CN1660338A - Technique for preparing 'Shenqi' of freeze drying powder for strengthening the body resistance - Google Patents
Technique for preparing 'Shenqi' of freeze drying powder for strengthening the body resistance Download PDFInfo
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Abstract
A freeze-dried powder injection of the oral liquid of ginseng and astragalus is prepared from existing oral liquid of ginseng and astragalus and excipient through prefreezing several times and drying.
Description
Technical field
The present invention relates to a kind of preparation method of SHENQI FUZHENG lyophilized injectable powder, belong to the technical field of medicament preparation.
Technical background
SHENQI FUZHENG ZHUSHEYE is a kind of Chinese medicine safely and effectively; its main component is a Radix Codonopsis; the Radix Astragali; the nature and flavor of two kinds of medicines and returning through unanimity; effect is basic identical; synergism is played in both additions, obviously heightens the effect of a treatment; has the strengthening the body resistance effect; strengthen macrophage phagocytic function simultaneously, can improve lymphocyte transformation ability and immunoglobulin, obvious antineoplastic is arranged; can help the cancer patient to finish radiotherapy smoothly; the curative effect of chemotherapeutics, the toxic and side effects of minimizing chemotherapeutics, the hemopoietic function of protection body; the effect that has the human body immunity improving function simultaneously, and can treat the heart; diseases such as cerebrovascular.But because of it is a liquid preparation, water content is higher, and stability is not good, and the main easy oxidation of effective ingredient flavone, Saponin be character such as unstable facile hydrolysis in water, is difficult for preserving, storage and transportation.Can suppress hydrolysis by adding alcohols material, improve stability, can bring untoward reaction such as pain, haemolysis but add alcohol,
Take all factors into consideration each factor, think that using Freeze Drying Technique can address the above problem, and is prepared into behind the lyophilized injectable powder owing to be solid state more satisfactoryly, water content is low, and stability strengthens greatly, and drying is carried out in a vacuum simultaneously, be difficult for oxidation, be fit to long-distance transport and long preservation.But difficult point is existing SHENQI FUZHENG ZHUSHEYE and adopts decoction and alcohol sedimentation technique prepared (Chinese patent medicine ministry standard WS-459 (Z-065)-95 and WS-387 (Z-50)-99), composition is comparatively complicated, the more complicated that balances each other of multicomponent solution, and extract compares thickness, therefore the difficult control of freeze-drying process, the time is longer.
Summary of the invention
Purpose of the present invention is exactly at the problems referred to above, and a kind of preparation method of SHENQI FUZHENG lyophilized injectable powder is provided.
Owing to can occur keeping original volume during the independent lyophilizing of this product, therefore the phenomenon of atrophy needs to add excipient.Adding not commensurability excipient in the SHENQI FUZHENG extracting solution, use the conventional method lyophilizing, is index with the complexity of freeze-drying process and the outward appearance of freeze-dried products, the suitable consumption of screening excipient, and concrete screening process is as follows:
| Excipient | Phenomenon | |
| ????1 | ????0％ | Freeze-drying process spray bottle, freeze-dried products can not molding, serious atrophy |
| ????2 | ????6％ | Freeze-drying process slightly sprays bottle, volumetric expansion |
| ????3 | ????8％ | Outward appearance is preferable, |
| ????4 | ????10％ | Freeze-drying process is more easy to control, and outward appearance is good, and is loose, uniform and smooth |
| ????5 | ????12％ | Outward appearance is preferable |
| ????7 | ????14％ | Outward appearance is slightly poor, and there is stiff shell on the surface |
Result of the test shows that the consumption of excipient is 8-14%, and optimum amount is 10%.
The excipient that the present invention adds in the SHENQI FUZHENG extracting solution is a kind of or combination in mannitol, sorbitol, dextran, lactose, the trehalose.
Excipient is preferably mannitol and trehalose, because test the glass transition temperature Tg that can improve medicinal liquid when finding these two kinds of materials as excipient.Can guarantee medicine vitrification state preferably like this, the vitrification medicine has porous network structure, and dissolution rate is fast, and the characteristics of good drug efficacy and stability are fine.Want to guarantee the vitrification state, Tg is an important parameter in the freezing dry process, and medicine is in first, second drying stage and storage process, and temperature must be lower than and the corresponding Tg of its concentration change.If surpass Tg in the first drying stage temperature, the vitrification state of the dry medicine in upper strata is destroyed, will hinder or influence the passing through of water vapour of lower floor frozen product distillation, frozen product absorbs the heat minimizing so rate of sublimation slows down, it is unnecessary that the heat of continue being supplied with by flaggy just has, cause the frozen product temperature to rise, the fusing foamed phenomenon takes place in product.If in second drying stage and storage process, ambient temperature surpasses the Tg of lyophilized formulations, and the vitrification state is destroyed, problems such as subsiding will appear in the preparation outward appearance, surperficial atrophy, caking, hardening, variable color, the loose structure of preparation is destroyed simultaneously, the water absorption variation.Therefore improve Tg, can farthest realize the medicine vitrification, shorten drying time, enlarge the allowable temperature scope that stores, increase stability.Improving the most significant embodiment of Tg is to reduce drying time, and below we test, and compares.
Wherein trehalose not only can obviously improve glass transition temperature, and organism and biomacromolecule are had non-specific protective effect.This non-specific protective effect is mainly reflected in: when biological cell is in that hunger, drying, high temperature, freezing, radiation, hyperosmosis and toxic reagent etc. are various coerces environment; Sargassum content rises rapidly in the cell, and multiple biomacromolecule is all had protective effect.Ectogenic trehalose has good nonspecific protective effect to organism and biomacromolecule equally.So excipient most preferably is trehalose.
After the SHENQI FUZHENG extracting solution that adds excipient carried out conventional treatment, put into freezer dryer and carry out lyophilization.Because this product contains polysaccharide, thickness comparatively, it is softening often to freeze piece in sublimation process, produces bubble, and forms thick structure at product surface, thereby influence sublimation drying, influence product appearance, in order to guarantee that product drying carries out smoothly, the available sublimed method of pre-freeze repeatedly makes goods top layer shell be become loose by densification, help water sublimed, also help improving Tg.We have also done battery of tests and have compared, and freeze dried repeatedly temperature range is chosen in-45～-24 ℃.
| Distinct methods | Drying time (h) | Outward appearance | |
| ????1 | Do not add excipient, the conventional method lyophilizing | ????22 | Freeze-dried products can not molding, serious atrophy |
| ????2 | Add usual excipients, the conventional method lyophilizing | ????19 | Outward appearance is preferable |
| ????3 | With mannitol, the conventional method lyophilizing | ????16 | Freeze-drying process is more easy to control, and outward appearance is good, and is loose, uniform and smooth |
| ????4 | With trehalose, the conventional method lyophilizing | ????14 | Freeze-drying process is more easy to control, and outward appearance is good, and is loose, uniform and smooth |
| ????5 | With mannitol, pre-freeze repeatedly | ????10 | Freeze-drying process is more easy to control, and outward appearance is good, and is loose, uniform and smooth |
| ????6 | With trehalose, pre-freeze repeatedly | ????8 | Freeze-drying process is more easy to control, and outward appearance is good, and is loose, uniform and smooth |
Complete preparation technology of the present invention is as follows: Radix Codonopsis, the Radix Astragali are put in the decoction device, and it is an amount of to add water, decocts twice, collecting decoction, filter, filtrate being concentrated into contains crude drug 5.0g/ml, adds ethanol then, leaves standstill 24 hours, filter, behind the recovery ethanol, add ethanol again, left standstill 24 hours, filter, reclaim ethanol, add ethanol again, left standstill 24 hours, filter, reclaim ethanol to there not being the alcohol flavor, adding distil water to 1000 milliliter adds active carbon, pH value is regulated in heating, filtration, and is stand-by.Get excipient and be dissolved in the proper amount of water for injection, stir and make dissolving fully, with above-mentioned solution mixing, add the injection water to 5000ml, extremely clear and bright through the membrane filtration degerming, behind mensuration pH value and the content, fill is in cillin bottle, place in the freeze dryer, enter drying stage after the pre-freeze repeatedly, after the drying, jump a queue, gland, check, packing, warehouse-in.
The SHENQI FUZHENG lyophilized powder that utilizes preparation technology of the present invention to make, drying time is short, good reproducibility, outward appearance is good, and is loose, and the uniform and smooth conformance with standard is carried out clarity test, loading quantity inspection, sterility test result and is all met standards of pharmacopoeia.
Specific embodiments
Embodiment 1
With Radix Codonopsis, the Radix Astragali is put and is decocted in the device, and it is an amount of to add water, decocts twice, 2 hours for the first time, 1.5 hours for the second time, collecting decoction, filter, filtrate being concentrated into contains crude drug 5.0g/ml, and adding ethanol then is 60% to containing the alcohol amount, left standstill 24 hours, and filtered, behind the recovery ethanol, adding ethanol again is 70% to containing the alcohol amount, leaves standstill 24 hours, filters, reclaim ethanol, adding ethanol again is 80% to containing the alcohol amount, leaves standstill 24 hours, filter, reclaim ethanol to there not being the alcohol flavor, adding distil water to 1000 milliliter adds 1% active carbon, 100 ℃ were heated 30 minutes down, filter, regulate pH value with sodium hydroxide solution and be 7.0, stand-by.Getting 500g mannitol is dissolved in the proper amount of water for injection, stirring makes dissolving fully, with above-mentioned solution mixing, add the injection water to 5000ml, extremely clear and bright through 0.45 μ m microporous filter membrane fine straining and 0.22 μ m filtering with microporous membrane degerming, behind mensuration pH value and the content, fill is in cillin bottle, place in the freeze dryer,-45 ℃ of pre-freezes 1 hour are warming up to-24 ℃ and keep reducing to-45 ℃ after 0.5 hour, enter first drying stage after several times repeatedly, be warming up to 30 ℃ in 10 hours, keep after 4 hours, jump a queue, gland, check, packing, warehouse-in.
Embodiment 2
With Radix Codonopsis, the Radix Astragali is put and is decocted in the device, and it is an amount of to add water, decocts twice, 2 hours for the first time, 1.5 hours for the second time, collecting decoction, filter, filtrate being concentrated into contains crude drug 5.0g/ml, and adding ethanol then is 60% to containing the alcohol amount, left standstill 24 hours, and filtered, behind the recovery ethanol, adding ethanol again is 70% to containing the alcohol amount, leaves standstill 24 hours, filters, reclaim ethanol, adding ethanol again is 80% to containing the alcohol amount, leaves standstill 24 hours, filter, reclaim ethanol to there not being the alcohol flavor, adding distil water to 1000 milliliter adds 1% active carbon, 100 ℃ were heated 30 minutes down, filter, regulate pH value with sodium hydroxide solution and be 7.0, stand-by.Getting the 400g trehalose is dissolved in the proper amount of water for injection, stirring makes dissolving fully, with above-mentioned solution mixing, add the injection water to 5000ml, extremely clear and bright through 0.45 μ m microporous filter membrane fine straining and 0.22 μ m filtering with microporous membrane degerming, behind mensuration pH value and the content, fill is in cillin bottle, place in the freeze dryer,-45 ℃ of pre-freezes 1 hour are warming up to-24 ℃ and keep reducing to-45 ℃ after 0.5 hour, enter first drying stage after several times repeatedly, be warming up to 30 ℃ in 8 hours, keep after 4 hours, jump a queue, gland, check, packing, warehouse-in.
Embodiment 3
With Radix Codonopsis, the Radix Astragali is put and is decocted in the device, and it is an amount of to add water, decocts twice, 2 hours for the first time, 1.5 hours for the second time, collecting decoction, filter, filtrate being concentrated into contains crude drug 5.0g/ml, and adding ethanol then is 60% to containing the alcohol amount, left standstill 24 hours, and filtered, behind the recovery ethanol, adding ethanol again is 70% to containing the alcohol amount, leaves standstill 24 hours, filters, reclaim ethanol, adding ethanol again is 80% to containing the alcohol amount, leaves standstill 24 hours, filter, reclaim ethanol to there not being the alcohol flavor, adding distil water to 1000 milliliter adds 1% active carbon, 100 ℃ were heated 30 minutes down, filter, regulate pH value with sodium hydroxide solution and be 7.0, stand-by.Getting the 600g lactose is dissolved in the proper amount of water for injection, stirring makes dissolving fully, with above-mentioned solution mixing, add the injection water to 5000ml, extremely clear and bright through 0.45 μ m microporous filter membrane fine straining and 0.22 μ m filtering with microporous membrane degerming, behind mensuration pH value and the content, fill is in cillin bottle, place in the freeze dryer,-45 ℃ of pre-freezes 1 hour are warming up to-24 ℃ and keep reducing to-45 ℃ after 0.5 hour, enter first drying stage after several times repeatedly, be warming up to 30 ℃ in 8 hours, keep after 4 hours, jump a queue, gland, check, packing, warehouse-in.
Although described the present invention by specific embodiment, some is revised and equivalence is obvious for the technical staff who is proficient in this field, and these variations are believed to comprise within the scope of the present invention.
Claims (7)
1. the preparation method of a SHENQI FUZHENG lyophilized injectable powder is included in the excipient that adds 8-14% in the SHENQI FUZHENG extracting solution, puts and carries out pre-freeze, drying in the freeze dryer.
2. preparation method as claimed in claim 1 is characterized in that the excipient addition is 10%.
3. preparation method as claimed in claim 1 is characterized in that excipient is a kind of or combination in mannitol, sorbitol, dextran, lactose, the trehalose.
4. preparation method as claimed in claim 1 is characterized in that excipient is mannitol, trehalose.
5. preparation method as claimed in claim 1 is characterized in that excipient is a trehalose.
6. preparation method as claimed in claim 1 is characterized in that pre-freeze adopts pre-freeze method repeatedly.
7. pre-freeze repeatedly as claimed in claim 6 is characterized in that repeatedly that the temperature range of pre-freeze is-45～-24 ℃.
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| CN 200510000114 CN1660338A (en) | 2005-01-04 | 2005-01-04 | Technique for preparing 'Shenqi' of freeze drying powder for strengthening the body resistance |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108066290A (en) * | 2017-12-31 | 2018-05-25 | 北京佑众全椒制药有限公司 | A kind of method that vacuum foam technique prepares licorice polysaccharide freeze-dried powder |
| CN108078932A (en) * | 2017-12-31 | 2018-05-29 | 北京佑众全椒制药有限公司 | A kind of processing method of licorice polysaccharide freeze-dried powder |
| CN114949031A (en) * | 2021-02-26 | 2022-08-30 | 湖州新活医疗科技有限公司 | Traditional Chinese medicine composition for improving spleen and stomach functions and enhancing immunity and application |
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2005
- 2005-01-04 CN CN 200510000114 patent/CN1660338A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108066290A (en) * | 2017-12-31 | 2018-05-25 | 北京佑众全椒制药有限公司 | A kind of method that vacuum foam technique prepares licorice polysaccharide freeze-dried powder |
| CN108078932A (en) * | 2017-12-31 | 2018-05-29 | 北京佑众全椒制药有限公司 | A kind of processing method of licorice polysaccharide freeze-dried powder |
| CN114949031A (en) * | 2021-02-26 | 2022-08-30 | 湖州新活医疗科技有限公司 | Traditional Chinese medicine composition for improving spleen and stomach functions and enhancing immunity and application |
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