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CN1329094A - Extraction and separation method of notoginseng polysaccharide - Google Patents

Extraction and separation method of notoginseng polysaccharide Download PDF

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Publication number
CN1329094A
CN1329094A CN 01108493 CN01108493A CN1329094A CN 1329094 A CN1329094 A CN 1329094A CN 01108493 CN01108493 CN 01108493 CN 01108493 A CN01108493 A CN 01108493A CN 1329094 A CN1329094 A CN 1329094A
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precipitate
polysaccharide
ethanol
notoginseng polysaccharide
notoginseng
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杨崇仁
王东
李海舟
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Kunming Institute of Botany of CAS
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Kunming Institute of Botany of CAS
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Abstract

提供一种三七多糖的提取分离方法,该方法以中药三七为原料生产三七多糖,增加了三七原料的综合利用,降低多糖的杂质,减少了溶剂用量,降低了成本,同时提高了生产效率,适合于大规模生产。同时,提供了用上述方法得到的三七多糖在制备抗肿瘤药物中的应用;三七多糖在制备增强免疫活性药物中的应用以及三七多糖在制备抗肝炎药物中的应用。A method for extracting and separating Panax notoginseng polysaccharide is provided. The method uses the traditional Chinese medicine Panax notoginseng as a raw material to produce Panax notoginseng polysaccharide, which increases the comprehensive utilization of Panax notoginseng raw materials, reduces the impurities of the polysaccharide, reduces the amount of solvent used, and reduces the cost. The production efficiency is improved, and it is suitable for large-scale production. At the same time, it provides the application of the notoginseng polysaccharide obtained by the above method in the preparation of antitumor drugs; the application of the notoginseng polysaccharide in the preparation of drugs for enhancing immune activity;

Description

The extraction and separation method of Radix Notoginseng polysaccharide
The invention belongs to the pharmaceutical chemistry field, specifically, belong to the extraction and separation method of medicinal plant Radix Notoginseng polysaccharide.
Pseudo-ginseng (Panax notoginseng (Burk.) F.H.Chen), have another name called pseudo-ginseng, be Araliaceae (Araliaceae) Panax (Panax Linn.) plant, mainly cultivate in Yunnan mountain of papers and Baise of Guangxi area, it is the famous valuable ingredient of traditional Chinese medicine of China, have hemostasis, loose effects such as silt, detumescence, pain relieving in recent years, the research and development of pseudo-ginseng come into one's own day by day.The pseudo-ginseng complex chemical composition was just studied from the thirties, but after the seventies along with the separation of plant glycoside and the development of chemical structure authenticate technology, significant progress has just been arranged.Result of study shows, contains saponin, flavones, amino acid, polysaccharide, lipid acid, aliphatics alkynes class and peptides etc. in the pseudo-ginseng, is all having important exploitation to be worth aspect pharmaceuticals and the natural health-care products.Wherein, dammarane type four-ring triterpenoid class saponin is considered to one of major physiological activeconstituents of pseudo-ginseng.So research in the past mainly concentrates on the arasaponin aspect, the polysaccharide component of pseudo-ginseng to be studied seldom, the extraction and separation method of Radix Notoginseng polysaccharide of the present invention is not seen in the prior art report.
The object of the present invention is to provide a kind of extraction and separation method of Radix Notoginseng polysaccharide, this method is the raw material production Radix Notoginseng polysaccharide with the Chinese medicine pseudo-ginseng, increased the comprehensive utilization of pseudo-ginseng raw material, reduce the impurity of polysaccharide, reduced solvent load, reduce cost, improved production efficiency simultaneously, be suitable for scale operation.Simultaneously, the present invention also provides the application of Radix Notoginseng polysaccharide in the preparation antitumor drug that aforesaid method obtains; Application and Radix Notoginseng polysaccharide the application in preparation Antihepatitis medicament of Radix Notoginseng polysaccharide in preparation enhancing immunity active medicine.
In order to realize above-mentioned purpose of the present invention, the invention provides following technical scheme:
The extraction and separation method of Radix Notoginseng polysaccharide is got Radix Notoginseng, uses boiling water extraction after crushed, and extracting solution is centrifugal or filter, and adds the long-pending ethanol sedimentation of diploid after clear liquid concentrates, collects centrifugal or filter after precipitation, get Radix Notoginseng polysaccharide after the drying.
In the aforesaid method, Radix Notoginseng is pulverized the back with boiling water extraction three times, and cooled and filtered is removed precipitation, and the clear liquid thin film concentration adds the long-pending ethanol of diploid and mixes to small volume, leaves standstill after one hour 9000rpm centrifugal 10 minutes, and collecting precipitation precipitate the dry Radix Notoginseng polysaccharide that gets.
In the aforesaid method, Radix Notoginseng is pulverized back boiling water extraction three times, cooled and filtered is removed precipitation, the clear liquid spraying drying gets dry powder, and dry powder is dissolved in boiling water, the centrifugal precipitation of going, clear liquid adds the long-pending ethanol of diploid and mixes, left standstill after one hour 9000rpm centrifugal 10 minutes, collecting precipitation, dry Radix Notoginseng polysaccharide.
The another kind of extraction and separation method of Radix Notoginseng polysaccharide is provided simultaneously, get Radix Notoginseng, use extraction using alcohol after crushed, ethanol extract is used to prepare arasaponin, residue is used boiling water extraction again, and the centrifugal or filtration of water extract adds the long-pending ethanol sedimentation of diploid after clear liquid concentrates, collect centrifugal or filter after precipitation, after the drying Radix Notoginseng polysaccharide.
In the aforesaid method, Radix Notoginseng is pulverized the back with 70% alcohol reflux, use boiling water extraction three times after the residue drying, cooled and filtered is removed precipitation, the clear liquid thin film concentration is to small volume, adds the long-pending ethanol of diploid and mixes, and leaves standstill after one hour 9000rpm centrifugal 10 minutes, collecting precipitation precipitates the dry Radix Notoginseng polysaccharide that gets.
In the aforesaid method, Radix Notoginseng is pulverized the back with 70% alcohol reflux, use boiling water extraction three times after the residue drying, cooled and filtered is removed precipitation, and the clear liquid spraying drying gets dry powder, get dry powder and be dissolved in boiling water, the centrifugal precipitation of going, clear liquid adds the long-pending ethanol of diploid and mixes, and leaves standstill after one hour 9000rpm centrifugal 10 minutes, collecting precipitation, the dry Radix Notoginseng polysaccharide that gets.
Simultaneously, the present invention also provides the application of the Radix Notoginseng polysaccharide that obtains with aforesaid method in the preparation antitumor drug; Application and Radix Notoginseng polysaccharide the application in preparation Antihepatitis medicament of Radix Notoginseng polysaccharide in preparation enhancing immunity active medicine.
In order to embody the compared with prior art existing superiority of the present invention, the pharmacology test result of the product that will go out with principle of the present invention and extraction separation of the present invention illustrates its superiority and purposes below:
1, principle of the present invention: the proposition of technical solution of the present invention is that the principle that can not be dissolved in alcohol according to the polysaccharide water soluble utilizes the method for ethanol sedimentation to extract Radix Notoginseng polysaccharide.
2, the pharmacology test result of Radix Notoginseng polysaccharide:
The Radix Notoginseng polysaccharide that obtains with extraction and separation method of the present invention carries out pharmacology test, and preliminary study result shows that Radix Notoginseng polysaccharide is to CCl 4Due to the kunming mice liver injury have significant protective effect, to animal transplanting tumor S 180The solid-type growth has the obvious suppression effect, to animal transplanting tumor liver cancer (H 22) solid-type growth has the obvious suppression effect, it is active and suppress the activity of hepatitis virus also to have significant enhancing immunity, and its toxicology test has also proved its security, has good application prospects.
2-1. Radix Notoginseng polysaccharide is to the provide protection of carbon tetrachloride hepatic injury
The result shows through preliminary experiment: give the animal abdominal injection, Radix Notoginseng polysaccharide dosage is respectively 75mg/kg and 150mg/kg, once a day, logotype three days, (0.1%, 10mg/kg) the kunming mice liver injury due to has the certain protection effect to tetracol phenixin.Gpt (ALT) is an evaluation index in the serum to measure.Model group ALT136.7 ± 15.6u; Polysaccharide dosage size is followed successively by 58.0 ± 22.3u and 80.2 ± 19.7u respectively, with model group (CCl 4) compare, difference has significance (p<0.05).
2-2. Radix Notoginseng polysaccharide is to the influence of animal transplanting tumor growth
(1) to animal transplanting tumor S 180The influence of solid-type growth
The result shows through preliminary experiment: Radix Notoginseng polysaccharide is 100mg/kg and 200mg/kg at dosage, once a day, logotype 8 days, the heavy inhibiting rate of knurl is followed successively by 23.8% and 37.3% respectively, and heavy dose of group is compared with control group has notable difference (p<0.05).
(2) to animal transplanting tumor liver cancer (H 22) influence of solid-type growth
The result shows through preliminary experiment: Radix Notoginseng polysaccharide is 100mg/kg and 200mg/kg at dosage, once a day, logotype 8 days, the heavy inhibiting rate of knurl is followed successively by 34.6% and 46.5% respectively, compares with control group all to have notable difference (p<0.05).
To sum up, compared with prior art, superiority of the present invention is:
1, prior art mainly concentrates on arasaponin research and extracts, the polysaccharide component of pseudo-ginseng is studied seldom, and be that the raw material production Radix Notoginseng polysaccharide does not appear in the newspapers with the Chinese medicine pseudo-ginseng;
2, the present invention at first uses 70% extraction using alcohol arasaponin, carries out the extraction of polysaccharide again, can strengthen the comprehensive utilization to the pseudo-ginseng raw material, increases the benefit, and can reduce the impurity of polysaccharide simultaneously;
3, prior art utilizes triploid to amass the ethanol sedimentation polysaccharide, and the present invention utilizes diploid to amass the ethanol sedimentation polysaccharide, also can achieve the goal, and can reduce the ethanol consumption, reduces cost;
4, the present invention utilizes spray drying process to concentrate the pseudo-ginseng water extract, has improved production efficiency, is suitable for large-scale industrial production;
5, do not see in the prior art that the application of Radix Notoginseng polysaccharide in the preparation antitumor drug arranged, the application of Radix Notoginseng polysaccharide in preparation enhancing immunity active medicine and the report of the application of Radix Notoginseng polysaccharide in the preparation Antihepatitis medicament.
Further specify essentiality content of the present invention with the embodiment of the invention below, but content of the present invention is not limited thereto.
Embodiment 1:
Material: Radix Notoginseng is dry medicinal material, originates from the Yunnan mountain of papers; Ethanol is that chemical reagent one factory in Tianjin produces, and whizzer is the Beckman product.
Experimental technique:
Get Radix Notoginseng 3kg, pulverize the back with boiling water extraction three times, cooled and filtered is removed precipitation, and the clear liquid thin film concentration adds the long-pending ethanol of diploid and mixes to small volume, leaves standstill after one hour 9000rpm centrifugal 10 minutes, and collecting precipitation precipitate the dry Radix Notoginseng polysaccharide 41g of getting.
Embodiment 2:
Material is selected with embodiment 1.Get Radix Notoginseng 3kg and pulverize back boiling water extraction three times, cooled and filtered is removed precipitation, the clear liquid spraying drying gets the about 100g of dry powder, dry powder is dissolved in boiling water, cross elimination precipitation, clear liquid adds the long-pending ethanol of diploid and mixes, and leaves standstill after one hour 9000rpm centrifugal 10 minutes, collecting precipitation, the dry Radix Notoginseng polysaccharide 33g that gets.
Embodiment 3:
Material is selected with embodiment 1.Get Radix Notoginseng 3kg, pulverize the back with 70% alcohol reflux, use boiling water extraction three times after the residue drying, cooled and filtered is removed precipitation, the clear liquid thin film concentration is to small volume, adds the long-pending ethanol of diploid and mixes, and leaves standstill after one hour 9000rpm centrifugal 10 minutes, collecting precipitation precipitates the dry Radix Notoginseng polysaccharide 35g of getting.
Embodiment 4:
Material is selected with embodiment 1.Get Radix Notoginseng 100kg, pulverize the back with 70% alcohol reflux, use boiling water extraction three times after the residue drying, cooled and filtered is removed precipitation, and the clear liquid spraying drying gets the about 3.5kg of dry powder, get dry powder 1kg and be dissolved in boiling water, centrifugal (or filter) goes precipitation, and the stillness of night adds the long-pending ethanol of diploid and mixes, and leaves standstill after one hour 9000rpm centrifugal 10 minutes, collecting precipitation, the dry Radix Notoginseng polysaccharide 390g that gets.

Claims (9)

1、三七多糖的提取分离方法,其特征是取三七根,经粉碎后用沸水提取,提取液离心或过滤,清液浓缩后加二倍体积乙醇沉淀,收集离心或过滤后的沉淀,干燥后得三七多糖。1. The extraction and separation method of Panax notoginseng polysaccharide is characterized in that notoginseng root is taken, extracted with boiling water after being pulverized, the extract is centrifuged or filtered, the supernatant is concentrated and then added with twice the volume of ethanol for precipitation, and the precipitate after centrifugation or filtration is collected , and dried to obtain Panax notoginseng polysaccharide. 2、根据权利要求1所说的方法,其特征是三七根粉碎后用沸水提取三次,冷却后过滤去除沉淀,清液薄膜浓缩至小体积,加二倍体积的乙醇混合,静置一小时后9000rpm离心10分钟,收集沉淀,沉淀干燥得三七多糖。2. The method according to claim 1, characterized in that the roots of Panax notoginseng are crushed and extracted three times with boiling water, filtered to remove the precipitate after cooling, the clear liquid film is concentrated to a small volume, mixed with twice the volume of ethanol, and left to stand for one hour Then centrifuge at 9000rpm for 10 minutes, collect the precipitate, and dry the precipitate to obtain Panax notoginseng polysaccharide. 3、根据权利要求1所说的方法,其特征是三七根粉碎后用沸水提取三次,冷却后过滤去除沉淀,清液喷雾干燥得干粉,干粉溶于沸水,离心去沉淀,清液加二倍体积的乙醇混合,静置一小时后9000rpm离心10分钟,收集沉淀,干燥得三七多糖。3. The method according to claim 1, characterized in that the roots of Panax notoginseng are crushed and extracted three times with boiling water, filtered to remove the precipitate after cooling, the clear liquid is spray-dried to obtain dry powder, the dry powder is dissolved in boiling water, centrifuged to remove the precipitate, and the clear liquid is added with two Double the volume of ethanol was mixed, and after standing for one hour, centrifuged at 9000rpm for 10 minutes, the precipitate was collected and dried to obtain Panax notoginseng polysaccharide. 4、三七多糖的提取分离方法,其特征是取三七根,经粉碎后用乙醇提取,乙醇提取液用于制备三七皂甙,残渣再用沸水提取,水提液离心或过滤,清液浓缩后加二倍体积乙醇沉淀,收集离心或过滤后的沉淀,干燥后得三七多糖。4. The extraction and separation method of notoginseng polysaccharide is characterized in that notoginseng roots are taken, extracted with ethanol after crushing, the ethanol extract is used to prepare notoginseng saponins, the residue is extracted with boiling water, the water extract is centrifuged or filtered, and cleaned After the solution is concentrated, add twice the volume of ethanol for precipitation, collect the precipitate after centrifugation or filtration, and dry it to obtain the Panax notoginseng polysaccharide. 5、根据权利要求4所说的方法,其特征是三七根粉碎后以70%乙醇回流提取,残渣干燥后用沸水提取三次,冷却后过滤去除沉淀,清液薄膜浓缩至小体积,加二倍体积的乙醇混合,静置一小时后9000rpm离心10分钟,收集沉淀,沉淀干燥得三七多糖。5. The method according to claim 4, characterized in that the roots of Panax notoginseng are crushed and extracted with 70% ethanol under reflux, the residue is dried and extracted three times with boiling water, filtered to remove the precipitate after cooling, the clear liquid film is concentrated to a small volume, and two Double the volume of ethanol was mixed, and after standing for one hour, centrifuged at 9000rpm for 10 minutes, the precipitate was collected, and the precipitate was dried to obtain Panax notoginseng polysaccharide. 6、根据权利要求4所说的方法,其特征是三七根粉碎后以70%乙醇回流提取,残渣干燥后用沸水提取三次,冷却后过滤去除沉淀,清液喷雾干燥得干粉,取干粉溶于沸水,离心去沉淀,清液加二倍体积的乙醇混合,静置一小时后9000rpm离心10分钟,收集沉淀,干燥得三七多糖。6. The method according to claim 4, characterized in that notoginseng root is pulverized and extracted with 70% ethanol under reflux, the residue is dried and extracted three times with boiling water, filtered to remove the precipitate after cooling, the clear liquid is spray-dried to obtain a dry powder, and the dry powder is dissolved Centrifuge in boiling water to remove the precipitate, add twice the volume of ethanol to the supernatant and mix, let stand for one hour, then centrifuge at 9,000 rpm for 10 minutes, collect the precipitate, and dry to obtain Panax notoginseng polysaccharide. 7、用权利要求1或4所说的方法得到的三七多糖在制备抗肿瘤药物中的应用。7. The use of the notoginseng polysaccharide obtained by the method of claim 1 or 4 in the preparation of antitumor drugs. 8、用权利要求1或4所说的方法得到的三七多糖在制备增强免疫活性药物中的应用。8. The use of the notoginseng polysaccharide obtained by the method of claim 1 or 4 in the preparation of drugs for enhancing immune activity. 9、用权利要求1或4所说的方法得到的三七多糖在制备抗肝炎药物中的应用。9. The use of the notoginseng polysaccharide obtained by the method of claim 1 or 4 in the preparation of anti-hepatitis drugs.
CN 01108493 2001-05-31 2001-05-31 Extraction and separation method of notoginseng polysaccharide Pending CN1329094A (en)

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Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102585029A (en) * 2012-03-08 2012-07-18 玉溪市维和生物技术有限责任公司 Preparation method and application of physiologically active notoginseng polysaccharide
CN102961424A (en) * 2012-11-23 2013-03-13 云南云科药业有限公司 Panax notoginseng polysaccharide extract and preparation method, preparations and applications thereof
CN103087211A (en) * 2013-01-16 2013-05-08 中国科学院昆明植物研究所 Method for reducing ash content of notoginseng polysaccharide
CN103589811A (en) * 2012-08-15 2014-02-19 天津天士力现代中药资源有限公司 Separation and purification method for monosaccharides and disaccharides in compound red sage root extract
CN104710538A (en) * 2013-12-16 2015-06-17 中国科学院上海药物研究所 Arabinogalactan of flowers of panax notoginseng (burK.)F.H.Chen, and preparation method and use thereof
CN106119429A (en) * 2016-06-27 2016-11-16 云南省农业科学院甘蔗研究所 A kind of production method of Radix Notoginseng sugar
CN106361602A (en) * 2016-08-24 2017-02-01 登封市科创商务咨询有限公司 Panax notoginseng polysaccharide balancing and moisturizing lotion
CN106565849A (en) * 2016-10-20 2017-04-19 河南中医药大学 A method of preparing sedum aizoon L. polysaccharides and applications of the polysaccharides
CN106832037A (en) * 2017-03-30 2017-06-13 云南润嘉药业有限公司 A kind of notoginseng polysaccharide extracting method rapidly and efficiently
CN109354629A (en) * 2018-09-07 2019-02-19 云南多糖生物科技有限公司 It is a kind of neutrality notoginseng polysaccharide method for extraction and purification and application
CN109467612A (en) * 2018-11-01 2019-03-15 山东汇润膳食堂股份有限公司 A kind of method for separating and extracting Panax notoginseng with alcohol grinding
CN116375903A (en) * 2023-04-23 2023-07-04 南京林业大学 Preparation method of natural notoginseng polysaccharide and Pickering emulsion preparation method

Cited By (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102585029A (en) * 2012-03-08 2012-07-18 玉溪市维和生物技术有限责任公司 Preparation method and application of physiologically active notoginseng polysaccharide
CN103589811A (en) * 2012-08-15 2014-02-19 天津天士力现代中药资源有限公司 Separation and purification method for monosaccharides and disaccharides in compound red sage root extract
CN102961424A (en) * 2012-11-23 2013-03-13 云南云科药业有限公司 Panax notoginseng polysaccharide extract and preparation method, preparations and applications thereof
CN103087211A (en) * 2013-01-16 2013-05-08 中国科学院昆明植物研究所 Method for reducing ash content of notoginseng polysaccharide
CN104710538B (en) * 2013-12-16 2017-10-31 中国科学院上海药物研究所 A kind of sanchi flower arabogalactan and its production and use
CN104710538A (en) * 2013-12-16 2015-06-17 中国科学院上海药物研究所 Arabinogalactan of flowers of panax notoginseng (burK.)F.H.Chen, and preparation method and use thereof
WO2015090180A1 (en) * 2013-12-16 2015-06-25 中国科学院上海药物研究所 Sanchi flower arab galactan and preparation method and use thereof
CN106119429A (en) * 2016-06-27 2016-11-16 云南省农业科学院甘蔗研究所 A kind of production method of Radix Notoginseng sugar
CN106361602A (en) * 2016-08-24 2017-02-01 登封市科创商务咨询有限公司 Panax notoginseng polysaccharide balancing and moisturizing lotion
CN106565849A (en) * 2016-10-20 2017-04-19 河南中医药大学 A method of preparing sedum aizoon L. polysaccharides and applications of the polysaccharides
CN106565849B (en) * 2016-10-20 2018-10-09 河南中医药大学 A kind of preparation method and applications of aizoon stonecrop polysaccharide
CN106832037A (en) * 2017-03-30 2017-06-13 云南润嘉药业有限公司 A kind of notoginseng polysaccharide extracting method rapidly and efficiently
CN109354629A (en) * 2018-09-07 2019-02-19 云南多糖生物科技有限公司 It is a kind of neutrality notoginseng polysaccharide method for extraction and purification and application
CN109467612A (en) * 2018-11-01 2019-03-15 山东汇润膳食堂股份有限公司 A kind of method for separating and extracting Panax notoginseng with alcohol grinding
CN116375903A (en) * 2023-04-23 2023-07-04 南京林业大学 Preparation method of natural notoginseng polysaccharide and Pickering emulsion preparation method
CN116375903B (en) * 2023-04-23 2024-01-26 南京林业大学 Preparation method of natural pseudo-ginseng polysaccharide and preparation method of Pickering emulsion

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