CN1264529C - Freeze-dried 'Shenqifuzheng' powder for injection and its preparing process - Google Patents
Freeze-dried 'Shenqifuzheng' powder for injection and its preparing process Download PDFInfo
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Abstract
The present invention relates to a method for preparing injection solution of Shenqi Fuzheng freezing dried powder for injection. The present invention is characterized in that active components of tangshen and milkvetch root are extracted by a water extraction method, polysaccharide effective parts are obtained by an alcohol deposition method, and effective parts of total saponins class are obtained by an organic solvent extraction method. The obtained polysaccharide effective parts and the obtained effective parts of the total saponins class are prepared into solution, a right amount of excipient vehicle is added, the mixture is filtered, is separated for pack, is sterilized, and is dried by using a subzero method to obtain the injection solution of the Shenqi Fuzheng freezing dried powder. The injection solution of the Shenqi Fuzheng freezing dried powder of the present invention has the advantages of high effective component content, high stability and conspicuous curative effect.
Description
Affiliated technical field
The invention belongs to field of traditional Chinese medicine pharmacy, more specifically relate to a kind of method for preparing injection SHENQI FUZHENG freeze-dried powder.
Background technology
SHENQI FUZHENG ZHUSHEYE is to use more a kind of Chinese medicine at present clinically, it is formed by Radix Codonopsis and the Radix Astragali two flavor Chinese medicine equivalent prescriptions, late tumor patient to qi-deficiency type has good curative effect clinically, centralizing function with lung benefiting spleen invigorating, benefiting qi and nourishing blood, can obviously improve disease, patient's clinical symptoms, improve life quality.With the chemotherapeutics fit applications, have efficacy enhancing and toxicity reducing, improve the effect of autoimmunity.Existing SHENQI FUZHENG ZHUSHEYE adopts decoction and alcohol sedimentation technique preparation (Chinese patent medicine ministry standard WS-459 (Z-065) and WS-387 (Z-50)-99), precipitate with ethanol after the water heating extraction, this process using alcohol deposition method edulcoration purification, purification effect is not very good, its content of effective is not high, and in the precipitate with ethanol remove impurity, glycocalix precipitate with ethanol in the Radix Codonopsis and the Radix Astragali is removed, and Radix Codonopsis polysaccharide and astragalus polysaccharides have the effect (Zhang Xiaojun that improves immunity preferably, Hu Li, relying little equality. Radix Codonopsis polysaccharide is to the influence [J] of mouse immune and hemopoietic function. new Chinese medicine and clinical pharmacology 2003,14 (3): 174-176; Liu Xing is humorous, Wang Meiying, Wu Housheng etc. the separation of astragalus polysaccharides and immunocompetent research [J] thereof. and research and development of natural products, 1994,16 (1): 23; Single person of outstanding talent, Wang Shunchun, Liu Di etc.The chemistry of astragalus polysaccharides and pharmacological research progress [J]. Shanghai Univ. of Traditional Chinese Medicine's journal 2000,14 (3): 61-65); There is transportation inconvenience in injection, and problems such as quality stability difference need make improvements.Be the further curative effect that improves, clinical better medicine, plan employing water extraction, cooperation organic solvent extraction, the active component in extraction, purification Radix Codonopsis and the Radix Astragali of providing is provided.
Contain effective ingredient such as flavone, glycoside, saponin in the Chinese traditional medicine water extract, also contain simultaneously impurity such as starch, polysaccharide, protein, phlegmatic temperament, tannin, pigment, resin, pectin, make that the solid preparation dose is big, the clarity of liquid preparation (as oral liquid, injection) is bad.For overcoming this shortcoming, extract and adopt the purification process remove impurity often.According to the Chinese medicine saponin component at organic solvent, the characteristics that big dissolubility is particularly arranged in n-butyl alcohol and isoamyl alcohol, solvent extraction extracts, the purification saponin component so adopt, behind the organic solvent extraction, utilize alkaline solution washing organic solution, can remove the part acid impurities, reach the purpose of separation and purification.The present invention adopts water extraction to extract active component in the Radix Codonopsis and the Radix Astragali, is settled out Radix Codonopsis and astragalus polysaccharides with alcohol deposition method earlier; Get the solution of precipitation behind the polysaccharide, reclaim ethanol to tasteless, add an amount of distilled water and make resolution of precipitate, the reuse organic solvent extracts, and saponin component is separated with the bigger impurity of water solublity in the solution, thereby reach the purpose of separation and purification.Preparation technology of the present invention in the purification remove impurity, has kept the polysaccharide component that has immunological enhancement in the Radix Codonopsis and the Radix Astragali again.Therefore, adopt the lyophilized injectable powder of the present invention's preparation, have active component content height, the characteristics of better stability of preparation.
Summary of the invention
The object of the present invention is to provide a kind of preparation technology rationally, good stability, injection SHENQI FUZHENG freeze-dried powder that active constituent content is high.It is characterized in that adopting the active component in the water extraction extraction Radix Codonopsis and the Radix Astragali, the water extract filters with the ethanol precipitation of 70%-80%, must precipitate and supernatant; Get to precipitate and use an amount of dissolved in distilled water, reuse 80% ethanol precipitation once filters, and 1% solution is made in the dissolving of precipitation adding distil water, crosses hollow fiber column ultrafilter (molecular cut off is greater than 6000), and filtrate decompression is concentrated into dried, gets polysaccharide effective site; The supernatant of water extract alcohol post precipitation, reclaim ethanol to there not being the alcohol flavor, add an amount of distilled water, make resolution of precipitate, filter, with organic solvent extraction three times, organic solvent extraction liquid merges, the sodium hydroxide solution water washing secondary with 1%, discard alkaline solution, organic solvent extraction liquid decompression and solvent recovery, drying obtains Radix Codonopsis and Radix Astragali total saponins effective kind part.Get Radix Codonopsis and Radix Astragali saponin effective kind part 2-10 part, polysaccharide effective site 1-8 part adds an amount of dissolved in distilled water, add freeze-dried excipient 5-50 part, isoosmotic adjusting agent 6-60 part, with water for injection wiring solution-forming 600-1400 part, decolorizing with activated carbon, filter with 0.1%, regulate pH value to 7-7.5, filter packing, sterilization, frozen drying, promptly.Adopt preparation technology of the present invention, the effective ingredient in the Radix Codonopsis and the Radix Astragali obtains good purification, and the content of total saponins can reach 30-60% in its saponins effective site, has the active component content height, prepares fast advantage.
Content of the present invention is achieved through the following technical solutions:
One, medical material pre-treatment
Granule is chosen, cleans, dries, is ground into to medical material Radix Codonopsis, the Radix Astragali respectively.
Two, extraction process
Get Radix Codonopsis, the Milkvetch Root granule of equivalent, the deionized water extraction of doubly measuring with 6-15 (extraction can be adopted decocting method, percolation and infusion process) 3 times, extracting solution merges, filter, filtrate is condensed into the medicinal liquid that every 1ml is equivalent to the 1.5g crude drug, and the 60%-80% precipitate with ethanol leaves standstill, filter, must precipitate and filtered solution; An amount of dissolved in distilled water of precipitation, reuse 80% ethanol precipitation once filter, and the precipitation adding distil water is dissolved into 1% solution, crosses hollow fiber column ultrafilter (molecular cut off is greater than 6000), and ultrafiltrate is evaporated to dried, gets polysaccharide effective site.The supernatant of water extract alcohol post precipitation, decompression recycling ethanol is to there not being the alcohol flavor, adding distil water makes resolution of precipitate, filters, and three times (organic solvent can be any organic solvent that is used to extract saponin component in the natural product chemistry with organic solvent extraction, comprise n-butyl alcohol and isoamyl alcohol), extract merges, and washs secondary with 1% aqueous sodium hydroxide washes, discards alkaline solution, reclaim under reduced pressure organic solvent extraction liquid and be concentrated into dried, Radix Codonopsis and Radix Astragali total saponins effective kind part.
Three, a kind of preparation technology of freeze dried ginseng-astragalus powder for injection to strengthen body's resistance
1, a kind of prescription of freeze dried ginseng-astragalus powder for injection to strengthen body's resistance consists of by weight:
Radix Codonopsis and Radix Astragali saponin effective kind part 1-10 part
Radix Codonopsis and astragalus polysaccharides effective kind part 1-8 part
Freeze-dried excipient 5-60 part
Isoosmotic adjusting agent 4-70 part
Water for injection 600-1400 part
2, a kind of optimization formula of freeze dried ginseng-astragalus powder for injection to strengthen body's resistance consists of by weight:
Radix Codonopsis and Radix Astragali saponin effective kind part 2-5 part
Radix Codonopsis and astragalus polysaccharides effective kind part 2-5 part
Freeze-dried excipient 20-40 part
Isoosmotic adjusting agent 6-60 part
Water for injection 800-1200 part
Get Radix Codonopsis and Radix Astragali saponin effective kind part 1-10 part, polysaccharide effective site 1-8 part adds an amount of water for injection dissolving, add lyophilizing and use excipient 5-60 part, isoosmotic adjusting agent 4-70 part is made into 600-1400 part with water for injection, the activated carbon of adding 0.1% boiled 15 minutes, filtered, regulate pH value to 7-7.5, filter packing, sterilization, frozen drying, promptly.
The assay of total saponins in Radix Codonopsis and the Radix Astragali total saponins effective kind part
Adopt vanillin assay to measure the content of total saponins in Radix Codonopsis and the Radix Astragali saponin effective kind part.
1, it is an amount of that the astragaloside reference substance is got in the preparation of reference substance, and accurate the title decides, and adds methanol and makes the solution that every 1ml contains 0.4mg, in contrast product solution.
2, the preparation of standard curve
The accurate respectively astragaloside reference substance solution (0.4mg/ml) 0.00 of drawing, 0.10,0.20,0.30,0.40,0.50ml in tool plug test tube, methanol is flung in water-bath, the vanillin glacial acetic acid 0.2ml of accurate adding 5%, the accurate again perchloric acid 0.8ml that adds, close plug, heated at constant temperature is 20 minutes in 70 ℃ of water-baths, takes out cooling, precision adds glacial acetic acid 5.00ml, shake up, measure trap respectively, must reclaim equation C=1.54+283.20A in the 560nm place, the result shows that the astragaloside reference substance is the good linear relation in 40-200 μ part/ml scope.R＝0.9988。
3, sample determination is got Radix Codonopsis and Radix Astragali total saponins effective kind part 0.10g, and accurate the title decides, and puts in the 25ml measuring bottle, add the methanol slight fever and make dissolving, add methanol and be diluted to scale, shake up, the accurate 2ml that draws puts in the 25ml measuring bottle, adds methanol and is diluted to scale, shake up, get 0.20ml, volatilize solvent, sighting target directrix curve item is blank down from the vanillin glacial acetic acid 0.2ml operation that adds 5% with the coordinative solvent, measures absorption value, go out the content of total saponins according to regression equation calculation, the content that records total saponins is 52%.
Two, below by the comparison to functions of murine peritoneal macrophages of a kind of SHENQI FUZHENG freeze-dried powder of the present invention and SHENQI FUZHENG ZHUSHEYE, the invention will be further described.
1, experiment material and instrument
50 of Male Kunming strain mice are provided by No.1 Military Medical Univ.'s Experimental Animal Center, body weight 20～25g; The SHENQI FUZHENG freeze-dried powder, Tianzhijiao Medication Development Co., Ltd., Guangdong's laboratory provides; SHENQI FUZHENG ZHUSHEYE, Livzon Group Limin Pharmaceutical Factory production.
2, experimental technique and result
36 of mices are divided into 3 groups at random: normal saline matched group, SHENQI FUZHENG lyophilized injectable powder group, SHENQI FUZHENG ZHUSHEYE group.Every day 1 time, inferior 0.2ml/ (contained crude drug amount is suitable when SHENQI FUZHENG freeze-dried powder and the injection of SHENQI FUZHENG ZHUSHEYE two medicines), continuous ip administration 7d, behind the last administration 1d, mouse peritoneal is injected 5% chicken red blood cell 1ml, puts to death mice after 50 minutes, get peritoneal fluid and smear sheet, Wright's staining, 100 positive phagocyte of microscopy counting are calculated phagocytic index.The eyeball blood sampling, the preparation blood smear, natural drying carries out α-acetic acid naphthols esterase dyeing (ANAE) according to a conventional method, and 200 lymphocytes of microscopy counting calculate the ANAE+T lymphocyte percentage.Experimental result sees Table 1.
The influence that table 1 SHENQI FUZHENG is engulfed Turnover of Mouse Peritoneal Macrophages (x ± s, n=12)
| Group | Dosage (mg/kg) | Phagocytic index | Phagocytic percentage (%) |
| Matched group SHENQI FUZHENG freeze-dried powder SHENQI FUZHENG ZHUSHEYE | - 100 100 | 1.80±0.15 3.06±0.34** 2.42±0.52* | 40.10±5.11 88.36±5.08** 60.10±4.60** |
Compare with matched group: * P＜0.05 * * P＜0.01
A kind of SHENQI FUZHENG lyophilized injectable powder of the present invention is identical with SHENQI FUZHENG ZHUSHEYE on prescription, but on preparation technology, improve, make the SHENQI FUZHENG lyophilized injectable powder in extracting composition, add the polysaccharide composition that can strengthen human immunity, and the saponin component in the Radix Codonopsis and the Radix Astragali extracted, thereby aspect pharmacodynamics, also shown better effect.
Specific embodiment
Embodiment 1
1, prescription: Radix Codonopsis 40g Radix Astragali 40g
2, technology: get recipe quantity Radix Codonopsis, Milkvetch Root granule, add 10 times of water gagings and decoct and extract 3 times, filter, filtrate is condensed into the medicinal liquid that every 1ml is equivalent to the 1.5g crude drug, adds ethanol and makes and contain the alcohol amount and reach 70%, leaves standstill, and filters, and must precipitate and supernatant; Precipitate and use an amount of dissolved in distilled water, reuse 80% ethanol precipitation once filters, and 1% solution is made in the dissolving of precipitation adding distil water, crosses hollow fiber column ultrafilter (molecular cut off is greater than 6000), and ultrafiltrate is evaporated to dried, gets polysaccharide effective site; Supernatant behind the water extract precipitate with ethanol, decompression recycling ethanol is to there not being the alcohol flavor, adding distil water makes resolution of precipitate in right amount, filter, use n-butanol extraction three times, butanol extraction liquid merges, aqueous sodium hydroxide washes with 1% is washed secondary, discard alkaline solution, the reclaim under reduced pressure n-butyl alcohol and be concentrated into dried, Radix Codonopsis and Radix Astragali total saponins effective kind part.Get Radix Codonopsis and Radix Astragali total glycosides effective kind part 1g, polysaccharide effective site 1g adds an amount of water for injection and makes dissolving, add injection mannitol 25g, lactose 10g, sodium chloride for injection 8g, add the solution that the injection water is made into 1000ml, add 0.1% activated carbon, boiled 15 minutes, filter, regulate pH value, filter to 7-7.5, packing, sterilization, frozen drying, promptly.
Embodiment 2
2, prescription: Radix Codonopsis 40g Radix Astragali 40g
2, technology: get recipe quantity Radix Codonopsis, Milkvetch Root granule, add 10 times of water gagings and decoct and extract 3 times, filter, filtrate is condensed into the medicinal liquid that every 1ml is equivalent to the 1.5g crude drug, adds ethanol and makes and contain the alcohol amount and reach 70%, leaves standstill, and filters, and must precipitate and supernatant; Precipitate and use an amount of dissolved in distilled water, reuse 80% ethanol precipitation once filters, and 1% solution is made in the dissolving of precipitation adding distil water, crosses hollow fiber column ultrafilter (molecular cut off is greater than 6000), and ultrafiltrate is evaporated to dried, gets polysaccharide effective site; Supernatant behind the water extract precipitate with ethanol, decompression recycling ethanol is to there not being the alcohol flavor, adding distil water makes resolution of precipitate in right amount, filter, use n-butanol extraction three times, butanol extraction liquid merges, aqueous sodium hydroxide washes with 1% is washed secondary, discard alkaline solution, the reclaim under reduced pressure n-butyl alcohol and be concentrated into dried, Radix Codonopsis and Radix Astragali total saponins effective kind part.Get Radix Codonopsis and Radix Astragali total glycosides effective kind part 10g, polysaccharide effective site 8g adds an amount of water for injection and makes dissolving, add injection mannitol 25g, lactose 10g, sodium chloride for injection 8g, add the solution that the injection water is made into 1000ml, add 0.1% activated carbon, boiled 15 minutes, filter, regulate pH value, filter to 7-7.5, packing, sterilization, frozen drying, promptly.
Embodiment 3
1, side: Radix Codonopsis 40g Radix Astragali 40g
2, technology: get recipe quantity Radix Codonopsis, Milkvetch Root, be ground into coarse powder, it is moistening to add low amounts of water, the percolator of packing into, add 5 times of water gaging soaked overnight, with 50 times of water gaging percolation, collect percolate, be condensed into the medicinal liquid that every 1ml is equivalent to the 1.5g crude drug, adding ethanol makes and contains the alcohol amount and reach 70%, leave standstill, filter, must precipitate and supernatant.Precipitate and use an amount of dissolved in distilled water, reuse 80% ethanol precipitation once filters, and 1% solution is made in the dissolving of precipitation adding distil water, crosses hollow fiber column ultrafilter (molecular cut off is greater than 6000), and ultrafiltrate is evaporated to dried, gets polysaccharide effective site; Supernatant behind the water extract precipitate with ethanol, decompression recycling ethanol is to there not being the alcohol flavor, adding distil water makes resolution of precipitate in right amount, filter, use n-butanol extraction three times, butanol extraction liquid merges, aqueous sodium hydroxide washes with 1% is washed secondary, discard alkaline solution, the reclaim under reduced pressure n-butyl alcohol and be concentrated into dried, Radix Codonopsis and Radix Astragali saponin effective kind part.Get Radix Codonopsis and Radix Astragali total glycosides effective kind part 3g, polysaccharide effective site 3g adds an amount of water for injection and makes dissolving, add injection mannitol 25g, lactose 10g, glucose for injection 50g, be made into the solution of 1000ml with water for injection, add 0.1% activated carbon, boiled 15 minutes, filter, regulate pH value, filter to 7-7.5, packing, sterilization, frozen drying, promptly.
Embodiment 4
1, prescription: Radix Codonopsis 40g Radix Astragali 40g
2, technology: get recipe quantity Radix Codonopsis, Milkvetch Root, be ground into fine powder, add 15 times of water gagings dipping and extract 3 times, filter, filtrate is concentrated into the medicinal liquid that every 1ml is equivalent to the 1.5g crude drug, adds ethanol and makes and contain the alcohol amount and reach 70%, leaves standstill, and filters, and must precipitate and supernatant.Precipitate and use an amount of dissolved in distilled water, reuse 80% ethanol precipitation once filters, and 1% solution is made in the dissolving of precipitation adding distil water, crosses hollow fiber column ultrafilter (molecular cut off is greater than 6000), and ultrafiltrate is evaporated to dried, gets polysaccharide effective site; Supernatant behind the water intaking extract precipitate with ethanol, decompression recycling ethanol is to there not being the alcohol flavor, adding distil water makes resolution of precipitate in right amount, filter, with isoamyl alcohol extraction three times, the isoamyl alcohol extract merges, aqueous sodium hydroxide washes with 1% is washed secondary, discard alkaline solution, the reclaim under reduced pressure isoamyl alcohol and be concentrated into dried, Radix Codonopsis and Radix Astragali saponin effective kind part.Get Radix Codonopsis and Radix Astragali total glycosides effective kind part 4g, polysaccharide effective site 4g adds an amount of water for injection and makes dissolving, add injection mannitol 25g, lactose 10g, sodium chloride for injection 8g, be made into the solution of 1000ml with water for injection, add 0.1% activated carbon, boiled 15 minutes, filter, regulate pH value, filter to 7-7.5, packing, sterilization, frozen drying, promptly.
Claims (5)
1, a kind of method for preparing freeze dried ginseng-astragalus powder for injection to strengthen body's resistance is characterized in that:
(1) get the Radix Codonopsis and the Radix Astragali of equivalent, the active component in the Radix Codonopsis and the Radix Astragali can adopt decocting method, percolation, infusion process to extract;
(2) contain the medicinal liquid 70%-80% ethanol precipitation of effective composition behind the water extraction, filter, polysaccharide precipitation effective site and supernatant, supernatant reclaims ethanol, use the organic solvent extraction saponin constituent, must Radix Codonopsis and Radix Astragali total saponins effective kind part behind the concentrating under reduced pressure;
Prescription wherein consists of by weight: Radix Codonopsis and Radix Astragali total saponins effective kind part 1-10 part, Radix Codonopsis and astragalus polysaccharides class position 1-8 part, freeze-dried excipient 5-50 part, isoosmotic adjusting agent 4-70 part, water for injection 600-1400 part.
2, a kind of method for preparing freeze dried ginseng-astragalus powder for injection to strengthen body's resistance according to claim 1, its prescription consists of by weight: Radix Codonopsis and Radix Astragali total saponins effective kind part 3-6 part, Radix Codonopsis and astragalus polysaccharides effective kind part 2-4 part, freeze-dried excipient 20-40 part, isoosmotic adjusting agent 6-55 part, water for injection 800-1200 part.
3, preparation freeze dried ginseng-astragalus powder for injection to strengthen body's resistance method according to claim 1, organic solvent wherein is n-butyl alcohol, isoamyl alcohol.
4, preparation freeze dried ginseng-astragalus powder for injection to strengthen body's resistance method according to claim 1, freeze-dried excipient wherein are the mixture of a kind of in mannitol, the lactose or two kinds.
5, preparation freeze dried ginseng-astragalus powder for injection to strengthen body's resistance method according to claim 1, isoosmotic adjusting agent wherein is sodium chloride for injection, glucose.
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| CN 200310120040 CN1264529C (en) | 2003-12-02 | 2003-12-02 | Freeze-dried 'Shenqifuzheng' powder for injection and its preparing process |
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| CN 200310120040 CN1264529C (en) | 2003-12-02 | 2003-12-02 | Freeze-dried 'Shenqifuzheng' powder for injection and its preparing process |
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| CN1264529C true CN1264529C (en) | 2006-07-19 |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1868485B (en) * | 2005-05-24 | 2010-06-09 | 山东绿叶天然药物研究开发有限公司 | Medicine composition and its application |
| CN100417396C (en) * | 2006-03-14 | 2008-09-10 | 北京国丹药物技术开发有限公司 | Preparing method of body resistance-strengthening ginseng-astragalus injection |
| CN101084981B (en) * | 2006-06-08 | 2011-06-08 | 天津天士力之骄药业有限公司 | Medicinal preparation for cancer auxiliary treatment and its preparation method |
| CN101084980B (en) * | 2006-06-08 | 2011-10-26 | 天津天士力之骄药业有限公司 | Medicinal composition freezing-dried powder injection for cancer auxiliary treatment and its preparation method |
| CN101088520B (en) * | 2006-06-13 | 2011-10-26 | 天津天士力之骄药业有限公司 | Medicine composition for auxiliary treatment of cancer and its prepn and quality control method |
| CN1899362B (en) * | 2006-07-19 | 2010-05-12 | 丽珠集团利民制药厂 | Quality control method for shenqi injection strengthening body resistance |
| CN109939136A (en) * | 2017-12-21 | 2019-06-28 | 北京盈科瑞创新药物研究有限公司 | A kind of sucking body resistance-strengthening ginseng-astragalus pharmaceutical solutions and preparation method thereof |
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