODS and CER, were compared and CER showed the best capacity for rohitukine separation. The purification procedure was optimized as follows： the plant material powder was extracted with 70% ethanol （v/m = 60） by ultrasonic agitation for 60 min, then the 70% ethanol extract was dissolved in aqueous solution （pH 1, adjusted with 0.5 mol/L HCl） and extracted with equal volume of n-butanol. The aqueous layer was retained and the pH was adjusted to 10 with 25% aqueous ammonia and a solventsolvent partition was performed with equal volume of n-butanol. The obtained n-butanol extract was dissolved in aqueous solution （pH 1, adjusted with 0.5 mol/L HCl）, and purified by a CER column eluting with H2O and 70% ethanol （pH 10, adjusted with 25% aqueous ammonia）, successively. Rohitukine existed in 70% ethanol eluate, with a purity up to 53.3%. The method developed in this study provides a simple and rapid approach for the preparation of rohitukine from the stem bark ofD. binectariferum.
文摘不同的大孔树脂对花青素的吸附能力不同,本试验依据花青素的特征,大孔树脂的特性,筛选出DM301、ADS-17、HPD-417 3种不同型号的大孔树脂,以吸附率α和解吸率β为评价指标,选择两种大孔树脂进行组合,对黑豆皮花青素粗提物进行吸附与解吸试验,采用UPLC-MS对纯化物进行检测。结果表明:最佳的树脂比例组合是DM301:HPD-417为4∶1(质量比),乙醇溶液体积分数65%,解吸液p H 3.5,动态吸附上样流速0.5 m L/min,洗脱液流速1.5 m L/min是最佳的选择,纯化的花青素主要成分为矢车菊素-3-O-葡萄糖苷。
