CN102229638B - 从宣木瓜果实中提取齐墩果酸及制备齐墩果酸标准品的方法 - Google Patents
从宣木瓜果实中提取齐墩果酸及制备齐墩果酸标准品的方法 Download PDFInfo
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Abstract
本发明公开了一种从宣木瓜果实中提取齐墩果酸及制备齐墩果酸标准品的方法。首先将宣木瓜果实洗净,阴干后粉碎成粉状,再用乙醇溶解,超声波助提,得到粗提物,加入水中混溶,再加入正丁醇的饱和水溶液萃取多次,浓缩后得浸膏状物质,溶解后纳滤得到齐墩果酸的样品液,所得的样品液经大孔树脂初步纯化,再经硅胶柱层析,HPLC制备色谱分离精制得到齐墩果酸标准品。本发明方法工艺简单,操作方便,齐墩果酸的收率高,纯度高,可以做成标准品。
Description
技术背景
本发明属于天然产物分离纯化领域,具体涉及一种从宣木瓜果实中提取齐墩果酸及制备齐墩果酸标准品的方法。
背景技术
宣木瓜是安徽著名特产,以“百益之果”著称,是***2003年公布的30个药食兼用品种之一。宣木瓜富含黄酮类、皂甙、氨基酸、超氧化物歧化酶(SOD)等多种生物活性物质,以及钾、钙、镁、锌、铁等多种微量元素,在医用化学、植物化学、生物制药、医疗保健和绿色食品等领域均有广泛的应用前景。
齐墩果酸(oleanolic acid,OA)别名土当归酸、庆四素等,为五环三萜酸,属齐墩果苷,是宣木瓜中主要的生理活性物质。目前相关研究大多集中在宣木瓜中芦丁、黄酮、微量元素的提取和测定上。齐墩果酸因结构较复杂,人工合成繁琐,目前主要依赖从植物中提取。因此,研究分离宣木瓜中齐墩果酸,有重要的实际应用价值。
齐墩果酸具有保肝、护胃、强心、降糖、降脂、降血压的生物活性外,还有抗菌消炎、抗氧化、免疫调节、抑制血小板凝集等作用,具有多种药理功效,并有一定的抗肿瘤、抗癌活性,是一种极具开发价值的天然活性物质。
与本发明接近的技术和研究,大多是木瓜(与宣木瓜成分,用途不同)。在宣木瓜齐墩果酸研究方面只有一篇关于齐墩果酸含量测定,其中有提取过程,但主要是测定过程中所需要的步骤,不是提取和制取产品,所以,存在本质差异,且提取工艺步骤繁琐,所得产品——齐墩果酸纯度不高。
发明内容
本发明公开了一种从宣木瓜果实中提取齐墩果酸及制备齐墩果酸标准品的方法。本发明方法提取齐墩果酸,工艺简单,齐墩果酸的收率高,稳定性好;纯化后的齐墩果酸纯度很高,最终产品纯度达到97.50%以上。
本发明的目的可以通过以下技术措施来实现:
一种从宣木瓜果实中提取齐墩果酸的方法,其特征在于:具体包括以下步骤:
(1)将经过筛选的宣木瓜果实、清洗、切片、阴干后,在40℃-60℃下真空干燥,然后再粉碎,过40-45目筛,得宣木瓜果实粉;
(2)将宣木瓜果实粉加入到乙醇溶液中,在30℃-50℃下,超声波辅助提取30-50min,经多次提取后,将提取液真空浓缩,得粗提物,并回收溶剂,宣木瓜果实粉与乙醇溶液的重量比为1∶(10-15),乙醇溶液的浓度为60-85%;
(3)将所得粗提物加水混溶后,再加入等量正丁醇的饱和水溶液萃取多次,收集有机层并真空浓缩,得浸膏状物质,同时回收正丁醇;
(4)将步骤(3)所得得浸膏状物质用甲醇溶解,经滤膜过滤,即得齐墩果酸样品液。
一种利用权利要求1提取的齐墩果酸制备齐墩果酸标准品的方法,其特征在于:具体包括以下步骤:
(1)大孔树脂初步纯化处理将权利要求1制得的齐墩果酸样品液浓缩,用95%乙醇溶解,以0.9-1.1mL/min流速上样,静止3~4h后,先用蒸馏水洗去水溶性杂质,再分别用20%、50%、95%乙醇溶液洗脱,洗脱流速为1.5mL/min,收集95%乙醇洗脱液,回收乙醇,蒸干,即得皂甙粗品;
(2)硅胶柱层析将经大孔树脂层析初步纯化的粗品用甲醇溶解后上柱,并用50%和95%甲醇洗脱,分段收集洗脱液,将95%甲醇洗脱液浓缩蒸干,即得白色针状结晶;
(3)将白色针状结晶溶于甲醇中,用HPLC制备色谱分离精制,按制备色谱图出峰时间分管收集洗脱液,将HPLC检测纯度大于95%的流份合并,氮吹去净溶剂,即得齐墩果酸标准品,HPLC检测纯度的流动相为乙腈∶水=95∶5(V∶V);检测波长:210nm;柱温:25℃。
所述的利用权利要求提取的齐墩果酸制备齐墩果酸标准品的方法,其特征在于:步骤(3)所述的HPLC制备色谱的条件为:洗脱液为甲醇水,甲醇水中甲醇与水的体积比为85∶15;体积流量:10mL/min;检测波长:210nm;柱温:25℃;进样量:1.5mL。
本发明的优点在于:
(1)本发明方法,提取分离工艺简单而严密,方法可靠;
(2)本发明方法,提取齐墩果酸的收率高,稳定性好;
(3)本发明方法,提取的齐墩果酸的纯度高,达到97.50%以上。
(4)利用宣木瓜果实为原料提取齐墩果酸,资源丰富,可以深度开发宣木瓜综合利用价值。
本发明以宣木瓜果实为原料,为综合利用宣木瓜资源提供理论和实际应用依据,本发明在工业化实施后,将对促进宣木瓜产业发展、对宣木瓜资源深度开发等方面具有积极意义。
具体实施方式
现以实验室实施为例,非限定实施例叙述如下:
将宣木瓜果实经筛选、清洗、切片、阴干后,50℃真空干燥,粉碎,过40目筛(孔径0.425mm);原料粉中加入相当于原料粉重量10-15倍的60-85%乙醇,30℃-50℃,300W功率条件下超声波辅助提取30-50min,经两次提取后,将提取液真空浓缩回收溶剂得粗提物。将所得浸膏加水混溶后再加入等量正丁醇的饱和水溶液萃取三次,将有机层合并后真空浓缩,回收正丁醇,浓缩得的浸膏状物质用甲醇溶解,摇匀,经0.45μm微孔滤膜过滤,即得样品液。样品液浓缩后,用95%乙醇溶解,以1.0mL/min流速上样,静止3~4h后,先用蒸馏水洗去水溶性杂质,再分别用20%、50%、95%乙醇溶液洗脱,洗脱流速为1.5mL/min。收集95%乙醇洗脱液,回收乙醇,蒸干,即得皂甙粗品;将C18硅胶用甲醇充分浸泡脱气后,重力沉降法装柱。用甲醇充分洗出杂质后,再用50-70%乙腈水溶液平衡。将经大孔树脂层析初步纯化的粗品,溶于甲醇后上柱,并用50%和95%甲醇洗脱,层析过程在常温常压下进行;分段收集洗脱液,将95%甲醇洗脱液浓缩蒸干,即得白色针状结晶。将白色针状结晶溶于甲醇,用HPLC制备色谱分离精制(HPLC制备色谱条件为甲醇水(85∶15);体积流量:10mL/min;检测波长:210nm;柱温:25℃;进样量:1.5mL),按制备色谱图出峰时间分管收集洗脱液,将HPLC检测(HPLC检测条件为乙腈∶水=95∶5(V∶V)为流动相;检测波长:210nm;柱温:25℃)纯度大于95%的流份合并,氮吹去净溶剂,即得齐墩果酸标准品,测得纯度为97.50%,产率为1.23mg/g。
Claims (2)
1.一种制备齐墩果酸标准品的方法,其特征在于:
(一)、首先进行齐墩果酸样品液的制备:
(1)将经过筛选的宣木瓜果实、清洗、切片、阴干后,在40℃-60℃下真空干燥,然后再粉碎,过40-45目筛,得宣木瓜果实粉;
(2)将宣木瓜果实粉加入到乙醇溶液中,在30℃-50℃下,超声波辅助提取30-50min,经多次提取后,将提取液真空浓缩,得粗提物,并回收溶剂,宣木瓜果实粉与乙醇溶液的重量比为 1:(10-15),乙醇溶液的浓度为60-85%;
(3)将所得粗提物加水混溶后,再加入等量正丁醇的饱和水溶液萃取多次,收集有机层并真空浓缩,得浸膏状物质,同时回收正丁醇;
(4)将步骤(3)所得的浸膏状物质用甲醇溶解,经滤膜过滤,即得齐墩果酸样品液 ;
(二)、然后,进行以下步骤:
(1)大孔树脂初步纯化处理 将(一)中制得的齐墩果酸样品液浓缩,用95%乙醇溶解,以0.9-1.1mL/min流速上样,静止3~4h后,先用蒸馏水洗去水溶性杂质,再分别用20%、50%、95%乙醇溶液洗脱,洗脱流速为1.5mL/min,收集95%乙醇洗脱液,回收乙醇,蒸干,即得皂甙粗品;
(2)硅胶柱层析 将经大孔树脂层析初步纯化的粗品用甲醇溶解后上柱,并用50%和95%甲醇洗脱,分段收集洗脱液,将95%甲醇洗脱液浓缩蒸干,即得白色针状结晶;
(3)将白色针状结晶溶于甲醇中,用HPLC制备色谱分离精制,按制备色谱图出峰时间分管收集洗脱液,将HPLC检测纯度大于95%的流份合并,氮吹去净溶剂,即得齐墩果酸标准品,HPLC检测纯度的流动相V:V为乙腈:水=95: 5;检测波长:210nm;柱温:25℃。
2.根据权利要求1所述的制备齐墩果酸标准品的方法,其特征在于:(二)中步骤(3)所述的HPLC制备色谱的条件为:洗脱液为甲醇水,甲醇水中甲醇与水的体积比为85:15 ;体积流量:10mL/min;检测波长:210nm ;柱温:25℃;进样量:1.5mL。
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