WO2004082695A1 - Poudre sterile shenfu et sa preparation - Google Patents

Poudre sterile shenfu et sa preparation Download PDF

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Publication number
WO2004082695A1
WO2004082695A1 PCT/CN2003/000190 CN0300190W WO2004082695A1 WO 2004082695 A1 WO2004082695 A1 WO 2004082695A1 CN 0300190 W CN0300190 W CN 0300190W WO 2004082695 A1 WO2004082695 A1 WO 2004082695A1
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WO
WIPO (PCT)
Prior art keywords
extract
water
aconite
filter
ethanol
Prior art date
Application number
PCT/CN2003/000190
Other languages
English (en)
Chinese (zh)
Inventor
Hai Yin
Yanming Zeng
Jilin Sun
Original Assignee
Sichuan Dikang Industry Holdings Group Co., Ltd.
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Sichuan Dikang Industry Holdings Group Co., Ltd. filed Critical Sichuan Dikang Industry Holdings Group Co., Ltd.
Priority to AU2003221295A priority Critical patent/AU2003221295A1/en
Priority to CN03825750.5A priority patent/CN1720056A/zh
Priority to PCT/CN2003/000190 priority patent/WO2004082695A1/fr
Publication of WO2004082695A1 publication Critical patent/WO2004082695A1/fr

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Classifications

    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18—Magnoliophyta (angiosperms)
    • A61K36/185—Magnoliopsida (dicotyledons)
    • A61K36/25—Araliaceae (Ginseng family), e.g. ivy, aralia, schefflera or tetrapanax
    • A61K36/258—Panax (ginseng)
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18—Magnoliophyta (angiosperms)
    • A61K36/185—Magnoliopsida (dicotyledons)
    • A61K36/71—Ranunculaceae (Buttercup family), e.g. larkspur, hepatica, hydrastis, columbine or goldenseal
    • A61K36/714—Aconitum (monkshood)

Definitions

  • the invention belongs to the field of pharmacy, and relates to a ginseng-containing sterile powder including a Chinese medicinal material red ginseng and aconite extracting effective parts, and a preparation method thereof. Background technique
  • the existing ginsenosides in active parts of red ginseng are generally extracted by refluxing with ethanol.
  • the disadvantages of this method of extraction are: the color of the extraction is deep, the impurities, especially the fat-soluble impurities are many, the purity of the pure dagger is difficult, the process is relatively complicated, and the cost is high.
  • the existing aconite alkaloids in effective parts of aconite are usually extracted by refluxing with ethanol. This method extracts aconite alkaloids with many pigment impurities, especially fat-soluble impurities. In addition, the effective content of aconite active ingredients is low, and subsequent purification is very difficult. The operation is complicated and costly.
  • the prepared Shenfu freeze-dried powder injection has a lot of impurities, which directly affects the efficacy of the medicine and the temperature of the product. Disclosure of invention
  • the purpose of the present invention is to provide a ginseng aseptic powder containing red ginseng and aconite extracting effective parts with a scientific preparation process, scientific mixing ratio, controllable quality, and low extraction cost.
  • Another object of the present invention is to provide a method for preparing aseptic powder.
  • the technical solution of the present invention is: a ginseng-attached sterile powder, which includes a red ginseng effective part extract and an aconite active part extract, characterized in that the red ginseng effective part extract is obtained by the following method: Weigh the required amount of red ginseng, add 10-20 times water to boil and keep at 80-90 ° C for 2 hours, filter, and drug residue add 10 to 20 times water to boil at 80-90 ° C and keep 1.
  • the ginseng water extract After 5 hours, filter, boil the residue with 10-20 times water and boil at 80-90 ° C for 1 hour, filter, combine the filtrates, and remove the precipitate by speed centrifugation to obtain the ginseng water extract; the ginseng water extract passes through Adsorption resin chromatography column. After adsorption, wash with 0.1-10% alkaline solution until colorless, and then wash with distilled water until the pH is neutral, elute with 75-85% ethanol, until no saponin reaction, elute The subsequent ethanol solution was passed through a purified decolorized resin chromatography column.
  • the effluent was collected and left to stand for 12-24 hours, filtered, and concentrated under reduced pressure to ethanol-free, filtered to obtain a transparent light yellow red ginseng extract, frozen under aseptic conditions. Dry to obtain a dry extract of the effective part of red ginseng, and the total saponin content of ginseng>50%; the extract of the effective part of aconite is obtained by the following method: Weigh the required amount of aconite, add 10-20 times PH3-9 water and boil it at 80-90 ° C Hold for 2 hours, filter, boil water with 10-20 times PH3-9 and boil at 80-90 ° C for 1.5 hours, filter, boil water with 10-20 times PH3-9 Hold at 80-90 ° C for 1 hour, filter, combine the filtrates, and remove the precipitate by speed centrifugation to obtain the aconite aqueous extract.
  • the aconite aqueous extract is passed through the adsorption resin chromatography column and washed with water until the eluate is colorless. -85% ethanol elutes to no alkaloid reaction, and passes through the purified decolorized resin chromatography column at a uniform speed. The eluate is left to be filtered and concentrated under reduced pressure to ethanol-free; filtered and freeze-dried under sterile conditions to obtain solids in the effective part of aconite. Extract containing aconite alkaloids> 50%.
  • the ginseng-containing sterile powder of the present invention comprises 10-20 parts by weight of the active part extract of red ginseng; 0.1-3.0 parts by weight of the active part extract of aconite.
  • the invention relates to a method for preparing a reference-attached sterile powder, which comprises the following steps:
  • Extract of effective part of aconite Weigh the required aconite, add 10-20 times PH3-9 water, boil it and keep it at 80-90 ° C for 2 hours, filter, add medicine residue 10-20 times PH3-9 After boiling, keep at 80-90 ° C for 1.5 hours, and filter. The residue is boiled with water at 10-20 times PH3-9. After boiling, keep at 80-90 ° C for 1 hour, filter, and combine the filtrates. Speed flow centrifugation Remove the sediment to obtain aconite water extract;
  • ginseng water extract passed through the adsorption resin chromatography column. After adsorption, it was washed with 0.1-10% alkaline solution to colorless, and then washed with distilled water until the pH was neutral. Elute with 75-85% ethanol until saponin-free reaction. The eluted ethanol solution is passed through a purified decolorizing resin chromatography column uniformly. The effluent is collected and left to stand for 12-24 hours, filtered, and the reduced pressure film is concentrated to ethanol-free, filtered. , Obtaining a transparent light yellow red ginseng extract, freeze-dried under aseptic conditions to obtain a dry extract of the effective part of red ginseng, and the total ginsenoside content is> 50%;
  • aconite water extract is passed through the adsorption resin chromatography column uniformly, washed with water until the eluent is colorless, and eluted with 75-85% ethanol until there is no alkaloid reaction, and the decolorized resin layer is purified at a uniform speed.
  • Analytical column the eluate is left to be filtered, and concentrated under reduced pressure to ethanol-free; filtered, freeze-dried under aseptic conditions to obtain a solid extract of the effective part of aconite, containing aconite alkaloid> 50%.
  • Red ginseng is dried in an oven at 80 ° C for 12 hours, crushed with a pulverizer, passed through a 20-mesh sieve, and dipped in ethanol in accordance with the method of ginseng saponin injection of Sichuan Pharmaceutical Standard
  • To extract red ginseng specifically weigh 100g of red ginseng powder and put it in a flask, soak it in 300ml of ethanol for 72 hours, filter, and use the filtrate for backup. Add 300ml of ethanol residue to the water bath and reflux for three times, 2 hours each time. Measure ginsenoside content.
  • Extraction of red ginseng using the water of the present invention Weigh 100g of red ginseng powder into a flask, add 100ml of distilled water, and boil it at 80-90 ° C for 2 hours, filter, and use the filtrate for later use. Extract the drug residue with 100ml of distilled water twice according to the aforementioned method, and the extraction time is 1.5 and 1 hour, respectively. The filtrate was sampled separately to determine the ginsenoside content.
  • Extraction of aconite from ethanol under reflux Aconite is dried in an oven at 60 ° C for 12 hours, crushed with a pulverizer, passed through a 20-mesh sieve, weighed 100g of aconite powder and placed in a clean steaming bottle, and added 80% ethanol to 500ml. Hours, filter for backup, and add 250% 80% ethanol to 250 ml reflux extraction for each time, each time is 1.5 and 1 hour, after each reflux sampling, extract extract aconite alkaloid content.
  • Extraction of aconite alkaloids using the water of the present invention Weigh 100g of aconite powder into a steamer bottle, add 1L of distilled water, and boil it for 2 hours at 80-9 ° C, filter, and use the filtrate as a reserve. Drug residue plus distilled water 1L was leached twice according to the aforementioned method, and the leaching times were 1. 5 and 1 hour. Samples were taken for alkaloid content after each boiling step.
  • Decoloring resin column control parameters 25ml alcohol solution / g decolorizing resin. After the decolorizing resin, the red ginseng and aconite extracts were 29.5L and 28.8L, respectively, and they were left overnight for 12 hours. Filter through a No. 4 glass sand funnel, and then filter with a No. 5 glass sand funnel. The membrane is concentrated under reduced pressure (temperature ⁇ 0-90 ° C, vacuum degree 68cm), and alcohol-free. Under aseptic conditions, it was filtered with a No.
  • red ginsenosides and Aconite alkaloids are 163 ⁇ 4 and 15J5g, respectively. It is slightly lower than the water extraction method, which is mainly due to the large amount of impurities and the large loss of the effective part during purification.
  • Tables 3 and 4 The results of three batches of purification and extraction are shown in Tables 3 and 4.
  • ginseng water extract passes through the adsorption resin chromatography column. After the adsorption is completed, it is washed with 0.1% alkaline solution until it is colorless, and then washed with distilled water to neutralize pH. Elute with 75% ethanol until there is no saponin reaction. After the elution, the ethanol solution is passed through a purified decolorizing resin chromatography column uniformly. The effluent is collected and allowed to stand for 12 hours, filtered, and the reduced pressure film is concentrated to ethanol-free. Yellow red ginseng extract, frozen and dried under aseptic conditions to obtain a dry extract of the effective part of red ginseng, the total saponin content of ginseng>50%;
  • aconite water extract is passed through the adsorption resin chromatography column uniformly, washed with water until the eluent is colorless, and eluted with 85% ethanol until no alkaloid reaction, and uniformly passed through the purified decolorized resin chromatography column.
  • the eluate was left to be filtered, and concentrated under reduced pressure to ethanol-free; filtered, and freeze-dried under a sterile glass to obtain a solid extract of the effective part of aconite, containing aconite alkaloids> 50%.
  • Extract of effective part of aconite Weigh the required aconite, add 10 times of PH9 water to boil, and keep it at 90 ° C for 2 hours, filter, and add 10 times of PH3 water to boil at 90 ° C. After 5 hours of filtration, the residue was boiled with 10 times PH3 of water and boiled at 90 ° C for 1 hour. After filtration, the filtrates were combined and the precipitate was removed by speed centrifugation to obtain an aqueous extract of aconite;
  • ginseng water extract passes through the adsorption resin chromatography column. After the adsorption is completed, it is washed with 10% alkaline solution until it is colorless, and then washed with distilled water until the pH is neutral, and 85% ethanol is used. Elution until saponin-free reaction. After the elution, the ethanol solution is passed through a purified decolorized resin chromatography column uniformly. The effluent is collected and allowed to stand for 24 hours, filtered, and concentrated under reduced pressure to ethanol-free. Filtered to obtain a transparent light yellow red ginseng extract. Liquid, freeze-dried under aseptic conditions to obtain a dry extract of the effective part of red ginseng, the total saponin content of ginseng> 50%;
  • aconite water extract Purification of aconite water extract: The aconite water extract is passed through an adsorption resin chromatography column with water, Wash until the eluent is colorless, and elute with 75% ethanol until there is no alkaloid reaction. Pass the purified decolorized resin chromatography column at a uniform speed. The eluent is left to stand for filtration, and concentrated under reduced pressure to ethanol-free; filtered, frozen under sterile conditions. Dry to obtain a solid extract of the effective part of aconite, containing aconite alkaloids> 50%.

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  • Health & Medical Sciences (AREA)
  • Natural Medicines & Medicinal Plants (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Alternative & Traditional Medicine (AREA)
  • Biotechnology (AREA)
  • Botany (AREA)
  • Medical Informatics (AREA)
  • Medicinal Chemistry (AREA)
  • Microbiology (AREA)
  • Mycology (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Epidemiology (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
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Abstract

L'invention porte sur une poudre stérile Shenfu comprenant l'extrait de composant actif de ginseng radix (rouge) et l'extrait de composant actif de radix aconiti praeparata. Cette invention se caractérise en ce que les deux extraits ont été isolés par extraction de l'eau et le procédé consiste à éliminer les impuretés par une colonne de résine absorbée, filtrer par une colonne de raffinage de résine décolorée et sécher pour obtenir une poudre stérile Shenfu. La teneur en ginsénosides et en alcanoïdes de radix aconiti praeparata est supérieure à 50 %.
PCT/CN2003/000190 2003-03-17 2003-03-17 Poudre sterile shenfu et sa preparation WO2004082695A1 (fr)

Priority Applications (3)

Application Number Priority Date Filing Date Title
AU2003221295A AU2003221295A1 (en) 2003-03-17 2003-03-17 Shenfu sterile powder and the preparation thereof
CN03825750.5A CN1720056A (zh) 2003-03-17 2003-03-17 参附无菌粉末及其制备方法
PCT/CN2003/000190 WO2004082695A1 (fr) 2003-03-17 2003-03-17 Poudre sterile shenfu et sa preparation

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/CN2003/000190 WO2004082695A1 (fr) 2003-03-17 2003-03-17 Poudre sterile shenfu et sa preparation

Publications (1)

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WO2004082695A1 true WO2004082695A1 (fr) 2004-09-30

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PCT/CN2003/000190 WO2004082695A1 (fr) 2003-03-17 2003-03-17 Poudre sterile shenfu et sa preparation

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CN (1) CN1720056A (fr)
AU (1) AU2003221295A1 (fr)
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20120076875A1 (en) * 2010-09-24 2012-03-29 Chen-Yu Lee Herbal medicinal composition and extract thereof for inducing proliferation of cranial nerve cells and method of manufacturing the same
CN104189041A (zh) * 2014-09-26 2014-12-10 西安皓天生物工程技术有限责任公司 一种提取人参皂苷的方法及制备得到的人参皂苷提取物

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1283499A (zh) * 1999-08-04 2001-02-14 成都迪康药物研究所 一种注射用参麦无菌粉末及其制备方法

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1283499A (zh) * 1999-08-04 2001-02-14 成都迪康药物研究所 一种注射用参麦无菌粉末及其制备方法

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
CAI XIONG ET AL.: "Study on purification process of ginsenosides with macroreticular resin", CHINESE TRADITIONAL PATENT MEDICINE, vol. 23, no. 9, September 2001 (2001-09-01), pages 631 - 634 *
YAN PING ET AL.: "Study on the extracting total sapouin of american ginseng flowers", SPECIAL WILD ECONOMIC ANIMAL AND PLANT RESEARCH, no. 4, 1999, pages 12 - 14 *
YANG HUA ET AL.: "Application of macoropore adsorbed resin for extracting and separating total alkaloidal from monshood", CHINESE TRADITIONAL PATENT MEDICINE, vol. 22, no. 8, August 2000 (2000-08-01), pages 535 - 538 *
ZHANG ZHAO-WANG ET AL.: "Component comparison with the extractions of Radix Aconiti by two methods", CHINESE TRADITIONAL PATENT MEDICINE, vol. 21, no. 1, January 1999 (1999-01-01), pages 5 - 7 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20120076875A1 (en) * 2010-09-24 2012-03-29 Chen-Yu Lee Herbal medicinal composition and extract thereof for inducing proliferation of cranial nerve cells and method of manufacturing the same
CN104189041A (zh) * 2014-09-26 2014-12-10 西安皓天生物工程技术有限责任公司 一种提取人参皂苷的方法及制备得到的人参皂苷提取物

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AU2003221295A1 (en) 2004-10-11
CN1720056A (zh) 2006-01-11

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