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ENRICHMENT AND PURIFICATION OF PEDUNCULOSIDE AND SYRINGIN FROM THE BARKS OFILEX ROTUNDAWITH MACROPOROUS RESINS
Journal of Liquid Chromatography & Related Technologies ( IF 1.3 ) Pub Date : 2013-12-11 , DOI: 10.1080/10826076.2012.749499
Chun Wang 1 , Zhimao Chao 1 , Wen Sun 1 , Xiaoyi Wu 1 , Yoichiro Ito 2
Affiliation  

Pedunculoside and syringin are two bioactive compounds in herbal tea and Chinese drug Jiubiying, the dried barks of Ilex rotunda Thunb. In the present study, the enrichment and purification of pedunculoside and syringin were investigated on the macroporous resins. The evaluation results of performance and adsorption characteristics of eight macroporous resins indicated that SP825 was most suitable for the separation of pedunculoside and syringin. Based on the series of experiments of separation, dynamic adsorption, and desorption on the column of SP825 resin, the optimal conditions were determined as follows: processing volume: 2 BV; temperature: 25°C; for desorption of syringin: ethanol-water (30:70, v/v), 4 BV as an eluent, flow rate: 1.0 mL/min/cm2; for desorption of pedunculoside:ethanol–water (60:40, v/v), 5 BV as an eluent, flow rate: 1.0 mL/min/cm2. One-step treatment of 600 mL Jiubiying extract containing 4.346 mg/mL pedunculoside and 1.478 mg/mL syringin, yielded 7.04 g (29.6% purity) crude pedunculoside powder and 2.32 g (31.0% purity) crude syringin powder. Followed by repeated recrystallization in methanol, 1600 mg pedunculoside with 99% purity, and 533 mg syringin with 96% purity were obtained. The method provides a new approach for scale-up enrichment and purification of pedunculoside and syringin from Jiubiying extract.

中文翻译:

用大孔树脂从 OFILEX ROTUNDA 树皮中富集和纯化花梗苷和丁香素

花梗苷和丁香苷是凉茶中的两种生物活性化合物,中药九必英是冬青的干燥树皮。在本研究中,在大孔树脂上研究了花梗苷和丁香苷的富集和纯化。8种大孔树脂的性能和吸附特性评价结果表明,SP825最适用于花梗苷和丁香苷的分离。通过对SP825树脂柱进行分离、动态吸附、解吸等一系列实验,确定最佳条件为:处理量:2 BV;温度:25°C;紫丁香素的解吸:乙醇-水(30:70,v/v),4 BV作为洗脱液,流速:1.0 mL/min/cm2;解吸花梗苷:乙醇-水 (60:40, v/v),5 BV 作为洗脱液,流速:1。0 毫升/分钟/平方厘米。对含有 4.346 mg/mL 花梗苷和 1.478 mg/mL 丁香苷的 600 mL 九必英提取物进行一步处理,得到 7.04 g(纯度 29.6%)的花梗苷粗粉和 2.32 g(纯度 31.0%)的丁香苷粗粉。经甲醇反复重结晶,得到纯度99%的花梗苷1600mg和纯度96%的丁香苷533mg。该方法为从九必英提取物中大规模富集纯化花梗苷和丁香苷提供了一种新途径。得到纯度为96%的丁香素533mg。该方法为从九必英提取物中大规模富集纯化花梗苷和丁香苷提供了一种新途径。得到纯度为96%的丁香素533mg。该方法为从九必英提取物中大规模富集纯化花梗苷和丁香苷提供了一种新途径。
更新日期:2013-12-11
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