CN1334267A - Process for preparing total sanchinoside - Google Patents

Process for preparing total sanchinoside Download PDF

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Publication number
CN1334267A
CN1334267A CN 01108591 CN01108591A CN1334267A CN 1334267 A CN1334267 A CN 1334267A CN 01108591 CN01108591 CN 01108591 CN 01108591 A CN01108591 A CN 01108591A CN 1334267 A CN1334267 A CN 1334267A
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China
Prior art keywords
radix notoginseng
alcohol
extraction
notoginseng total
wash
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Pending
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CN 01108591
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Chinese (zh)
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杨崇仁
李海舟
黎福南
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Kunming Institute of Botany of CAS
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Kunming Institute of Botany of CAS
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Priority to CN 01108591 priority Critical patent/CN1334267A/en
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Abstract

A process for preparing total sanchinoside includes crushing notoginseng as raw material, leaching, concentrating, clarifying, desugarizing, decolouring, concentrating and drying. Its advantages are fully retaining the total sanchinoside, high purity (more than 95%), high automatization level, low cost and no pollution.

Description

The preparation method of Radix Notoginseng total glucosides
The present invention relates to a kind of is the method for feedstock production Radix Notoginseng total glucosides with the Chinese medicinal materials pseudo-ginseng.
Pseudo-ginseng (Panax notoginseng (Burk) F.H.Chen ex C.Y.Wu et K.M.Feng), have another name called pseudo-ginseng, Panax pseudoginseng, Typhonium flagelliforme (Lodd.) Blume, mountain lacquer, invaluable and blood ginseng etc., be Araliaceae (Araliaceae) Panax (Panax Linn) plant, mainly cultivate in mountain of papers area, Yunnan, being the famous valuable ingredient of traditional Chinese medicine of China, also is one of the main component of " Yunnan white powder ".Sweet and slightly bitter taste, warm in nature, the stasis of blood of loosing hemostasis, swelling and pain relieving is used for the treatment of spitting of blood, haematemesis, traumatic hemorrhage, uterine bleeding, treating swelling and pain by traumatic injury, chest ventral spine pain.Contain in the pseudo-ginseng and the similar chemical ingredients of genseng (Panax ginseng C.A.Meyer), comprising: saponin, flavones, amino acid, polysaccharide, lipid acid, aliphatics alkynes class and peptides etc.Wherein, dammarane type four-ring triterpenoid class saponin is considered to the major physiological activeconstituents of pseudo-ginseng, genseng, Radix Panacis Quinquefolii etc.Containing this abundant compounds in the Radix Notoginseng, is that the content of content soprano, particularly ginsenoside Rg1 and Rb1 is more much higher than genseng and Radix Panacis Quinquefolii in the panax species.Therefore, pseudo-ginseng is all having important exploitation to be worth aspect medicine and the natural health-care products.To the many traditionally methods with n-butanol extraction of the extraction of saponin component in the pseudo-ginseng, this method is used organic solvents such as propyl carbinol, and toxicity is big, operation is loaded down with trivial details, yield is lower, cost is high.
The purpose of this invention is to provide a kind of Radix Notoginseng total glucosides novel preparation method, replace n-butanol extraction, have level of automation height, low, the free of contamination advantage of cost, to overcome the above-mentioned weak point of prior art with resin column chromatography Solid-Phase Extraction.
In order to realize above-mentioned purpose of the present invention, the invention provides following technical scheme:
The preparation method of Radix Notoginseng total glucosides, comprise the extraction of pseudo-ginseng raw material, clarification, decolouring, desugar, the spraying drying step, after Radix Notoginseng is pulverized, in closed continuous extracting device with 70% alcohol Continuous Heat refluxing extraction 4-5 hour, concentrate alcoholic extract, it is centrifugal after static 4 hours to add finings, clear liquid adds on the macroporous adsorptive resins, deionized-distilled water wash-out carbohydrate and tannin part with 20 times of column volumes, again with the 70-90% alcohol wash-out arasaponin of 5 times of column volumes, the decolorizing column of alcohol elutriant by forming by ion exchange resin, and with 1 times of column volume 70-90% alcohol wash-out, after elutriant concentrated, spraying drying obtained Radix Notoginseng total glucosides.
For a better understanding of the present invention, illustrate that with inventive principle of the present invention and product performance detected result the present invention is than the excellent part of prior art below.
1, principle of the present invention is based on advantage such as resin absorption, exchange separation process have the extraction efficiency height, processing unit is simple and production cost is low, in the extraction of natural drug, polymeric adsorbent not only has good selectivity, also has inspissated (generally can make concentration improve about 10 times).Macroporous adsorbent resin (macro-reticular resins) is a kind of novel material, be adsorptivity and molecular sieve principle bonded parting material, the netted opening structure of polymer that itself is polymerized by vinylbenzene, toluylene or a-methacrylic ester etc., adsorptive power is strong and have a good adsorption selectivity in the aqueous solution.Its column chromatography is with the method for Solid-Phase Extraction, in absorption arasaponin class with plant in separation such as invalid components carbohydrate, and in guaranteeing the pseudo-ginseng raw medicinal material, under the prerequisite of the content of saponin constituents, optionally remove tannin and carbohydrate, effectively the enrichment Radix Notoginseng total glucosides.Ion exchange resin (Ion exchange resins) is a kind of cancellated solid spherical macromolecular compound that has, and is mainly polystyrene type (being formed by the divinylbenzene hinge).On the reticulated structure of these macromolecule resins, be connected with various different acid-basicity groups, the acid-basicity compound that exists in the natural drug extracting solution under certain condition, can take place to exchange and be combined on the resin with these acid-basicity groups, when the solution that adopts certain basicity or acidity when being adsorbed with the exchange resin of sample molecule, sample molecule can be replaced, so can reach and the separating of non-exchangeability compound.And pigment is different with the acid-basicity of arasaponin, arasaponin is that neutrality belongs to non-exchangeability compound, natural pigment mostly is acidic component and belongs to the interchangeability compound, but when the pseudo-ginseng extracting solution passes through the ion exchange resin column chromatography under neutrallty condition, pigment is by resin absorption and arasaponin is not adsorbed with the moving phase wash-out, pigment is separated, so have better decolorization with arasaponin.Therefore, the present invention uses absorption exchange resin method and can not only cut down the consumption of energy in the extraction separation of pseudo-ginseng effective ingredient----Radix Notoginseng total glucosides, shortens extraction time, improve drug effect and reduce cost, but also can change the conventional dosage forms of Chinese medicine, in the process of the modernization of Chinese medicine, play a significant role.
2, with method of the present invention 5 batches of pseudo-ginseng have been carried out middle trial production, tested product colour, yield, saponin content and principal monomer saponin content, the result is as shown in table 1:
Total saponin content measuring method: use the ginsenoside Rg1 as reference standards, Vanillin-perchloric acid colour developing adopts spectrophotometry in wavelength 560nm place, measures the optical density of different concns standard substance, according to the relation between optical density and concentration (mg/ml), draw out typical curve.With the dissolve with ethanol Radix Notoginseng total glucosides, constant volume, Vanillin-perchloric acid colorimetric estimation optical density.Just can be according to the gained optical density by the content of finding the ginsenoside Rg1 on the typical curve, and calculate the sign content of Radix Notoginseng total glucosides.
Principal monomer saponin content assay method: with Chinese patent medicine ministerial standard Radix Notoginseng total arasaponins assay item, with the content of high effective liquid chromatography for measuring ginsenoside Rg1, ginsenoside Rb1 and arasaponin R1.
Table 1 Radix Notoginseng total arasaponins content and principal monomer saponin content
Lot number Charging capacity (kg) Radix Notoginseng total glucosides (Kg) Color Yield % Total saponin content The ginsenoside Rg1 The ginsenoside Rb1 Arasaponin R1
??99101 ????5 ?300 ?32.6 White ?10.9 ??98.2% 29.5% ?32.1% ?5.2%
??99120 ????6 ?300 ?33.8 White ?11.3 ??98.8% 30.1% ?33.4% ?5.4%
??00010 ????4 ?300 ?33.6 White ?11.2 ??98.5% 29.7% ?32.6% ?5.2%
??00030 ????5 ?300 ?33.8 White ?11.3 ??98.6% 30.0% ?33.3% ?5.3%
??00031 ????2 ?300 ?34.1 White ?11.4 ??98.4% 29.7% ?33.2% ?5.3%
Conclusion as can be drawn from Table 1: the Radix Notoginseng total glucosides that method of the present invention is produced is of light color, saponin content is high, reach the standard of the Radix Notoginseng total arasaponins of Chinese patent medicine ministerial standard defined, has advantages such as yield height, production cost are low, technological specification simultaneously.
In order to understand the present invention better, further specify essentiality content of the present invention below in conjunction with embodiments of the invention, but content of the present invention is not limited thereto.
Embodiment 1:
After Radix Notoginseng 10kg pulverizes, in closed continuous extracting device with 70% alcohol Continuous Heat refluxing extraction 5 hours, concentrate alcoholic extract, it is centrifugal after static 4 hours to add finings, clear liquid adds on the macroporous adsorptive resins, with after the invalid parts such as 40 liters deionized-distilled water wash-out carbohydrates and tannin with 10 liters 75% alcohol wash-out arasaponin, the decolorizing column of 75% alcohol elutriant by forming by ion exchange resin, and it is continuous with 2 liter of 75% alcohol wash-out, after elutriant concentrates, spraying drying obtains white Radix Notoginseng total glucosides finished product 1.14kg, yield 11.4%.
Embodiment 2:
After Radix Notoginseng 10kg pulverizes, in closed continuous extracting device with 70% alcohol Continuous Heat refluxing extraction 5 hours, concentrate alcoholic extract, it is centrifugal after static 4 hours to add finings, clear liquid adds on the macroporous adsorptive resins, with after the invalid parts such as 40 liters deionized-distilled water wash-out carbohydrates and tannin with 10 liters 80% alcohol wash-out arasaponin, the decolorizing column of 80% alcohol elutriant by forming by ion exchange resin, and it is continuous with 2 liter of 80% alcohol wash-out, after elutriant concentrates, spraying drying obtains white Radix Notoginseng total glucosides finished product 1.18kg, yield 11.8%.
Embodiment 3:
After Radix Notoginseng 10kg pulverizes, in closed continuous extracting device with 80% alcohol Continuous Heat refluxing extraction 5 hours, concentrate alcoholic extract, it is centrifugal after static 4 hours to add finings, clear liquid adds on the macroporous adsorptive resins, with after the invalid parts such as 40 liters deionized-distilled water wash-out carbohydrates and tannin with 10 liters 90% alcohol wash-out arasaponin, the decolorizing column of 90% alcohol elutriant by forming by ion exchange resin, and it is continuous with 2 liter of 90% alcohol wash-out, after elutriant concentrates, spraying drying obtains white three general glycoside finished product 1.08kg, yield 10.8%.

Claims (1)

1, the preparation method of Radix Notoginseng total glucosides, comprise the extraction of pseudo-ginseng raw material, clarification, decolouring, desugar, the spraying drying step, after it is characterized in that Radix Notoginseng is pulverized, in closed continuous extracting device with 70% alcohol Continuous Heat refluxing extraction 4-5 hour, concentrate alcoholic extract, it is centrifugal after static 4 hours to add finings, clear liquid adds on the macroporous adsorptive resins, deionized-distilled water wash-out carbohydrate and tannin part with 20 times of column volumes, again with the 70-90% alcohol wash-out arasaponin alcohol elutriant of 5 times of column volumes decolorizing column by forming by ion exchange resin, and with 1 times of column volume 70-90% alcohol wash-out, after elutriant concentrated, spraying drying obtained Radix Notoginseng total glucosides.
CN 01108591 2001-06-28 2001-06-28 Process for preparing total sanchinoside Pending CN1334267A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1825860A1 (en) * 2004-11-09 2007-08-29 The Pharmaceutical Factory of Chengdu Hoist Inc., Ltd. A panaxatriol saponins composition and its preparing method and the use
CN102204944A (en) * 2011-05-26 2011-10-05 沈阳神龙药业有限公司 Preparation method of raw materials of Xuesaitong (thrombus removal) injection
CN103251541A (en) * 2013-05-30 2013-08-21 云南七丹药业股份有限公司 Liquid shampoo containing notoginsenoside and preparation method thereof
CN103462009A (en) * 2013-09-04 2013-12-25 云南七丹药业股份有限公司 Traditional Chinese medicine extract for assisting reduction of blood fat and preparation method thereof
CN103520193A (en) * 2009-09-24 2014-01-22 昆明制药集团股份有限公司 Pharmaceutical composition and preparation method thereof
CN109432151A (en) * 2018-12-29 2019-03-08 金七药业股份有限公司 Method for improving Radix Notoginseng under ground portion recovery rate
WO2020113450A1 (en) * 2018-12-03 2020-06-11 泰州医药城国科化物生物医药科技有限公司 Preparation method for pseudo-ginseng total saponins by means of extraction and purification

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1825860A1 (en) * 2004-11-09 2007-08-29 The Pharmaceutical Factory of Chengdu Hoist Inc., Ltd. A panaxatriol saponins composition and its preparing method and the use
EP1825860A4 (en) * 2004-11-09 2009-03-11 Pharmaceutical Factory Of Chen A panaxatriol saponins composition and its preparing method and the use
CN103520193A (en) * 2009-09-24 2014-01-22 昆明制药集团股份有限公司 Pharmaceutical composition and preparation method thereof
CN102204944A (en) * 2011-05-26 2011-10-05 沈阳神龙药业有限公司 Preparation method of raw materials of Xuesaitong (thrombus removal) injection
CN102204944B (en) * 2011-05-26 2012-11-21 沈阳神龙药业有限公司 Preparation method of raw materials of Xuesaitong (thrombus removal) injection
CN103251541A (en) * 2013-05-30 2013-08-21 云南七丹药业股份有限公司 Liquid shampoo containing notoginsenoside and preparation method thereof
CN103462009A (en) * 2013-09-04 2013-12-25 云南七丹药业股份有限公司 Traditional Chinese medicine extract for assisting reduction of blood fat and preparation method thereof
WO2020113450A1 (en) * 2018-12-03 2020-06-11 泰州医药城国科化物生物医药科技有限公司 Preparation method for pseudo-ginseng total saponins by means of extraction and purification
CN109432151A (en) * 2018-12-29 2019-03-08 金七药业股份有限公司 Method for improving Radix Notoginseng under ground portion recovery rate

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