CN1317295C - 一种绞股蓝总皂甙的制取方法 - Google Patents
一种绞股蓝总皂甙的制取方法 Download PDFInfo
- Publication number
- CN1317295C CN1317295C CNB031144713A CN03114471A CN1317295C CN 1317295 C CN1317295 C CN 1317295C CN B031144713 A CNB031144713 A CN B031144713A CN 03114471 A CN03114471 A CN 03114471A CN 1317295 C CN1317295 C CN 1317295C
- Authority
- CN
- China
- Prior art keywords
- raw material
- ethanol
- gynostemma
- gynostemma pentaphylla
- macroporous resin
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
- 235000002956 Gynostemma pentaphyllum Nutrition 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims description 6
- 239000001397 quillaja saponaria molina bark Substances 0.000 title abstract description 10
- 229930182490 saponin Natural products 0.000 title abstract description 10
- 150000007949 saponins Chemical class 0.000 title abstract description 10
- 240000006509 Gynostemma pentaphyllum Species 0.000 title abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000011347 resin Substances 0.000 claims abstract description 22
- 229920005989 resin Polymers 0.000 claims abstract description 22
- 238000000605 extraction Methods 0.000 claims abstract description 19
- 239000002994 raw material Substances 0.000 claims abstract description 18
- 238000011010 flushing procedure Methods 0.000 claims abstract description 17
- 241001065361 Gynostemma Species 0.000 claims abstract description 16
- 238000001179 sorption measurement Methods 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000010828 elution Methods 0.000 claims abstract description 10
- 229930187479 gypenoside Natural products 0.000 claims abstract description 9
- 239000006228 supernatant Substances 0.000 claims abstract description 9
- 230000007935 neutral effect Effects 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 6
- 239000007788 liquid Substances 0.000 claims description 19
- 239000003513 alkali Substances 0.000 claims description 8
- 238000005352 clarification Methods 0.000 claims description 7
- FBFMBWCLBGQEBU-RXMALORBSA-N (2s,3r,4s,5s,6r)-2-[(2r,3r,4s,5s,6r)-2-[[(3s,5r,6s,8r,9r,10r,12r,13r,14r,17s)-3,12-dihydroxy-4,4,8,10,14-pentamethyl-17-[(2s)-6-methyl-2-[(2s,3r,4s,5s,6r)-3,4,5-trihydroxy-6-(hydroxymethyl)oxan-2-yl]oxyhept-5-en-2-yl]-2,3,5,6,7,9,11,12,13,15,16,17-dodecah Chemical class O([C@@](C)(CCC=C(C)C)[C@@H]1[C@@H]2[C@@]([C@@]3(C[C@@H]([C@H]4C(C)(C)[C@@H](O)CC[C@]4(C)[C@H]3C[C@H]2O)O[C@H]2[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O2)O[C@H]2[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O2)O)C)(C)CC1)[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O FBFMBWCLBGQEBU-RXMALORBSA-N 0.000 claims description 4
- 238000000034 method Methods 0.000 abstract description 14
- 239000012530 fluid Substances 0.000 abstract description 6
- ZRBFCAALKKNCJG-UHFFFAOYSA-N gypenoside-XVII Natural products C1CC(C2(CCC3C(C)(C)C(OC4C(C(O)C(O)C(CO)O4)O)CCC3(C)C2CC2O)C)(C)C2C1C(C)(CCC=C(C)C)OC(C(C(O)C1O)O)OC1COC1OC(CO)C(O)C(O)C1O ZRBFCAALKKNCJG-UHFFFAOYSA-N 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000010438 heat treatment Methods 0.000 abstract description 2
- 239000012670 alkaline solution Substances 0.000 abstract 1
- 238000003889 chemical engineering Methods 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 abstract 1
- 239000000284 extract Substances 0.000 description 7
- 239000002253 acid Substances 0.000 description 5
- 230000001476 alcoholic effect Effects 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 239000012535 impurity Substances 0.000 description 5
- 229920006395 saturated elastomer Polymers 0.000 description 5
- 238000004042 decolorization Methods 0.000 description 4
- 238000001291 vacuum drying Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 235000012054 meals Nutrition 0.000 description 2
- 206010013786 Dry skin Diseases 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 240000003185 Gynostemma laxum Species 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 238000005349 anion exchange Methods 0.000 description 1
- 230000001093 anti-cancer Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 230000003311 flocculating effect Effects 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 239000003862 glucocorticoid Substances 0.000 description 1
- 229930182470 glycoside Natural products 0.000 description 1
- 150000002338 glycosides Chemical class 0.000 description 1
- 230000000147 hypnotic effect Effects 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 210000000689 upper leg Anatomy 0.000 description 1
Landscapes
- Extraction Or Liquid Replacement (AREA)
Abstract
本发明属于化工技术，提出一种工艺流程短、皂甙得率高、纯度高的绞股蓝皂甙制备方法。该方法以绞股蓝为原料，将绞股蓝加入碱水煮沸提取，过滤提取液，澄清，将上清液通入大孔树脂吸附，碱液冲洗柱子至流出液无色，再用水冲洗至中性，然后用原料5-8倍量50%-95%乙醇洗脱，脱除乙醇经干燥处理得股蓝总皂甙制品。本发明用碱水加热提取绞股蓝皂甙，用HPD类大孔树脂吸附，使绞股蓝总皂甙的提取率达到7%，纯度可达95%以上；采用碱液冲洗柱子，减少了树脂柱的再生处理工序，使工艺流程缩短，同时提高了设备利用率，降低生产成本。
Description
技术领域
本发明属于化工技术，具体地说是绞股蓝总皂甙的制取方法。
背景技术
绞股蓝总甙具有降血脂、防治糖皮质激素副作用、镇静、催眠、治疗白发、抑制癌细胞生长等功能，广泛用于医药工业和食品工业。现有技术通常采用活性炭法、溶剂萃取法、树脂吸附法等工艺来提取。申请号为92101498，名称为“长梗绞股蓝总皂甙的生产工艺”就是采用树脂吸附法，将原料水煎提取，水煎液通过聚酰胺柱或者在水煎液中加入絮凝剂去除非皂甙类杂质，然后通过大孔树脂吸附和乙醇洗脱，洗脱液再通过阴离子交换柱，流出液经干燥处理得成品。申请号为93106940，名称为“绞股蓝有效成分的提取工艺及绞股蓝饮料”提出的工艺是将绞股蓝浸入弱碱性介质中加热浸提，再加入沉淀助滤剂得皂甙、天然维生素C的绞股蓝提取液。现有技术得率高的工艺复杂，生产成本高。工艺简单的皂甙得率低且纯度也低。
发明内容
本发明为克服现有技术之不足，提出一种工艺流程短、皂甙得率高、纯度高的绞股蓝皂甙制备方法。
本发明解决其技术问题的方案是：以绞股蓝为原料，将绞股蓝加入PH值为9-11的碱水煮沸提取，过滤提取液，澄清，将上清液通入大孔树脂吸附，冲洗，然后用原料5-8倍量50％-95％乙醇洗脱，脱除乙醇经干燥处理得股蓝总皂甙制品。
本发明的进一步改进是，将上清液通入大孔树脂吸附，用PH值为9-11的碱液冲洗柱子至流出液无色，再用水冲洗至中性，然后用原料5-8倍量50％-95％乙醇洗脱，脱除乙醇经干燥处理得股蓝总皂甙制品。
本发明的有益效果是：本发明用碱水加热提取绞股蓝皂甙，用HPD类大孔树脂吸附，如国产HPD500树脂，使绞股蓝总皂甙的提取率达到2-7％，纯度可达95％以上；采用碱液冲洗柱子，减少了树脂柱的再生处理工序，使工艺流程缩短，同时提高了设备利用率，降低生产成本。
具体实施方式
下面结合实施例对本发明作进一步说明：
实施例1
以100公斤绞股蓝为原料，将绞股蓝加入PH值为9-10的碱水中提取3次，每次的碱水分别为绞股蓝重量的8倍、6倍和6倍，提取时间分别为2小时、1.5小时和1.5小时。合并提取液，过滤后放置24小时澄清，将上清液通入HPD大孔树脂吸附，待流出液饱和后，用PH值为9-10的碱液冲洗柱子至流出液无色，再用水冲洗至中性，然后用原料7倍量的70％乙醇洗脱，收集洗脱液并脱色，回收乙醇至相对密度1.20-1.30(80℃测)时，将除去乙醇的流浸膏于80°-90°干燥5小时得绞股蓝总皂甙6.7公斤，含量为98.8％。
实施例2
以100公斤绞股蓝为原料，粉碎成粗粉，用20倍PH 9-10的碱水提取3次，提取时间分别为1.0小时、0.5小时和0.5小时。合并提取液，过滤后放置24小时澄清，将上清液通入D101大孔树脂吸附，待流出液饱和后，用PH 9-10的碱液冲洗柱子除杂至流出液无色，再用水冲洗至中性，然后用原料6倍量的80％乙醇洗脱，收集洗脱液并用LSI-632树脂脱色，回收乙醇至相对密度1.2(80℃测)时，将除去乙醇的流浸膏于70℃真空干燥5小时得绞股蓝总皂甙5.6公斤，含量为98.1％。
实施例3
以100公斤绞股蓝为原料，用20倍PH 9-10的碱水提取3次，提取时间分别为2小时、1.5小时和1.5小时。合并提取液，过滤放置澄清，将上清液通入D140大孔树脂吸附，待流出液饱和后，用PH 9-10的碱液冲洗柱子除杂至流出液无色，再用水冲洗至中性，然后用原料5倍量的95％乙醇洗脱，收集洗脱液并用LSI-632树脂脱色，回收乙醇至相对密度1.2(80℃测)时，将除去乙醇的流浸膏于60℃真空干燥5小时得绞股蓝总皂甙4.9公斤，含量为97.8％。
实施例4
以100公斤绞股蓝为原料，粉碎成粗粉，用20倍PH 9-10的碱水提取3次，提取时间分别为1小时、0.5小时和0.5小时。合并过滤，滤液放置澄清，将上清液通入D101B大孔树脂吸附，待流出液饱和后，用PH 9-10的碱液冲洗柱子除杂至流出液无色，再用水冲洗至中性，然后用原料7倍量的75％乙醇洗脱，收集洗脱液并用LSI-632树脂脱色，回收乙醇至相对密度1.2(80℃测)时，将除去乙醇的流浸膏于75℃真空干燥5小时得绞股蓝总皂甙6.0公斤，含量为96.0％。
实施例5
以100公斤绞股蓝为原料，用20倍PH 9-10的碱水提取3次，每次的碱水用量是绞股蓝重量的8倍、6倍、6倍，提取时间分别为2小时、1.5小时和1.5小时。合并提取液，过滤后放置24小时澄清，将上清液通入D101大孔树脂吸附，待流出液饱和后，用PH 9-10的碱液冲洗柱子除杂至流出液无色，再用水冲洗至中性，然后用原料6倍量的80％乙醇洗脱，收集洗脱液并用BS-1树脂脱色，回收乙醇至相对密度1.2(80℃测)时，将除去乙醇的流浸膏于70℃真空干燥5小时得绞股蓝总皂甙6.2公斤，含量为95.6％。
Claims (2)
1 一种绞股蓝总皂甙的制取方法，其特征是：以绞股蓝为原料，将绞股蓝加入PH值为9-11的碱水煮沸提取，过滤，澄清，将上清液通入大孔树脂吸附，用PH值为9-11的碱液冲洗柱子至流出液无色，再用水冲洗至中性，然后用原料5-8倍量50％-95％乙醇洗脱，脱除乙醇洗脱液中的乙醇经干燥处理得绞股蓝总皂甙制品。
2 根据权利要求1所述的绞股蓝总皂甙的制取方法，其特征是：大孔树脂采用HPD类树脂。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031144713A CN1317295C (zh) | 2003-01-16 | 2003-01-16 | 一种绞股蓝总皂甙的制取方法 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031144713A CN1317295C (zh) | 2003-01-16 | 2003-01-16 | 一种绞股蓝总皂甙的制取方法 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1517359A CN1517359A (zh) | 2004-08-04 |
| CN1317295C true CN1317295C (zh) | 2007-05-23 |
Family
ID=34283961
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB031144713A Expired - Lifetime CN1317295C (zh) | 2003-01-16 | 2003-01-16 | 一种绞股蓝总皂甙的制取方法 |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1317295C (zh) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102603849A (zh) * | 2012-02-10 | 2012-07-25 | 厦门华侨亚热带植物引种园 | 一种绞股蓝次生皂苷及其制备方法与应用 |
| CN104398677B (zh) * | 2014-11-10 | 2018-11-16 | 云南谷冠生物科技有限公司 | 一种苦荞麦总黄酮和绞股兰总皂苷复方组合物 |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1068575A (zh) * | 1992-03-11 | 1993-02-03 | 孙文基 | 长梗绞股蓝总皂甙的生产工艺 |
| CN1096433A (zh) * | 1993-06-15 | 1994-12-21 | 曾庆桂 | 绞股蓝有效成分的提取工艺及绞股蓝饮料 |
-
2003
- 2003-01-16 CN CNB031144713A patent/CN1317295C/zh not_active Expired - Lifetime
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1068575A (zh) * | 1992-03-11 | 1993-02-03 | 孙文基 | 长梗绞股蓝总皂甙的生产工艺 |
| CN1096433A (zh) * | 1993-06-15 | 1994-12-21 | 曾庆桂 | 绞股蓝有效成分的提取工艺及绞股蓝饮料 |
Non-Patent Citations (1)
| Title |
|---|
| "恩七叶甜"绞股蓝总皂甙提取工艺研究 郑小江，湖北民族学院学报(自然科学版)，第19卷第3期 2001 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1517359A (zh) | 2004-08-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100572552C (zh) | 罗汉果苷v含量≥40%的罗汉果提取物及其制备方法 | |
| CN109593034B (zh) | 一种从银杏叶提取废液中制备莽草酸的方法 | |
| CN108752231B (zh) | 从甜茶中提取茶氨酸以及同时提取甜茶苷和茶多酚的方法 | |
| CN111285916B (zh) | 一种积雪草总苷含量高的积雪草提取物的制备方法 | |
| CN106822196B (zh) | 一种从银杏叶中同时提取银杏叶多糖和银杏叶黄酮的方法 | |
| CN113896754B (zh) | 一种从黄芩中提取纯化黄芩苷的工业化生产方法 | |
| CN105175462A (zh) | 一种渗漉法提取甜菊糖的工艺 | |
| CN111269171B (zh) | 一种高纯度1-脱氧野尻霉素的制备方法 | |
| CN102977217A (zh) | 一种红薯淀粉的加工方法 | |
| CN1317294C (zh) | 一种绞股蓝总皂甙的制取方法 | |
| CN102617668A (zh) | 一种高纯度阿维菌素精粉生产工艺 | |
| CN1982279B (zh) | 一种制备莽草酸的新技术 | |
| CN107602390B (zh) | 一种从烟叶中提取绿原酸和东莨菪素的方法 | |
| CN103012518B (zh) | 一种从杜仲叶中同时提取车叶草苷和绿原酸的生产工艺 | |
| CN102250969B (zh) | 从虎杖中制备高纯度白藜芦醇的工艺 | |
| CN1317295C (zh) | 一种绞股蓝总皂甙的制取方法 | |
| CN113501759A (zh) | 一种从甜叶菊废渣中获取绿原酸和异绿原酸的方法 | |
| CN101077355A (zh) | 双效天然澄清剂及其应用技术 | |
| CN102961422B (zh) | 高纯度人参提取物的提取方法 | |
| CN112723997A (zh) | 一种提取高纯度补骨脂酚的绿色工艺 | |
| CN101985439B (zh) | 从毛冬青地上部分分离提取98%槲皮素的工艺 | |
| CN110922413A (zh) | 一种光甘草定的提取分离方法 | |
| CN101475618A (zh) | 注射用黄芩苷的精制方法 | |
| CN101543519A (zh) | 菊花提取物的制备方法 | |
| CN105837543A (zh) | 一种从发酵液中提取精制曲酸的方法 |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: Preparation method of gynostemma pentaphylia total saponin Effective date of registration: 20160104 Granted publication date: 20070523 Pledgee: Ankang city credit financing Company limited by guarantee Pledgor: ANKANG PHARMACEUTICAL INSTITUTE OF PEKING University Registration number: 2015610000022 |
|
| PLDC | Enforcement, change and cancellation of contracts on pledge of patent right or utility model | ||
| CP03 | Change of name, title or address | ||
| CP03 | Change of name, title or address |
Address after: 725000 No. 6 Pioneering East Road, Ankang High-tech Industrial Development Zone, Shaanxi Province Patentee after: Ankang Innovation Institute of Chinese Pharmaceutical Research Co.,Ltd. Address before: 725000 No. 2 Xing'an East Road, Ankang City, Shaanxi Province Patentee before: ANKANG PHARMACEUTICAL INSTITUTE OF PEKING University |
|
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20190222 Address after: 725000 No. 6 Pioneering East Road, Ankang High-tech Industrial Development Zone, Shaanxi Province Patentee after: ANKANG BEIYIDA PHARMACEUTICAL CO.,LTD. Address before: 725000 No. 6 Pioneering East Road, Ankang High-tech Industrial Development Zone, Shaanxi Province Patentee before: Ankang Innovation Institute of Chinese Pharmaceutical Research Co.,Ltd. |
|
| PC01 | Cancellation of the registration of the contract for pledge of patent right | ||
| PC01 | Cancellation of the registration of the contract for pledge of patent right |
Date of cancellation: 20210111 Granted publication date: 20070523 Pledgee: Ankang city credit financing Company limited by guarantee Pledgor: ANKANG PHARMACEUTICAL INSTITUTE OF PEKING University Registration number: 2015610000022 |
|
| CX01 | Expiry of patent term | ||
| CX01 | Expiry of patent term |
Granted publication date: 20070523 |