淫羊藿有效成分提取工艺研究
摘要
在中国传统医学日益被人们所认知的今天,分离活性植物化合物,确认其保健功能,并将其进一步开发成具有中国特色的功能性食品,是目前营养学的研究方向之一。
近年来,随着国内、外对植物化合物研究和应用的逐渐深入,淫羊藿内的淫羊藿苷因其具有药用价值和较高保健作用可作为辅药应用于多种疾病的预防与治疗。已日益受到人们的广泛重视。
为此,我们以淫羊藿为研究原料,对其所含的淫羊藿苷进行提取、分离纯化及含量测定,以淫羊藿苷为指标成分,以使其物质基础明确、质量稳定可控、使用检测方便,能作为功能性基料使用。可进行工业化生产,开发相应的保健食品,供应市场。
本课题对淫羊藿的活性成分淫羊藿苷进行了鉴别、提取、分离纯化和制定其检测方法的研究。
1.本文首先对淫羊藿提取物进行了定性鉴别和药材质量鉴别进一步验证其有效成分为芦丁、淫羊藿苷和榭皮素等黄酮类化合物。
2.制定了淫羊藿苷的紫外和HPLC的检测方法。绘制了淫羊藿苷标准样的紫外分光标准曲线和HPLC标准曲线。
3.比较了淫羊藿苷的多种提取方法,并考察了其影响因素,通过正交实验确定提取最佳提取工艺为：超声功率为300W、60%乙醇溶液、液固比25：1、提取时间60min、提取温度50℃。根据优选工艺验证实验表明,有效成分提取率92.88%,纯度为28.70%,重现性较好。
4.淫羊藿苷精提工艺：粗提干粉过30目的标准筛,称取0.5g加3BV的蒸馏水,超声充分溶解并将其pH值调至6,上AB-8树脂柱吸附30min,以1SV的流速70%乙醇溶液进行洗脱操作,收集洗脱液,洗脱率为83.60%。淫羊藿苷的纯度为83.60%。
5.淫羊藿苷膜分离条件：截留淫羊藿大分子杂质处理条件为选择截留分子量为1000的短有机膜超滤0095,料液温度为30℃、膜前压力为0.25MPa、操作时间100min；去除淫羊藿小分子杂质处理条件为选择截留分子量为300纳滤膜DK2540,料液温度为30℃、膜前压力为0.2 MPa、操作时间80min；脱水浓缩选用反渗透膜SGRO-2540条件为料液温度为30℃、膜前压力为0.2MPa、操作时间80min。提取纯化的淫羊藿苷的纯度为88.10%。
That separation of active components,confirmed their health functions,and developed further into functional foods with Chinese characteristics,one of the nutrition research directions,in the today of that Chinese traditional medicine are acknowledged by all peaple.
In recent years, with the development of domestic and foreign research and applications of plants compounds, the Icariin in Epimedium has been increasing attention to all peaple.Beacause of that has medicinal value and healthy care and applied in the prevention and treatment of many diseases as traditional Chinese medicine.
So as to,we study Epimedium as the raw materials.Extraction,purification and identification of Icariin are made it clear,that has stable quality and easy to detect.It supplyed market as the base material that are used into industrial productions and developed into the healthy foods.
The extraction,purification and identification of Icariin were set up.And it made up a serious methods on identification of Icariin in this paper.
Firstly, it was recognized that the components of Epimedium were Icariin.This paper made up the methods of detections of Epimedium by-UV and HPLC.
Secondly,the extracted methods of Icariin were selected by the comparing from water, ethanol and other assistant extractions.And then the optimal conditions by orthogonal design was obtained as follow:Ultrasound 300W,60% ethanol,Material ratio 25:1,Temperature of extraction 50℃,Times of extraction 60min. The content of Icariin was 92.88% with a good reproductbility.
Thirdly,Icariin is puricated by AB-8 macroporous adsorption resin.The conditions of it is time:30min,pH=6,watered with distilled water to clear out other components.And then it is washed by 70% ethanol of 3 polyamide volume.At last,it collected and checked by UV or HPLC.Washout rate is 93.30%.The content of extracted and purificated Icariin is 83.60%.
Lastly,The optimal conditions for membrane of Icariin:conditions of intercepted Macromolecular processing is that temperature is 30℃,pressure is 0.25MPa,operating time is 100min by short organic membrane0095 of MW1000.And the conditions of remove small molecule processing is that temperature is 30℃,pressure is 0.2MPa,operating time is 80min by nanofiltration membrane DK2540 of MW300.The concentration of solution isthat temperature is 30℃,pressure is 0.2MPa,operating time is 80min by SGRO-2540 membrane The content of extracted and purificated Epimedium is 88.10%.
近年来,随着国内、外对植物化合物研究和应用的逐渐深入,淫羊藿内的淫羊藿苷因其具有药用价值和较高保健作用可作为辅药应用于多种疾病的预防与治疗。已日益受到人们的广泛重视。
为此,我们以淫羊藿为研究原料,对其所含的淫羊藿苷进行提取、分离纯化及含量测定,以淫羊藿苷为指标成分,以使其物质基础明确、质量稳定可控、使用检测方便,能作为功能性基料使用。可进行工业化生产,开发相应的保健食品,供应市场。
本课题对淫羊藿的活性成分淫羊藿苷进行了鉴别、提取、分离纯化和制定其检测方法的研究。
1.本文首先对淫羊藿提取物进行了定性鉴别和药材质量鉴别进一步验证其有效成分为芦丁、淫羊藿苷和榭皮素等黄酮类化合物。
2.制定了淫羊藿苷的紫外和HPLC的检测方法。绘制了淫羊藿苷标准样的紫外分光标准曲线和HPLC标准曲线。
3.比较了淫羊藿苷的多种提取方法,并考察了其影响因素,通过正交实验确定提取最佳提取工艺为：超声功率为300W、60%乙醇溶液、液固比25：1、提取时间60min、提取温度50℃。根据优选工艺验证实验表明,有效成分提取率92.88%,纯度为28.70%,重现性较好。
4.淫羊藿苷精提工艺：粗提干粉过30目的标准筛,称取0.5g加3BV的蒸馏水,超声充分溶解并将其pH值调至6,上AB-8树脂柱吸附30min,以1SV的流速70%乙醇溶液进行洗脱操作,收集洗脱液,洗脱率为83.60%。淫羊藿苷的纯度为83.60%。
5.淫羊藿苷膜分离条件：截留淫羊藿大分子杂质处理条件为选择截留分子量为1000的短有机膜超滤0095,料液温度为30℃、膜前压力为0.25MPa、操作时间100min；去除淫羊藿小分子杂质处理条件为选择截留分子量为300纳滤膜DK2540,料液温度为30℃、膜前压力为0.2 MPa、操作时间80min；脱水浓缩选用反渗透膜SGRO-2540条件为料液温度为30℃、膜前压力为0.2MPa、操作时间80min。提取纯化的淫羊藿苷的纯度为88.10%。
That separation of active components,confirmed their health functions,and developed further into functional foods with Chinese characteristics,one of the nutrition research directions,in the today of that Chinese traditional medicine are acknowledged by all peaple.
In recent years, with the development of domestic and foreign research and applications of plants compounds, the Icariin in Epimedium has been increasing attention to all peaple.Beacause of that has medicinal value and healthy care and applied in the prevention and treatment of many diseases as traditional Chinese medicine.
So as to,we study Epimedium as the raw materials.Extraction,purification and identification of Icariin are made it clear,that has stable quality and easy to detect.It supplyed market as the base material that are used into industrial productions and developed into the healthy foods.
The extraction,purification and identification of Icariin were set up.And it made up a serious methods on identification of Icariin in this paper.
Firstly, it was recognized that the components of Epimedium were Icariin.This paper made up the methods of detections of Epimedium by-UV and HPLC.
Secondly,the extracted methods of Icariin were selected by the comparing from water, ethanol and other assistant extractions.And then the optimal conditions by orthogonal design was obtained as follow:Ultrasound 300W,60% ethanol,Material ratio 25:1,Temperature of extraction 50℃,Times of extraction 60min. The content of Icariin was 92.88% with a good reproductbility.
Thirdly,Icariin is puricated by AB-8 macroporous adsorption resin.The conditions of it is time:30min,pH=6,watered with distilled water to clear out other components.And then it is washed by 70% ethanol of 3 polyamide volume.At last,it collected and checked by UV or HPLC.Washout rate is 93.30%.The content of extracted and purificated Icariin is 83.60%.
Lastly,The optimal conditions for membrane of Icariin:conditions of intercepted Macromolecular processing is that temperature is 30℃,pressure is 0.25MPa,operating time is 100min by short organic membrane0095 of MW1000.And the conditions of remove small molecule processing is that temperature is 30℃,pressure is 0.2MPa,operating time is 80min by nanofiltration membrane DK2540 of MW300.The concentration of solution isthat temperature is 30℃,pressure is 0.2MPa,operating time is 80min by SGRO-2540 membrane The content of extracted and purificated Epimedium is 88.10%.
引文
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