CN108066290A - A kind of method that vacuum foam technique prepares licorice polysaccharide freeze-dried powder - Google Patents

A kind of method that vacuum foam technique prepares licorice polysaccharide freeze-dried powder Download PDF

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Publication number
CN108066290A
CN108066290A CN201711495220.6A CN201711495220A CN108066290A CN 108066290 A CN108066290 A CN 108066290A CN 201711495220 A CN201711495220 A CN 201711495220A CN 108066290 A CN108066290 A CN 108066290A
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CN
China
Prior art keywords
dried powder
licorice polysaccharide
freeze
vacuum foam
polysaccharide freeze
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Legal status (The legal status 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 status listed.)
Pending
Application number
CN201711495220.6A
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Chinese (zh)
Inventor
陈�光
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Beijing Zhong Yu Quanjiao Pharmaceutical Co Ltd
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Beijing Zhong Yu Quanjiao Pharmaceutical Co Ltd
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Priority to CN201711495220.6A priority Critical patent/CN108066290A/en
Publication of CN108066290A publication Critical patent/CN108066290A/en
Pending legal-status Critical Current

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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/14Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
    • A61K9/19Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles lyophilised, i.e. freeze-dried, solutions or dispersions
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K31/00Medicinal preparations containing organic active ingredients
    • A61K31/70Carbohydrates; Sugars; Derivatives thereof
    • A61K31/715Polysaccharides, i.e. having more than five saccharide radicals attached to each other by glycosidic linkages; Derivatives thereof, e.g. ethers, esters
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/06Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite
    • A61K47/16Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite containing nitrogen, e.g. nitro-, nitroso-, azo-compounds, nitriles, cyanates
    • A61K47/18Amines; Amides; Ureas; Quaternary ammonium compounds; Amino acids; Oligopeptides having up to five amino acids
    • A61K47/183Amino acids, e.g. glycine, EDTA or aspartame
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/06Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite
    • A61K47/26Carbohydrates, e.g. sugar alcohols, amino sugars, nucleic acids, mono-, di- or oligo-saccharides; Derivatives thereof, e.g. polysorbates, sorbitan fatty acid esters or glycyrrhizin

Abstract

The present invention proposes a kind of method that vacuum foam technique prepares licorice polysaccharide freeze-dried powder, includes the following steps:Licorice polysaccharide, excipient, foaming agent are added in sterile chamber, water for injection is added in, stirs evenly, adds in PH buffer solutions, mixed solution is made;Licorice polysaccharide freeze-dried powder is made through the pre-freeze that cools down, vacuum foam and heating drying process in mixed solution.The obtained licorice polysaccharide freeze-dried powder of the present invention has the advantages that water content is low, multiple dissolubility is good, form is loose and is easy to preservation for a long time, and preparation method is easy, and cost is relatively low.

Description

A kind of method that vacuum foam technique prepares licorice polysaccharide freeze-dried powder
Technical field
The present invention relates to freeze-dried powder preparing technical fields more particularly to a kind of vacuum foam technique to prepare licorice polysaccharide and freeze The method of powder.
Background technology
Radix Glycyrrhizae as a kind of traditional Chinese medicine, just has the good reputation of " ten sides, nine grass ", the main active of Radix Glycyrrhizae since ancient times There are glycyrrhizic acid, licoflavone and licorice polysaccharide, the above two, which have had, compares in-depth study, and the application and development side of licorice polysaccharide Face research is seldom.
Licorice polysaccharide is the reductive polysacchride based on α-glucosides, and ivory buff powder can be dissolved in water, mainly by grape Sugar, galactolipin and arabinose composition.Research shows that licorice polysaccharide has immunological regulation, antiviral, antitumor and raising body The effect of oxidation resistance.Licorice polysaccharide is a kind of immunomodulator, and energy immune cell activated promotes reticuloendothelial system phagocytic Function improves the activity of anticomplement, and while body's immunity is improved, normal cell nonhazardous is acted on;Licorice polysaccharide Anti-virus formulation can be used as, influences the formation of viral plasomidum, there is certain inhibitory action to ox AIDS virus (BIV), Inhibiting rate is 36.2%;There is apparent inhibit with directly inactivating to III type of adenovirus (AdV III) and Coxsackie virus (CBV3) Effect is infected available for virus is treated and prevented;Oxygen radical is the by-product of aerobe cell eubolism, and a small amount of oxygen is certainly It is necessary to sustaining life by base, but excessive oxygen radical can cause disease, and licorice polysaccharide has certain antioxidation activity, Free radical excessive in vivo can be removed, improves Antioxidative Defense System, antioxidation is played, so as to prevent oxidative damage.
Chinese patent CN1473571A proposes a kind of licorice polysaccharide new medical use and its pharmaceutical preparation, by licorice polysaccharide, Excipient and other component drugs are through mixing, through dry obtained licorice polysaccharide tablet, capsule, granule, suspension, dripping pill, mouth Liquid, aerosol, injection are taken, has and replenishes qi to invigorate the spleen, body's immunity can be enhanced, cure mainly chronic and recurrent respiratory infections It is evident in efficacy, the characteristics of toxic side effect is small, but the water content of licorice polysaccharide medicine product is high, multiple dissolubility is poor, and shelf lives are short.
The content of the invention
Technical problems based on background technology, the present invention propose a kind of vacuum foam technique and prepare licorice polysaccharide jelly Licorice polysaccharide freeze-dried powder is made with water content is low, multiple dissolubility is good, form is loose and is easy to preserve for a long time excellent in the method for dry powder Point, preparation method is easy, and cost is relatively low.
The present invention proposes a kind of method that vacuum foam technique prepares licorice polysaccharide freeze-dried powder, includes the following steps:
S1, licorice polysaccharide, excipient, foaming agent are added in sterile chamber, adds in water for injection, be stirring evenly and then adding into The mixed solution that PH is 7.0~8.0 is made in PH buffer solutions;
S2, mixed solution is cooled to -28~-38 DEG C from room temperature, is evacuated to -400~-550mmHg foaming, keeps 1 ~2h is warming up to -16~-20 DEG C, keeps 1~2h, is warming up to 25~35 DEG C, keeps 1~2h, and licorice polysaccharide freeze-dried powder is made.
Preferably, licorice polysaccharide, excipient and blowing agent composition weight ratio are 25~50 in S1:74~89:1~2.
Preferably, excipient is amino acid, mannitol, polyethylene glycol, glucose, sodium chloride, citrate, phosphoric acid in S1 One or more in salt.
Preferably, foaming agent is the one or more in F108 foaming agents, F87 foaming agents and F68 foaming agents in S1.
Preferably, in S1 pH value buffer solution be ammonium hydroxide, sodium carbonate, sodium acid carbonate, the one or more in sodium acetate.
Preferably, rate of temperature fall is 0.3-0.8 DEG C/min in S2, and heating rate is 0.1-0.3 DEG C/min.
Preferably, the water content of licorice polysaccharide freeze-dried powder is less than 5% in S2.
Licorice polysaccharide freeze-dried powder is made through vacuum foam and drying process with licorice polysaccharide cooperation excipient in the present invention, foams Agent can make licorice polysaccharide and excipient be expanded to foam-like in vacuum, significantly increase specific surface area, improve heat transfer effect Rate, so as to which rate of drying be greatly improved;Excipient is a kind of good cosolvent of licorice polysaccharide and leavening agent, and Radix Glycyrrhizae can be made more Sugared freeze-dried powder forms full and bulk skeleton, and it is good to improve multiple dissolubility;Foaming agent can promote tax of the excipient to licorice polysaccharide Shape acts on, and excipient is amino acid and polyalcohols, is conducive to the stabilization of foam, and the two has good synergistic effect.The present invention Faster vacuum refrigeration cooling rate and relatively slow heating rate of drying are controlled, is conducive to improve rate of drying, reduces licorice polysaccharide Middle active ingredient loss is few, and the multiple dissolubility of obtained licorice polysaccharide freeze-dried powder is good, and water content is low, and retention cycle is long, present invention system Preparation Method is simple, and cost is relatively low, and application prospect is wide.
Specific embodiment
In the following, technical scheme is described in detail by specific embodiment.
Embodiment 1
A kind of method that vacuum foam technique prepares licorice polysaccharide freeze-dried powder, includes the following steps:
S1,25 parts of licorice polysaccharides, 39 parts of amino acid, 50 portions of mannitol, 1 part of F87 foaming agent are added in by weight it is sterile In container, water for injection is added in, is stirring evenly and then adding into sodium acetate, the mixed solution that PH is 7.0 is made;
S2, mixed solution is cooled to -28 DEG C from room temperature with the rate of 0.3 DEG C/min, is evacuated to -400mmHg foaming, 1h is kept, -16 DEG C is warming up to the rate of 0.1 DEG C/min, keeps 1h, be warming up to 25 DEG C, keep 1h, it is 4% that water content, which is made, Licorice polysaccharide freeze-dried powder.
Embodiment 2
A kind of method that vacuum foam technique prepares licorice polysaccharide freeze-dried powder, includes the following steps:
S1,50 parts of licorice polysaccharides, 34 parts of polyethylene glycol, 40 parts of glucose, 2 parts of F108 foaming agents are added in into nothing by weight In bacterium container, water for injection is added in, is stirring evenly and then adding into ammonium hydroxide, the mixed solution that PH is 8.0 is made;
S2, mixed solution is cooled to -38 DEG C from room temperature with the rate of 0.8 DEG C/min, is evacuated to -550mmHg foaming, 2h is kept, the rate of 0.3 DEG C/min is warming up to -20 DEG C, keeps 2h, is warming up to 35 DEG C, keeps 2h, it is sweet for 1% that water content is made Grass polysaccharide freeze-dried powder.
Embodiment 3
A kind of method that vacuum foam technique prepares licorice polysaccharide freeze-dried powder, includes the following steps:
S1, by weight by 30 parts of licorice polysaccharides, 25 parts of amino acid, 25 portions of mannitol, 15 parts of polyethylene glycol, 15 portions of grapes Sugar, 2 parts of F68 foaming agents are added in sterile chamber, are added in water for injection, are stirring evenly and then adding into sodium acid carbonate, and it is 7.3 that PH, which is made, Mixed solution;
S2, mixed solution is cooled to -32 DEG C from room temperature with the rate of 0.4 DEG C/min, is evacuated to -450mmHg foaming, 1.3h is kept, the rate of 0.1 DEG C/min is warming up to -18 DEG C, keeps 1.3h, is warming up to 27 DEG C, keeps 1.3h, obtained water content is 2% licorice polysaccharide freeze-dried powder.
Embodiment 4
A kind of method that vacuum foam technique prepares licorice polysaccharide freeze-dried powder, includes the following steps:
S1, by weight by 40 parts of licorice polysaccharides, 18 parts of amino acid, 42 portions of mannitol, 15 parts of polyethylene glycol, 10 portions of grapes Sugar, 3 parts of sodium chloride, 1 part of F68 foaming agent are added in sterile chamber, are added in water for injection, are stirring evenly and then adding into sodium carbonate, make Obtain the mixed solution that PH is 7.6;
S2, the rate of 0.4 DEG C/min of mixed solution is cooled to -34 DEG C from room temperature, is evacuated to -500mmHg foaming, protects 1.7h is held, the rate of 0.2 DEG C/min is warming up to -19 DEG C, keeps 1.6h, is warming up to 32 DEG C, keeps 1.7h, obtained water content is 3% licorice polysaccharide freeze-dried powder.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto, Any one skilled in the art in the technical scope disclosed by the present invention, technique according to the invention scheme and its Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.

Claims (7)

1. a kind of method that vacuum foam technique prepares licorice polysaccharide freeze-dried powder, which is characterized in that include the following steps:
S1, licorice polysaccharide, excipient, foaming agent are added in sterile chamber, adds in water for injection, be stirring evenly and then adding into PH and delay The mixed solution that PH is 7.0~8.0 is made in fliud flushing;
S2, mixed solution is cooled to -28~-38 DEG C, is evacuated to -400~-550mmHg foaming, keep 1~2h, heating To -16~-20 DEG C, 1~2h is kept, is warming up to 25~35 DEG C, keeps 1~2h, licorice polysaccharide freeze-dried powder is made.
2. the method that vacuum foam technique prepares licorice polysaccharide freeze-dried powder according to claim 1, which is characterized in that sweet in S1 The weight ratio of grass polysaccharide, excipient and foaming agent is 25~50:74~89:1~2.
3. the method that vacuum foam technique according to claim 1 or claim 2 prepares licorice polysaccharide freeze-dried powder, which is characterized in that S1 Middle excipient is amino acid, the one or more in mannitol, polyethylene glycol, glucose, sodium chloride, citrate, phosphate.
4. according to the method that any one of the claim 1-3 vacuum foam techniques prepare licorice polysaccharide freeze-dried powder, feature exists In foaming agent is the one or more in F108 foaming agents, F87 foaming agents and F68 foaming agents in S1.
5. according to the method that any one of the claim 1-4 vacuum foam method techniques prepare licorice polysaccharide freeze-dried powder, feature It is, pH value buffer solution is the one or more in ammonium hydroxide, sodium carbonate, sodium acid carbonate, sodium acetate in S1.
6. according to the method that any one of the claim 1-5 vacuum foam techniques prepare licorice polysaccharide freeze-dried powder, feature exists In rate of temperature fall is 0.3-0.8 DEG C/min in S2, and heating rate is 0.1-0.3 DEG C/min.
7. according to the method that any one of the claim 1-6 vacuum foam techniques prepare licorice polysaccharide freeze-dried powder, feature exists In the water content of licorice polysaccharide freeze-dried powder is less than 5% in S2.
CN201711495220.6A 2017-12-31 2017-12-31 A kind of method that vacuum foam technique prepares licorice polysaccharide freeze-dried powder Pending CN108066290A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1473571A (en) * 2003-08-01 2004-02-11 天津市贝特科技发展有限公司 New medicinal use of liquorice polysaccharide and its medicinal preparation
CN1660338A (en) * 2005-01-04 2005-08-31 北京瑞伊人科技发展有限公司 Technique for preparing 'Shenqi' of freeze drying powder for strengthening the body resistance
CN101292982A (en) * 2007-04-25 2008-10-29 广州名冠医药科技有限公司 Enoxacin freeze-dried powder needle composing prescription and preparation technique
CN106137979A (en) * 2015-03-31 2016-11-23 深圳翰宇药业股份有限公司 A kind of lyophilized injectable powder and preparation method thereof
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

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1473571A (en) * 2003-08-01 2004-02-11 天津市贝特科技发展有限公司 New medicinal use of liquorice polysaccharide and its medicinal preparation
CN1660338A (en) * 2005-01-04 2005-08-31 北京瑞伊人科技发展有限公司 Technique for preparing 'Shenqi' of freeze drying powder for strengthening the body resistance
CN101292982A (en) * 2007-04-25 2008-10-29 广州名冠医药科技有限公司 Enoxacin freeze-dried powder needle composing prescription and preparation technique
CN106137979A (en) * 2015-03-31 2016-11-23 深圳翰宇药业股份有限公司 A kind of lyophilized injectable powder and preparation method thereof
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

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张绍志等: "泡沫真空冷冻干燥的实验研究", 《真空》 *
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