CN101306017A - Hyper-concentrated placenta lipopolysaccharide freeze-drying capsules and its preparation method - Google Patents
Hyper-concentrated placenta lipopolysaccharide freeze-drying capsules and its preparation method Download PDFInfo
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- CN101306017A CN101306017A CNA2007101079114A CN200710107911A CN101306017A CN 101306017 A CN101306017 A CN 101306017A CN A2007101079114 A CNA2007101079114 A CN A2007101079114A CN 200710107911 A CN200710107911 A CN 200710107911A CN 101306017 A CN101306017 A CN 101306017A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
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Abstract
The invention relates to a manufacture method of a hyperconcentration placental lipopolysaccharide freeze-dried capsule, which comprises the steps as follows: (a) placental lipopolysaccharide stock solution is processed through the CO2 supercritical fluid extraction to obtain placental peptide extracts; (b) biological enzyme is utilized to process the placental peptide extracts, and molecular weight is reduced to below 6000 daltons; (c) small molecule extracts which are obtained in the step (b) are processed through freeze drying, so as to obtain freeze-dried powder; and (d) the freeze-dried powder is manufactured into the hyperconcentration placental lipopolysaccharide freeze-dried capsule by adopting the lipidosome preparation method. The invention also provides a capsule which is manufactured by the manufacture method. The capsule and the manufacture method eliminate the problem of inconvenient use and carrying in the prior injection products.
Description
Technical field
The present invention relates to a kind of method that contains the health product of Placenta extract polysaccharide and prepare these health product.
Background technology
Placenta Hominis Chinese medicine is called Placenta Hominis, have regulate function of human body, build up resistance, the effect of strongly invigorating primordial QI essence and blood.Placenta extract is the medicinal ingredient that extracts from Placenta Hominis, contains multiple hormone and enzyme.The spissated method of steaming and decocting is adopted in the extraction of Placenta extract in the past more.The inventor is by research, a kind of method of utilizing carbon dioxide supercritical fluid extraction to extract Placenta extract is provided, see also Chinese patent 200410096974.0, the active component that the Placenta extract that utilizes this method to extract has in the Placenta extract that is extracted can not run off, and the Placenta extract in the Placenta Hominis extracts advantage more completely.
The Placenta extract that the inventor once will utilize carbon dioxide supercritical extraction method to extract has been made injection, injection is painful, application risk is higher to being brought by the injection people but the injection product has, the shortcoming of being inconvenient to carry, and some the active gene regulatory factors and the part metabolic regulation enzyme that utilized digesting technoloy method acquisition Placenta extract to have in the Placenta Hominis originally can be because of the shortcomings of high temperature action inactivation.Therefore, for providing a kind of being more convenient for to use, injection is not painful, application risk is low, is convenient for carrying, and can fully keeps the Placenta extract product of active gene regulatory factor and metabolic regulation enzyme to have extensively and exigence.
In addition, utilize Co 2 supercritical fluid low-temperature extraction technology (SFE) though on the extraction separation level of Placenta extract, obtained than quantum jump, use the composition of the Placenta Hominis of this technology extraction to improve more than 1100 times than traditional handicraft, and its molecular weight that extracts composition is littler than traditional method, be more conducive to absorption of human body, and this technology great advantage is can be almost 100% to keep the physiologically active that extracts composition.But, utilize the Placenta extract of SFE technology " active extract " also to exist the molecular weight of product not enough little, the Placenta extract nucleus that human body finally absorbs fusion does not still reach the problem of very high level.
Summary of the invention
Therefore, at the still bigger problem of molecular weight of the Placenta extract that utilizes the SFE technology to extract at present, the inventor provides a kind of hyper-concentrated placenta lipopolysaccharide freeze-drying capsules preparation that utilizes biological enzyme technology to extract.
The molecular weight of the effective ingredient of hyper-concentrated placenta lipopolysaccharide freeze-drying capsules provided by the invention reaches 6000 dalton, preferably reaches below 4000 dalton.
The present invention also provides the production method of hyper-concentrated placenta lipopolysaccharide freeze-drying capsules, may further comprise the steps:
A) with placental lipo-glucosaminoglycan stock solution process co_2 supercritical fluid extraction, obtain the Placenta extract extract;
B utilizes enzyme to handle described Placenta extract extract, and molecular weight is reduced to below 6000 dalton;
C) with the micromolecule extract lyophilization that obtains in the step b), obtain lyophilized powder; And
D) adopt method for preparing lipidosome that described lyophilized powder is made hyper-concentrated placenta lipopolysaccharide freeze-drying capsules.
The main component of Placenta extract polyoses factor provided by the invention comprises placental lipo-glucosaminoglycan, placental nucleic acid, and more than 8000 kind of rich primitive life material of Placenta Hominis.
The Placenta Hominis polyoses factor capsule that is made by the present invention also has following advantage:
1. can extract the 8000 various active materials that Placenta Hominis is rich in more, extraction ratio can be up to 99.999% (being the highest purity of present Orally taken product).
2. but its molecular weight purifies and separates of extracting the Placenta Hominis active ingredient is to minimum 4000 dalton;
3. effect is not worse than the Placenta extract injection: level of activity and activity substance content are near the Placenta extract injection, and effects such as its beauty treatment, health care, skin protection, treatment disease are also near the Placenta extract injection.Experimental results show that: the beautifying and anti-aging effect of about 1 bottle of hyper-concentrated placenta lipopolysaccharide freeze-drying capsules is equivalent to the Placenta extract injection of 2 same dosage.
4. experimental results show that: the level of activity of the Placenta Hominis composition of its extraction can than the 4th generation the Placenta extract product improve about 67.73%.
The specific embodiment
Usually, the production method of hyper-concentrated placenta lipopolysaccharide freeze-drying capsules provided by the invention may further comprise the steps:
A) with placental lipo-glucosaminoglycan stock solution process co_2 supercritical fluid extraction, obtain the Placenta extract extract;
B) utilize enzyme to handle described Placenta extract extract, molecular weight is reduced to below 6000 dalton;
C) with the micromolecule extract lyophilization that obtains in the step b), obtain lyophilized powder; And
D) adopt method for preparing lipidosome that described lyophilized powder is made hyper-concentrated placenta lipopolysaccharide freeze-drying capsules.
Characteristics of the present invention are that the placental lipo-glucosaminoglycan stock solution that market can get is carried out supercritical carbon dioxide extraction.This step is to carry out under the pressure at 30～40Mpa, 30～40 ℃ the temperature conditions, and the extraction time is generally 8～12h.Carry out two-stage decompression separation then through the one-level decompression separation, adopt the operating pressure of 8～12Mpa and 6Mpa respectively, and the operative temperature of 30～35 ℃ and 15～25 ℃.Obtain the Placenta extract extract.
Of the present invention another specificly be, adopts enzyme to handle described Placenta extract extract, so that molecular weight is reduced to the scope that helps absorption of human body.In one embodiment, utilize restricted or half restricted enzyme under 30～40 ℃ to Placenta extract in the nucleic acid or the polysaccharide of macromolecule carry out the reaction of Restriction Enzyme inscribe.Described restricted enzyme is Mmel, TCCRAC (20/18); Eco57I, CTGAAG (16/14); Eco57MI, CTGRAG (16/14); Or Bce83I, CTTGAG (16/14).
In actual production, preferably at above-mentioned steps b) back introduces ultrafiltration step,, with the ultrafilter membrane of preset aperture the treatment fluid of gained carried out ultrafiltration that is.In one embodiment of the invention, the molecular cut off of having selected for use U.S. millipore company to produce is 6000 daltonian ultrafilter membranes, so that the molecular weight of the effective ingredient of products obtained therefrom reaches below 6000; In another embodiment of the present invention, the molecular cut off of having selected for use U.S. millipore company to produce is 6000 daltonian ultrafilter membranes, so that the molecular weight of the effective ingredient of products obtained therefrom reaches below 6000.The control of this effective ingredient molecular weight benefits to the performance of product, because micromolecular Placenta extract more helps absorption by human body.In this case, correspondingly repeat INT step and ultrafiltration step, to improve the yield of active component.In the present invention, above-mentioned two steps can be repeated 3 to 4 times, almost to reach the active component below 6000 dalton very; If above-mentioned two steps are repeated 7 to 9 times, then can very obtain the following active component of 4000 dalton.
In the present invention, it is useful adopting freeze-drying that the extract of gained is carried out drying, because it can keep the activity of these biological active substanceies in good condition, especially keeps the activity of heat-sensitive substance.This lyophilization is known at food and pharmaceutical field, promptly under low temperature (normally-60～-10 ℃) and fine vacuum (for example 6.67～40Pa) with material or solution in the drying means that directly distils of moisture content.In operation, at first exsiccant medicinal liquid is packed in bottle or the square position, place drying baker then, for example be cooled to-50～-40 ℃ and carry out pre-freeze, medicinal liquid or material are freezed, then open vacuum pump, make drying baker internal drop to 6.67～40Pa.Meanwhile, the temperature in the drying baker that suitably raises makes water accelerate distillation.The selection that it should be noted that vacuum will be depended on the temperature that drying baker is interior.For example, in the time of-30 ℃, the vapour pressure of water is 38.12Pa, should with vacuum degree control this vapour pressure 1/4～1/2 between, promptly between 9.33～18.63Pa.
Further advantage of the present invention also is to use liposome to prepare hyper-concentrated placenta lipopolysaccharide freeze-drying capsules, rather than adopts other carriers.Liposome is very suitable for the carrier as polyoses capsule of the present invention because of it has nontoxic, stabilizing active, slow release, advantage long-acting and targeting.Be suitable for very much oral formulations for the liposome form.
The method for preparing liposome has multiple, comprises membrane process, multi-emulsion method, centrifuging, calcium fusion method, injection method, pH gradient method and prerequisite liposome method.These methods all are applicable to the production of polyoses capsule of the present invention.The detailed content of these methods is referring to microcapsule technology-principle and application, people such as Xu Shiying, and Chemical Industry Press, 2006, pp91～124 were incorporated herein by reference in this content with its disclosure.
Preferred precursor liposome method of the present invention is used for the production of hyper-concentrated placenta lipopolysaccharide freeze-drying capsules, and that the pro-liposome method has is with low cost, mild condition, the heat-sensitive substance that also is applicable to simultaneously easy and simple to handle.The prerequisite liposome method comprises spray drying method, freeze-drying, Film forming method and boulton process.This several method all is applicable to the present invention, but preferred film sedimentation and freeze-drying.Because its technology is simple, and is easy to operate, be suitable for suitability for industrialized production, the pro-liposome good stability that makes.Its concrete technology comprises:
The preparation lipid soln takes by weighing an amount of phospholipid, cholesterol and dispersant, and it is standby to be dissolved into lipid soln with a certain amount of chloroform or dichloromethane;
Core with get an amount of carrier (as mannitol, glucose, sorbitol, trehalose or sucrose) and core mixing of carrier, with carrier and the abundant mix homogeneously of core, put into the coating pan of rotation;
Seal core and preparing carriers pro-liposome, lipid soln repeatedly is sprayed on the mixture of the carrier that rolling and medicine on a small quantity with aerosol apparatus.30 ℃ of hot blast heating are treated to spray after the organic solvent volatilization again, until lipid soln has been sprayed, obtain the prerequisite liposome, can use immediately.Face with before adding the water hydration, liposome.
Can be used as capsule coating of the present invention is selected from by polyvinyl alcohol, modification of chitosan, gelatin, sodium alginate, hydroxypropyl cellulose, methylcellulose, hydroxypropyl emthylcellulose, hydroxyethyl-cellulose, polyvinylpyrrolidone, polyvinylpyrrolidone-vinyl acetate copolymer, polyvinyl acetal-lignocaine acetate copolymer, diethyllaminoethyl acrylic acid methyl ester .-methylmethacrylate copolymer, cellulose acetate-phthalate, Hydroxypropyl Methylcellulose Phathalate, the hexahydrophthalic acid cellulose acetate, the hexahydrophthalic acid hydroxypropyl emthylcellulose, polymethyl acrylate, polyethyl acrylate, butyl polyacrylate, polymethyl methacrylate, polyethyl methacrylate, butyl polyacrylate, Poly(Hydroxyethyl Methacrylate), poly hydroxy ethyl acrylate, the polyacrylic acid hydroxypropyl acrylate, the polymethylacrylic acid hydroxypropyl acrylate, polyacrylic acid 4-hydroxy butyl ester, polymethylacrylic acid 4-hydroxy butyl ester, and in the group of copolymer or admixture formation.
In a specific embodiment,, capsule coating of the present invention is a gastric solubility.
And in another specific embodiment, capsule coating of the present invention is an enteric solubility
Further describe the present invention with embodiment below, help better understanding, be used for restriction but described embodiment only is used to illustrate the present invention to the present invention and advantage thereof.
Embodiment 1
Placental lipo-glucosaminoglycan stock solution is put into extraction kettle, feed the carbon dioxide of 30～40Mpa, under 30～40 ℃ of conditions, extract 8～12h; Through the one-level decompression separation, operating pressure is 8～12Mpa, and operative temperature is 30～35 ℃; Carry out second depressurized again and separate, condition is below the operating pressure 6Mpa, and operative temperature is 15～25 ℃, obtains the Placenta extract extract.This Placenta extract extract was handled 24 hours down at 30 ℃ with restriction endonuclease TCCRAC (20/18), the molecular weight of main component is reduced to below 6000 dalton.With the micromolecule extract that obtains under-40 ℃, the vacuum of 12Pa through lyophilization, obtain lyophilized powder.
Claim 80g phospholipid, 40g cholesterol and 33g poloxamer (F68),, make the liposome solutions barium salt with 1000ml chloroform or dichloromethane dissolving.Other gets the 80g extract, 240g mannitol is crossed 100 mesh sieve mix homogeneously, place coating pan, 30 ℃ of hot blast heating, coating pan rotates with 30r/min, with aerosol apparatus the lipid soln of being prepared is sprayed in the material that is stirring on a small quantity, hot blast volatilizes solvent, and then a small amount of spraying, volatilizes, extremely whole lipidosiss are on the mixture of medicine and carrier so repeatedly, volatilize solvent and place exsiccator to spend the night material, sieve, promptly get the Placenta extract liposome of exsiccant good fluidity.The gelatine capsule of packing at last.
Embodiment 2
Placental lipo-glucosaminoglycan stock solution is put into extraction kettle, feed the carbon dioxide of 20～30Mpa, under 30～40 ℃ of conditions, extract 8～12h; Through the one-level decompression separation, operating pressure is 8～12Mpa, and operative temperature is 30～35 ℃; Carry out second depressurized again and separate, condition is below the operating pressure 6Mpa, and operative temperature is 15～25 ℃, obtains the Placenta extract extract.(16/14 handled 18 hours under 30 ℃, and the molecular weight of main component is reduced to below 6000 dalton with restriction endonuclease CTGAAG to make this Placenta extract extract then.With molecular cut off is ultrafilter membrane (U.S. millipore company, standard ultrafiltration system) the ultrafiltration extract that 6000 roads pause, and makes ultrafiltrate through lyophilization, obtains lyophilized powder, the ultrafiltration trapped substance is repeated restriction endonuclease handle, and carries out ultra-filtration again.So repeat up to almost all extracts can see through ultrafilter membrane.Repeat about 4 to 5 times.With the micromolecule extract that obtains under-40 ℃, the vacuum of 12Pa through lyophilization, obtain lyophilized powder.
Claim 80g phospholipid, 40g cholesterol and 33g poloxamer (F68),, make the liposome solutions barium salt with 1000ml chloroform or dichloromethane dissolving.Other gets the 80g extract, 240g mannitol is crossed 100 mesh sieve mix homogeneously, place coating pan, 30 ℃ of hot blast heating, coating pan rotates with 30r/min, with aerosol apparatus the lipid soln of being prepared is sprayed in the material that is stirring on a small quantity, hot blast volatilizes solvent, and then a small amount of spraying, volatilizes, extremely whole lipidosiss are on the mixture of medicine and carrier so repeatedly, volatilize solvent and place exsiccator to spend the night material, sieve, promptly get the Placenta extract liposome of exsiccant good fluidity.The gelatine capsule of packing at last.
Embodiment 3
Placental lipo-glucosaminoglycan stock solution is put into extraction kettle, feed the carbon dioxide of 20～30Mpa, under 30～40 ℃ of conditions, extract 8～12h; Through the one-level decompression separation, operating pressure is 8～12Mpa, and operative temperature is 30～35 ℃; Carry out second depressurized again and separate, condition is below the operating pressure 6Mpa, and operative temperature is 15～25 ℃, obtains the Placenta extract extract.This Placenta extract extract was handled 24 hours down at 30 ℃ with restriction endonuclease CTTGAG (16/14), the molecular weight of main component is reduced to below 4000 dalton.With molecular cut off is 4000 daltonian ultrafilter membranes (U.S. millipore company, standard ultrafiltration system) ultrafiltration extracts, the ultrafiltration trapped substance is repeated restriction endonuclease handle, and carries out ultra-filtration again.So repeat up to almost all extracts can see through ultrafilter membrane.Repeat about 7 to 9 times.
With the micromolecule extract that obtains under-40 ℃, the vacuum of 12Pa through lyophilization, obtain lyophilized powder.Claim 80g phospholipid, 40g cholesterol and 33g poloxamer (F68),, make the liposome solutions barium salt with 1000ml chloroform or dichloromethane dissolving.Other gets the 80g extract, 240g mannitol is crossed 100 mesh sieve mix homogeneously, place coating pan, 30 ℃ of hot blast heating, coating pan rotates with 30r/min, with aerosol apparatus the lipid soln of being prepared is sprayed in the material that is stirring on a small quantity, hot blast volatilizes solvent, and then a small amount of spraying, volatilizes, extremely whole lipidosiss are on the mixture of medicine and carrier so repeatedly, volatilize solvent and place exsiccator to spend the night material, sieve, promptly get the Placenta extract liposome of exsiccant good fluidity.The gelatine capsule of packing at last.
The invention has the advantages that carbon dioxide supercritical extraction and the restriction endonuclease polysaccharide system of adopting The combination of standby technology. Carbon dioxide supercritical extraction technology fully all placental hormones is extracted The biologically active of thing, and the restriction endonuclease technology can effectively be controlled the molecular weight of active component, makes The active component that gets in the oral capsule obtained by this method can be absorbed by the body fully, its Health-care effect is not worse than the injection product, and has avoided the inconvenience of injection product and user to prick The misery of pin. Therefore, compared with prior art, method provided by the invention and product are better than Existing placenta element health product.
Claims (10)
1. the production method of a hyper-concentrated placenta lipopolysaccharide freeze-drying capsules may further comprise the steps:
A) with placental lipo-glucosaminoglycan stock solution process co_2 supercritical fluid extraction, obtain the Placenta extract extract;
B) utilize enzyme to handle described Placenta extract extract, molecular weight is reduced to below 6000 dalton;
C) with the micromolecule extract lyophilization that obtains in the step b), obtain lyophilized powder; And
D) adopt method for preparing lipidosome that described lyophilized powder is made hyper-concentrated placenta lipopolysaccharide freeze-drying capsules.
2. method according to claim 1, wherein, described extraction step is at 20～40MPa, carries out under 30～40 ℃ the condition.
3. method according to claim 2 wherein, repeats described extraction step 3 times to 10 times preferred 5 times to 10 times.
4. method according to claim 1, wherein, in step b, utilize restricted or half restricted enzyme under 30～40 ℃ to Placenta extract in the nucleic acid or the polysaccharide of macromolecule carry out the reaction of Restriction Enzyme inscribe.
5. method according to claim 4, wherein, described restricted enzyme is Mmel, TCCRAC (20/18); Eco57I, CTGAAG (16/14); Eco57MI, CTGRAG (16/14); Or Bce83I, CTTGAG (16/14).
6. method according to claim 1 wherein, further comprises a ultrafiltration step after step b), and controls molecular cut off by the aperture of selecting ultrafilter membrane.
7. method according to claim 1 wherein, is selected from described method for preparing lipidosome the group that is made of membrane process, multi-emulsion method, centrifuging, calcium fusion method, injection method, pH gradient method and prerequisite liposome method.
8. hyper-concentrated placenta lipopolysaccharide freeze-drying capsules that makes by each described method of claim 1 to 7.
9. hyper-concentrated placenta lipopolysaccharide freeze-drying capsules according to claim 8, wherein the molecular weight of Placenta extract polysaccharide is below 6000 dalton.
10. hyper-concentrated placenta lipopolysaccharide freeze-drying capsules according to claim 9, wherein the molecular weight of Placenta extract polysaccharide is below 4000 dalton.
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| CNA2007101079114A CN101306017A (en) | 2007-05-15 | 2007-05-15 | Hyper-concentrated placenta lipopolysaccharide freeze-drying capsules and its preparation method |
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| CNA2007101079114A CN101306017A (en) | 2007-05-15 | 2007-05-15 | Hyper-concentrated placenta lipopolysaccharide freeze-drying capsules and its preparation method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101837005A (en) * | 2010-04-12 | 2010-09-22 | 湖南圣雅凯生物科技有限公司 | Process for preparing pig placenta extract |
| CN106729601A (en) * | 2016-12-16 | 2017-05-31 | 王景仙 | Placental lipo-glucosaminoglycan, polypeptide bigeminy immunopotentiator and preparation method thereof |
-
2007
- 2007-05-15 CN CNA2007101079114A patent/CN101306017A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101837005A (en) * | 2010-04-12 | 2010-09-22 | 湖南圣雅凯生物科技有限公司 | Process for preparing pig placenta extract |
| CN106729601A (en) * | 2016-12-16 | 2017-05-31 | 王景仙 | Placental lipo-glucosaminoglycan, polypeptide bigeminy immunopotentiator and preparation method thereof |
| CN106729601B (en) * | 2016-12-16 | 2021-01-19 | 王景仙 | Placenta lipopolysaccharide and polypeptide dual immunopotentiator and preparation method thereof |
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Open date: 20081119 |