高效离心分配色谱(HPCPC)分离纯化苹果树枝中的根皮苷

根皮苷是苹果中主要的水溶性多酚化合物,对人体具有多种生理保健功能。为了获得高纯度的根皮苷,运用高效离心分配色谱技术对苹果树枝乙醇提取物中的根皮苷进行分离纯化。对两相溶剂体系、转子转速和流动相流速等参数进行系统的优化实验。结果表明,最佳两相溶剂系统为正己烷-乙酸乙酯-甲醇-水(1∶5∶1∶5,v/v),上相有机相为固定相,下相水相为流动相,转子转速为1500r·min-1,流速为3.0mL·min-1,紫外检测波长为287nm。在此条件下,在30min内,从纯度为17.91%苹果树枝乙醇提取物中一步分离纯化得到根皮苷,高效液相色谱法测定其纯度为91.20%,根皮苷的回收率为98.10%。

应用高效离心分配色谱技术分离肉苁蓉中苯乙醇苷化合物

目的应用高效离心分配色谱技术分离肉苁蓉中的苯乙醇苷类化合物。方法采用醋酸乙酯∶正丁醇∶乙醇∶水(1∶1∶0.1∶2,V/V/V/V)为分离体系。结果从肉苁蓉中成功分离得到了6种苯乙醇苷类化合物。结论采用电喷雾多级串联质谱(ESI-MSn)技术分析并鉴定了6种苯乙醇苷化合物的结构。

Isolation and purification of phenylethanoid glycosides from plant extract of Plantago asiatica by high performance centrifugal partition chromatography

Two phenylethanoid glycosides （PhGs） were isolated and purified from the aerial parts of Plantago asiatica for the first time by high performance centrifugal partition chromatography （HPCPC） using ethyl acetate-n-butanol-ethanol-water （0.5：0.5：0.1：1, v/v/v/v）. A total of 45.6 mg of compound 1 and 293.8 mg of compound 2 were purified from 1341 mg of the n-butanol extract of P. asiatica. The structures of the two PhGs were tentatively identified as plantamajoside and aeteoside or isoacteoside by eleetrospray ionization multi stage tandem mass spectrometry （ESI-MS^n） in the negative ion mode.

响应面试验优化苦杏仁粕中苦杏仁苷提取工艺及其高效离心分配色谱纯化

为实现苦杏仁资源的高效利用,以带皮生杏仁为原料,首先研究热烫去皮对苦杏仁苷含量的影响,然后采用响应面试验优化了超声辅助提取压榨脱脂苦杏仁粕中苦杏仁苷的工艺条件,应用高效离心分配色谱分离制备高纯度苦杏仁苷。结果表明:按料液比1∶5(g/mL)加入沸水,煮沸10 min,能够较好地达到灭酶保苷的目的,苦杏仁苷含量为(4.72±0.14)%;压榨脱脂苦杏仁粕中苦杏仁苷最佳提取工艺条件为73%乙醇溶液、液料比8∶1、超声温度70℃、提取时间20 min、提取2次,苦杏仁苷的提取率达8.03%;高效离心分配色谱纯化苦杏仁苷的最佳条件为以正丁醇-乙酸乙酯-甲醇-水(2.5∶0.625∶0.5∶4,V/V)为溶剂体系,上相为固定相,下相为流动相,转速900 r/min,流速2.0 mL/min,分离纯化得纯度为96.14%的苦杏仁苷。

Isolation and Purification of Plantamajoside and Acteoside from Plant Extract of Plantago asiatica L. by High Performance Centrifugal Partition Chromatography

Two phenylethanoid glycosides（PhGs）, plantamajoside and acteoside, were isolated and purified from the aerial parts ofPlantago asiatica for the first time by high performance centrifugal partition chromatography（HPCPC） with ethyl acetate, n-butanol, ethanol and water（0.5：0.5：0.1：1, volume ratio） as solvent system. A total of 45.6 mg of plantamajoside and 293.8 mg of acteoside were purified from 1341 mg of the n-butanol extract of P. asiatica, with a purity of 〉93.3% as determined by HPLC. The HPCPC fractions were analyzed by HPLC-DAD and the structures were identified by their retention time, UV, electrospray ionization multi stage tandem mass spectrometry（ESI-MSn） in the negative ion mode, and confirmed by NMR experiments. The characteristic fragment ions of ESI-MS of the two PhGs isolated from Plantago asiatica were discussed, which are specific and useful for the identification of the structures of PhGs.

高效离心分配色谱法分离制备秋葵种子中的异槲皮苷

目的:采用高效离心分配色谱法分离制备秋葵种子中的异槲皮苷。方法:以乙酸乙酯-乙醇-水(5∶1∶5)为溶剂系统,上相为固定相,下相为流动相,流动相流速为2.0 mL.min-1,主机转速为1000 r.min-1,检测波长为256 nm,分离制备秋葵种子中的异槲皮苷。结果:从秋葵种子中分离得到纯度为98.2%的异槲皮苷。结论:该方法快速、简单,重复性好,分离样品纯度高。