CN105506044A - Preparation method for blood cell protein peptide chelated calcium microcapsule preparation - Google Patents
Preparation method for blood cell protein peptide chelated calcium microcapsule preparation Download PDFInfo
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- CN105506044A CN105506044A CN201511005541.4A CN201511005541A CN105506044A CN 105506044 A CN105506044 A CN 105506044A CN 201511005541 A CN201511005541 A CN 201511005541A CN 105506044 A CN105506044 A CN 105506044A
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- 108090000765 processed proteins & peptides Proteins 0.000 title claims abstract description 86
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 title claims abstract description 77
- 239000011575 calcium Substances 0.000 title claims abstract description 77
- 229910052791 calcium Inorganic materials 0.000 title claims abstract description 77
- 210000000601 blood cell Anatomy 0.000 title claims abstract description 44
- 239000003094 microcapsule Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 32
- 102000004169 proteins and genes Human genes 0.000 title claims abstract description 27
- 108090000623 proteins and genes Proteins 0.000 title claims abstract description 27
- 238000006243 chemical reaction Methods 0.000 claims abstract description 37
- 108091005804 Peptidases Proteins 0.000 claims abstract description 27
- 239000000463 material Substances 0.000 claims abstract description 23
- 102000004190 Enzymes Human genes 0.000 claims abstract description 19
- 108090000790 Enzymes Proteins 0.000 claims abstract description 19
- 239000000203 mixture Substances 0.000 claims abstract description 19
- 239000004365 Protease Substances 0.000 claims abstract description 16
- 159000000007 calcium salts Chemical class 0.000 claims abstract description 15
- 239000008367 deionised water Substances 0.000 claims abstract description 15
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 230000007062 hydrolysis Effects 0.000 claims abstract description 3
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 3
- 102100037486 Reverse transcriptase/ribonuclease H Human genes 0.000 claims abstract 4
- 229960005069 calcium Drugs 0.000 claims description 68
- 239000000243 solution Substances 0.000 claims description 48
- 206010020633 Hyperglobulinaemia Diseases 0.000 claims description 28
- 102000035195 Peptidases Human genes 0.000 claims description 23
- 238000009472 formulation Methods 0.000 claims description 18
- 239000000706 filtrate Substances 0.000 claims description 15
- 235000019419 proteases Nutrition 0.000 claims description 15
- 238000005507 spraying Methods 0.000 claims description 15
- 238000010792 warming Methods 0.000 claims description 14
- 238000013019 agitation Methods 0.000 claims description 13
- 238000001976 enzyme digestion Methods 0.000 claims description 13
- 238000001914 filtration Methods 0.000 claims description 12
- 239000000796 flavoring agent Substances 0.000 claims description 10
- 235000019634 flavors Nutrition 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- 230000001105 regulatory effect Effects 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 101000693530 Staphylococcus aureus Staphylokinase Proteins 0.000 claims description 6
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 5
- 206010018910 Haemolysis Diseases 0.000 claims description 5
- 239000005913 Maltodextrin Substances 0.000 claims description 5
- 229920002774 Maltodextrin Polymers 0.000 claims description 5
- 241001465754 Metazoa Species 0.000 claims description 5
- 229930006000 Sucrose Natural products 0.000 claims description 5
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims description 5
- 239000001110 calcium chloride Substances 0.000 claims description 5
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 5
- 230000008588 hemolysis Effects 0.000 claims description 5
- 238000009413 insulation Methods 0.000 claims description 5
- 229940035034 maltodextrin Drugs 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- 238000002203 pretreatment Methods 0.000 claims description 5
- 239000005720 sucrose Substances 0.000 claims description 5
- 108090000145 Bacillolysin Proteins 0.000 claims description 4
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 4
- 102000035092 Neutral proteases Human genes 0.000 claims description 4
- 108091005507 Neutral proteases Proteins 0.000 claims description 4
- NEEHYRZPVYRGPP-IYEMJOQQSA-L calcium gluconate Chemical compound [Ca+2].OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C([O-])=O.OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C([O-])=O NEEHYRZPVYRGPP-IYEMJOQQSA-L 0.000 claims description 4
- MKJXYGKVIBWPFZ-UHFFFAOYSA-L calcium lactate Chemical compound [Ca+2].CC(O)C([O-])=O.CC(O)C([O-])=O MKJXYGKVIBWPFZ-UHFFFAOYSA-L 0.000 claims description 4
- 239000001527 calcium lactate Substances 0.000 claims description 4
- 229960002401 calcium lactate Drugs 0.000 claims description 4
- 235000011086 calcium lactate Nutrition 0.000 claims description 4
- 239000002131 composite material Substances 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 2
- 235000010216 calcium carbonate Nutrition 0.000 claims description 2
- 235000011148 calcium chloride Nutrition 0.000 claims description 2
- 239000001506 calcium phosphate Substances 0.000 claims description 2
- 229910000389 calcium phosphate Inorganic materials 0.000 claims description 2
- 235000011010 calcium phosphates Nutrition 0.000 claims description 2
- 239000004744 fabric Substances 0.000 claims description 2
- 238000000265 homogenisation Methods 0.000 claims description 2
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 claims description 2
- 239000000047 product Substances 0.000 abstract description 7
- 238000010521 absorption reaction Methods 0.000 abstract description 6
- 210000004369 blood Anatomy 0.000 abstract description 6
- 239000008280 blood Substances 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 4
- 230000009920 chelation Effects 0.000 abstract description 3
- 235000020776 essential amino acid Nutrition 0.000 abstract description 2
- 239000003797 essential amino acid Substances 0.000 abstract description 2
- 239000002366 mineral element Substances 0.000 abstract description 2
- 230000002949 hemolytic effect Effects 0.000 abstract 2
- 230000009849 deactivation Effects 0.000 abstract 1
- 235000015872 dietary supplement Nutrition 0.000 abstract 1
- 210000001035 gastrointestinal tract Anatomy 0.000 abstract 1
- 238000001694 spray drying Methods 0.000 abstract 1
- 241000282898 Sus scrofa Species 0.000 description 19
- 235000018102 proteins Nutrition 0.000 description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 239000002253 acid Substances 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 239000003513 alkali Substances 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 102000015636 Oligopeptides Human genes 0.000 description 2
- 108010038807 Oligopeptides Proteins 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 235000010755 mineral Nutrition 0.000 description 2
- 239000011812 mixed powder Substances 0.000 description 2
- 231100000957 no side effect Toxicity 0.000 description 2
- 102000004196 processed proteins & peptides Human genes 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000013589 supplement Substances 0.000 description 2
- 241000251468 Actinopterygii Species 0.000 description 1
- 102000004506 Blood Proteins Human genes 0.000 description 1
- 108010017384 Blood Proteins Proteins 0.000 description 1
- 208000024172 Cardiovascular disease Diseases 0.000 description 1
- 108010035532 Collagen Proteins 0.000 description 1
- 102000008186 Collagen Human genes 0.000 description 1
- 102000006395 Globulins Human genes 0.000 description 1
- 108010044091 Globulins Proteins 0.000 description 1
- 235000010469 Glycine max Nutrition 0.000 description 1
- 244000068988 Glycine max Species 0.000 description 1
- IMQLKJBTEOYOSI-GPIVLXJGSA-N Inositol-hexakisphosphate Chemical compound OP(O)(=O)O[C@H]1[C@H](OP(O)(O)=O)[C@@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@@H]1OP(O)(O)=O IMQLKJBTEOYOSI-GPIVLXJGSA-N 0.000 description 1
- XUYPXLNMDZIRQH-LURJTMIESA-N N-acetyl-L-methionine Chemical compound CSCC[C@@H](C(O)=O)NC(C)=O XUYPXLNMDZIRQH-LURJTMIESA-N 0.000 description 1
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 1
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 1
- 102000007544 Whey Proteins Human genes 0.000 description 1
- 108010046377 Whey Proteins Proteins 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 235000021120 animal protein Nutrition 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000975 bioactive effect Effects 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 150000001669 calcium Chemical class 0.000 description 1
- 229940106635 calcium amino acid chelate Drugs 0.000 description 1
- 229920001436 collagen Polymers 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000007071 enzymatic hydrolysis Effects 0.000 description 1
- 238000006047 enzymatic hydrolysis reaction Methods 0.000 description 1
- 150000003278 haem Chemical class 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 235000013372 meat Nutrition 0.000 description 1
- 229930182817 methionine Natural products 0.000 description 1
- 235000002949 phytic acid Nutrition 0.000 description 1
- 239000011669 selenium Substances 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 210000002784 stomach Anatomy 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 235000021119 whey protein Nutrition 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- UOXSXMSTSYWNMH-UHFFFAOYSA-L zinc;2-aminoacetate Chemical compound [Zn+2].NCC([O-])=O.NCC([O-])=O UOXSXMSTSYWNMH-UHFFFAOYSA-L 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P21/00—Preparation of peptides or proteins
- C12P21/06—Preparation of peptides or proteins produced by the hydrolysis of a peptide bond, e.g. hydrolysate products
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K38/00—Medicinal preparations containing peptides
Abstract
The invention relates to a preparation method for a blood cell protein peptide chelated calcium microcapsule preparation. The preparation method comprises the specific steps that pig blood cells and deionized water are prepared into hemolytic blood, then protease is added to the hemolytic blood, enzyme deactivation and filter pressing are carried out after hydrolysis, and the mixture carries out a chelation reaction with soluble calcium salt after the pH is adjusted; then a proper wall material solution is adopted for embedding the protein peptide chelated calcium solution, and blood cell protein peptide chelated calcium microcapsules are obtained through spray drying after embedding. The prepared blood cell protein peptide chelated calcium microcapsules are high in chelation rate and embedding rate, the solubility of calcium salt in the gastrointestinal tract environment can be improved, and the slow release effect can be achieved. In addition, after calcium salt is released, the absorption rate of calcium is increased through the form of small peptide chelated calcium, the preparation process is safe and free of pollution, absorption of mineral element calcium is promoted while essential amino-acid for the human body is supplemented, and the blood cell protein peptide chelated calcium microcapsule preparation is a good nutrient supplement product.
Description
Technical field
The invention belongs to bioengineering field, be specifically related to a kind of preparation method of hyperglobulinemia peptide chelating calcium microcapsule formulation.
Background technology
At present all there is drawback in various degree for first, second and third calcium preparation of supplementary human body mineral substance, first-generation calcium preparation mostly is inorganic calcium in generation, although its calcium content is high, convenient for production, cheap, specific absorption is lower and easily cause stomach side effect; S-generation calcium preparation be traditional organic calcium as calcium lactate, calglucon etc., its solvability is better than inorganic calcium, but phytate easily and in food, oxalate react and cause utilization ratio low, and the acid group of organic calcium salt is put aside in vivo and can be produced untoward reaction; Although third generation calcium amino acid chelate solvability and absorptivity are all relatively good, have no side effect, in transhipment, have certain defect, high not as oligopeptides chelating calcium absorptivity.Forth generation calcium preparation peptide calcium, due to the transporting mechanism of its uniqueness, its absorption rate and utilization ratio are all far above current all calcium supplementing products, and therefore developing peptide calcium product has wide market outlook.
In recent years, the mineral substance such as calcium, iron, zinc, selenium and the small-peptide chelated research preparing mineral element supplement get more and more, current multiplex soybean peptides, whey protein peptide, collagen peptide, animal bone peptide, fish processing byproduct etc. as peptide source, and with less as peptide source of hyperglobulinemia peptide.
Domestic pig blood resource is very abundant, have the title of liquid meat, and its amino acid is comprehensive, but effective rate of utilization is not high, except minority is edible or spraying dry is except blood cell plasma protein powder, globulin powder, majority is exhausted in surrounding environment, produce and greatly pollute, high value-added product is less.If blood cell enzyme-squash techniqued can be utilized to obtain hyperglobulinemia peptide, control peptide production technique and can obtain rich heme peptide, now successfully realize the chelating of itself and calcium again, products obtained therefrom can play albumen, iron, the re-absorbed effect of calcium three.Not only can reduce the wasting of resources, also can be food, medicines and health protection field provides new protein peptide and calcium preparation source.
Summary of the invention
The object of the invention is to: provide a kind of with pig blood cell for the preparation method of hyperglobulinemia peptide chelating calcium microcapsule formulation prepared by raw material.
In order to realize foregoing invention object, the invention provides following technical scheme:
A kind of preparation method of hyperglobulinemia peptide chelating calcium microcapsule formulation, make in accordance with the following methods: pig blood cell and deionized water are configured to hemolysate, then proteolytic enzyme is added in hemolysate, to go out after hydrolysis enzyme, press filtration, chelatropic reaction is carried out with soluble calcium salt after regulating pH, adopt suitable wall material solution to embed protein peptide chelating calcium solution again, after embedding, namely spraying dry obtains hyperglobulinemia peptide chelating calcium microcapsule.
Preferably, the preparation method of described hyperglobulinemia peptide chelating calcium microcapsule formulation, concrete steps are as follows:
(1) pre-treatment of blood cell: pig haemolysis is made hemolysate in deionized water, the weight ratio of pig blood cell and deionized water is 1:1.5 ~ 1:5; Then hemolysate pH value is regulated to be 7 ~ 11;
(2) protease hydrolyzed: proteolytic enzyme is added in hemolysate, Keep agitation enzyme digestion reaction 1 ~ 15 hour after being warming up to 45 ~ 65 DEG C, wherein, the add-on of proteolytic enzyme is 0.5 ~ 4% of former pig blood cell weight;
(3) to go out enzyme, press filtration: enzymolysis solution is warming up to 85 ~ 95 DEG C, keep 20 ~ 60min to go out enzyme, after being cooled to 40 ~ 65 DEG C, regulate enzymolysis solution pH value to be 2 ~ 8; Enzymolysis solution after adjustment pH is squeezed into plate-and-frame filter press press filtration and obtains blood cell peptide filtrate;
(4) chelatropic reaction: regulate blood cell peptide filtrate pH to 9 ~ 11, soluble calcium salt is added after being heated to 55 ~ 70 DEG C, the mass ratio of soluble calcium salt and blood cell peptide filtrate is 1:3 ~ 1:6, insulation intermittent stirring carries out chelatropic reaction in 1 ~ 6 hour, obtain protein peptide chelating calcium solution, in whole chelatropic reaction process, regulator solution pH makes it to maintain 9 ~ 11;
(5) homogeneous: add wall material solution after chelatropic reaction completes in protein peptide chelating calcium solution, intimate mixing;
(6) spraying dry embedding: get the wall material core mixed solution after mixing, the hyperglobulinemia peptide chelating calcium microcapsule that spraying dry is.
Preferably, in step (1), after hemolysate mixes with deionized water, stir 2 ~ 4h and make blood cell breakage discharge oxyphorase, obtain hemolysate.
Preferably, in step (2), when proteolytic enzyme used is Sumizyme MP, neutral protease and flavor protease, initial pH regulator to 8.5 ~ 9.5 of hemolysate enzymolysis, first add Sumizyme MP, after being warming up to 50 ~ 60 DEG C, Keep agitation enzyme digestion reaction 1 ~ 4h, then adds 1398 neutral proteinase and flavor protease, do not regulate pH, Keep agitation enzyme digestion reaction 2 ~ 6h after adjusting the temperature to 45 ~ 55 DEG C.
Preferably, in step (2), when proteolytic enzyme used is composite animal albumen enzyme, initial pH regulator to 7 ~ 7.5 of hemolysate enzymolysis, after enzyme-added, Keep agitation enzyme digestion reaction 4 ~ 12h after being warming up to 50 ~ 60 DEG C.
Preferably, be cooled to 50 ~ 60 DEG C after the enzyme that goes out in step (3), regulate pH to 4.5 ~ 5.5, the aperture that the filter cloth of plate-and-frame filter press is selected is 400 orders.
Preferably, in step (4), soluble calcium salt is one or several the combination in calcium chloride, calcium carbonate, calcium phosphate, calcium lactate, calglucon.
Preferably, in step (5) wall material solution, the ratio of Yelkin TTS, sucrose, maltodextrin is 2:1:1 or 3:1.5:2, the mass ratio of wall material solution and protein peptide chelating calcium solution is 4:1 ~ 2:1, and when mixing with clarifixator, homogenization pressure is 40 ~ 60Mpa, homogenizing time 5 ~ 10min.
Preferably, in step (6), during spraying dry, inlet temperature is 150 ~ 200 DEG C, air outlet temperature 65 ~ 80 DEG C, fresh feed pump flow velocity 7 ~ 10r/min.
Preferably, the yield of the protein peptide chelating calcium microcapsule described in step (6) is 70 ~ 90%, calcium content 8.0 ~ 12.0%.
Beneficial effect of the present invention is:
1, gained hyperglobulinemia peptide chelating calcium microcapsule of the present invention are off-white powder, Oranoleptic indicator is better, gained protein peptide chelation percent reaches 70 ~ 90%, in inner complex, peptide is oligopeptides, molecular weight is between 200 ~ 1000Da, and more easily for transhipment absorbs in enteron aisle, its stability, utilization ratio and absorption rate are all far above current calcium class preparation, safe preparation process, pollution-free, have no side effect.
2, in addition due to the existence of chelated calcium biologically active peptides, this product also have certain anti-oxidant, improve immunity, prevent the effects such as cardiovascular disorder, treatment process products obtained therefrom after controlled enzymatic hydrolysis, containing a certain amount of protoheme, also realizes the absorption facilitating body iron while supplement calcium and bioactive peptide.
3, raw material that the present invention adopts is butchery by product pig blood, its essential amino acids content is higher, particularly Methionin, cost is lower comparatively speaking, not only increase utilization ratio and the added value of pig blood, reduce the environmental pollution of pig blood discharge, simultaneously also for animal protein peptide provides a kind of new peptide class raw material.
Embodiment
Embodiment 1:
A preparation method for hyperglobulinemia peptide chelating calcium microcapsule formulation, concrete steps are as follows:
(1) pre-treatment of blood cell: a certain amount of pig haemolysis is made hemolysate in deionized water, the weight ratio of hemolysate and deionized water is 1:1.5; Then hemolysate pH value is regulated to be 7.0 with 6MNaOH;
(2) protease hydrolyzed: composite animal albumen enzyme is added in hemolysate, Keep agitation enzyme digestion reaction 6 hours after being warming up to 55 DEG C, wherein, the add-on of proteolytic enzyme is 0.8% of former pig blood cell weight; Composite animal albumen enzyme used provides for Nanning Pang Bo biotechnology company limited.
(3) to go out enzyme, press filtration: enzymolysis solution is warming up to 85 DEG C, keep 25min to go out enzyme, after being cooled to 55 DEG C, regulate enzymolysis solution pH value to be 5.0 with hydrochloric acid; Enzymolysis solution after adjustment pH is squeezed into plate-and-frame filter press press filtration and obtains blood cell peptide filtrate;
(4) chelatropic reaction: regulate blood cell peptide filtrate pH to 10.0 with sodium hydroxide or hydrochloric acid, calcium chloride and calglucon 1:1 mixed powder is added after being heated to 60 DEG C, the addition of calcium salt and the mass ratio of blood cell peptide filtrate are 1:4, insulation intermittent stirring carries out chelatropic reaction in 1.5 hours, obtain protein peptide chelating calcium solution, regulate with acid or alkali in whole chelatropic reaction process and make pH value maintain 10.0;
(5) homogeneous: add the wall material solution dissolved in advance after chelatropic reaction completes in chelating liquid, Yelkin TTS in wall material solution: sucrose: maltodextrin is 2:1:1, wall material solution and the ratio of core (protein peptide chelating calcium solution) they are that after 2:1 mixes, 50Mpa homogeneous 10min fully mixes;
(6) spraying dry embedding: get the wall material core mixed solution after mixing, inlet temperature 180 DEG C, air outlet temperature 80 DEG C, under fresh feed pump flow velocity 8r/min, namely spraying dry obtains hyperglobulinemia peptide chelating calcium microcapsule, the yield of described protein peptide chelating calcium microcapsule is 75%, calcium content 8.5%.
Embodiment 2:
A preparation method for hyperglobulinemia peptide chelating calcium microcapsule formulation, concrete steps are as follows:
(1) pre-treatment of blood cell: a certain amount of pig haemolysis is made hemolysate in deionized water, the weight ratio of hemolysate and deionized water is 1:3; Then hemolysate pH value is regulated to be 9.0 with 6MNaOH;
(2) protease hydrolyzed: Sumizyme MP is added in hemolysate, Keep agitation enzyme digestion reaction 2h after being warming up to 58 DEG C, then 1398 neutral proteinase and flavor protease is added, do not regulate pH, Keep agitation enzyme digestion reaction 4h after adjusting the temperature to 50 DEG C, wherein, the add-on of Sumizyme MP is 1.5% of former pig blood cell weight, the add-on of 1398 neutral proteinase is 1% of former pig blood cell weight, and the add-on of flavor protease is 1% of former pig blood cell weight.Sumizyme MP used, neutral protease and flavor protease provide for Si Beite bio tech ltd, Xingtai.
(3) to go out enzyme, press filtration: enzymolysis solution is warming up to 95 DEG C, keep 15min to go out enzyme, after being cooled to 50 DEG C, regulate enzymolysis solution pH value to be 4.8 with hydrochloric acid; Enzymolysis solution after adjustment pH is squeezed into plate-and-frame filter press press filtration and obtains blood cell peptide filtrate;
(4) chelatropic reaction: regulate blood cell peptide filtrate pH to 10.5 with sodium hydroxide or hydrochloric acid, calcium chloride is added after being heated to 65 DEG C, the addition of calcium salt and the mass ratio of blood cell peptide filtrate are 1:3.5, insulation intermittent stirring carries out chelatropic reaction in 1 hour, obtain protein peptide chelating calcium solution, regulate with acid or alkali in whole chelatropic reaction process and make pH value maintain 10.5;
(5) homogeneous: add the wall material solution dissolved in advance after chelatropic reaction completes in chelating liquid, Yelkin TTS in wall material solution: sucrose: maltodextrin is 3:1.5:2, the ratio of wall material solution and core (protein peptide chelating calcium solution) is 3:1, and after mixing, 45Mpa homogeneous 10min fully mixes;
(6) spraying dry embedding: get the wall material core mixed solution after mixing, inlet temperature 190 DEG C, air outlet temperature 75 DEG C, under fresh feed pump flow velocity 7r/min, namely spraying dry obtains hyperglobulinemia peptide chelating calcium microcapsule, the yield of described protein peptide chelating calcium microcapsule is 85%, calcium content 10%.
Embodiment 3:
A preparation method for hyperglobulinemia peptide chelating calcium microcapsule formulation, concrete steps are as follows:
(1) pre-treatment of blood cell: a certain amount of pig haemolysis is made hemolysate in deionized water, the weight ratio of hemolysate and deionized water is 1:4; Then hemolysate pH value is regulated to be 8.5 with 6MNaOH;
(2) protease hydrolyzed: Sumizyme MP is added in hemolysate, Keep agitation enzyme digestion reaction 1h after being warming up to 55 DEG C, then 1398 neutral proteinase and flavor protease is added, do not regulate pH, Keep agitation enzyme digestion reaction 3h after adjusting the temperature to 50 DEG C, wherein, the add-on of Sumizyme MP is 1.5% of former pig blood cell weight, the add-on of 1398 neutral proteinase is 1.5% of former pig blood cell weight, and the add-on of flavor protease is 1% of former pig blood cell weight.Sumizyme MP used, neutral protease and flavor protease provide for Si Beite bio tech ltd, Xingtai.
(3) to go out enzyme, press filtration: enzymolysis solution is warming up to 90 DEG C, keep 20min to go out enzyme, after being cooled to 53 DEG C, regulate enzymolysis solution pH value to be 5.4 with hydrochloric acid; Enzymolysis solution after adjustment pH is squeezed into plate-and-frame filter press press filtration and obtains blood cell peptide filtrate;
(4) chelatropic reaction: regulate blood cell peptide filtrate pH to 9.5 with sodium hydroxide or hydrochloric acid, the mixed powder of calcium lactate and calcium chloride 1:3 is added after being heated to 70 DEG C, the addition of calcium salt and the mass ratio of blood cell peptide filtrate are 1:5, insulation intermittent stirring carries out chelatropic reaction in 2.0 hours, obtain protein peptide chelating calcium solution, regulate with acid or alkali in whole chelatropic reaction process and make pH value maintain 9.5;
(5) homogeneous: add the wall material solution dissolved in advance after chelatropic reaction completes in chelating liquid, Yelkin TTS in wall material solution: sucrose: maltodextrin is 2:1:1, wall material solution and the ratio of core (protein peptide chelating calcium solution) are that after 4:1 mixes, 60Mpa homogeneous 5min fully mixes
(6) spraying dry embedding: get the wall material core mixed solution after mixing, inlet temperature 190 DEG C, air outlet temperature 70 DEG C, under fresh feed pump flow velocity 6r/min, namely spraying dry obtains hyperglobulinemia peptide chelating calcium microcapsule, the yield of described protein peptide chelating calcium microcapsule is 90%, calcium content 11.5%.
Claims (10)
1. the preparation method of a hyperglobulinemia peptide chelating calcium microcapsule formulation, it is characterized in that: make in accordance with the following methods: pig blood cell and deionized water are configured to hemolysate, then proteolytic enzyme is added in hemolysate, to go out after hydrolysis enzyme, press filtration, chelatropic reaction is carried out with soluble calcium salt after regulating pH, adopt suitable wall material solution to embed protein peptide chelating calcium solution again, after embedding, namely spraying dry obtains hyperglobulinemia peptide chelating calcium microcapsule.
2. the preparation method of hyperglobulinemia peptide chelating calcium microcapsule formulation according to claim 1, is characterized in that: concrete steps are as follows:
(1) pre-treatment of blood cell: pig haemolysis is made hemolysate in deionized water, the weight ratio of pig blood cell and deionized water is 1:1.5 ~ 1:5; Then hemolysate pH value is regulated to be 7 ~ 11;
(2) protease hydrolyzed: proteolytic enzyme is added in hemolysate, Keep agitation enzyme digestion reaction 1 ~ 15 hour after being warming up to 45 ~ 65 DEG C, wherein, the add-on of proteolytic enzyme is 0.5 ~ 4% of former pig blood cell weight;
(3) to go out enzyme, press filtration: enzymolysis solution is warming up to 85 ~ 95 DEG C, keep 20 ~ 60min to go out enzyme, after being cooled to 40 ~ 65 DEG C, regulate enzymolysis solution pH value to be 2 ~ 8; Enzymolysis solution after adjustment pH is squeezed into plate-and-frame filter press press filtration and obtains blood cell peptide filtrate;
(4) chelatropic reaction: regulate blood cell peptide filtrate pH to 9 ~ 11, soluble calcium salt is added after being heated to 55 ~ 70 DEG C, the mass ratio of soluble calcium salt and blood cell peptide filtrate is 1:3 ~ 1:6, insulation intermittent stirring carries out chelatropic reaction in 1 ~ 6 hour, obtain protein peptide chelating calcium solution, in whole chelatropic reaction process, regulator solution pH makes it to maintain 9 ~ 11;
(5) homogeneous: add wall material solution after chelatropic reaction completes in protein peptide chelating calcium solution, intimate mixing;
(6) spraying dry embedding: get the wall material core mixed solution after mixing, the hyperglobulinemia peptide chelating calcium microcapsule that spraying dry is.
3. the preparation method of hyperglobulinemia peptide chelating calcium microcapsule formulation according to claim 2, it is characterized in that: in step (1), after hemolysate mixes with deionized water, stir 2 ~ 4h and make blood cell breakage discharge oxyphorase, obtain hemolysate.
4. the preparation method of hyperglobulinemia peptide chelating calcium microcapsule formulation according to claim 2, it is characterized in that: in step (2), when proteolytic enzyme used is Sumizyme MP, neutral protease and flavor protease, initial pH regulator to 8.5 ~ 9.5 of hemolysate enzymolysis, first add Sumizyme MP, Keep agitation enzyme digestion reaction 1 ~ 4h after being warming up to 50 ~ 60 DEG C, then 1398 neutral proteinase and flavor protease is added, do not regulate pH, Keep agitation enzyme digestion reaction 2 ~ 6h after adjusting the temperature to 45 ~ 55 DEG C.
5. the preparation method of hyperglobulinemia peptide chelating calcium microcapsule formulation according to claim 2, it is characterized in that: in step (2), when proteolytic enzyme used is composite animal albumen enzyme, initial pH regulator to 7 ~ 7.5 of hemolysate enzymolysis, after enzyme-added, Keep agitation enzyme digestion reaction 4 ~ 12h after being warming up to 50 ~ 60 DEG C.
6. the preparation method of hyperglobulinemia peptide chelating calcium microcapsule formulation according to claim 2, it is characterized in that: after the enzyme that goes out in step (3), be cooled to 50 ~ 60 DEG C, regulate pH to 4.5 ~ 5.5, the aperture that the filter cloth of plate-and-frame filter press is selected is 400 orders.
7. the preparation method of hyperglobulinemia peptide chelating calcium microcapsule formulation according to claim 2, is characterized in that: in step (4), soluble calcium salt is one or several the combination in calcium chloride, calcium carbonate, calcium phosphate, calcium lactate, calglucon.
8. the preparation method of hyperglobulinemia peptide chelating calcium microcapsule formulation according to claim 2, it is characterized in that: in step (5) wall material solution, the ratio of Yelkin TTS, sucrose, maltodextrin is 2:1:1 or 3:1.5:2, the mass ratio of wall material solution and protein peptide chelating calcium solution is 4:1 ~ 2:1, when mixing with clarifixator, homogenization pressure is 40 ~ 60Mpa, homogenizing time 5 ~ 10min.
9. the preparation method of hyperglobulinemia peptide chelating calcium microcapsule formulation according to claim 2, is characterized in that: in step (6), during spraying dry, inlet temperature is 150 ~ 200 DEG C, air outlet temperature 65 ~ 80 DEG C, fresh feed pump flow velocity 7 ~ 10r/min.
10. the preparation method of hyperglobulinemia peptide chelating calcium microcapsule formulation according to claim 2, is characterized in that: the yield of the protein peptide chelating calcium microcapsule described in step (6) is 70 ~ 90%, calcium content 8.0 ~ 12.0%.
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