CN108531531A - A kind of casein phosphopeptide preparation method of beta-cyclodextrin and the de- hardship of chitosan - Google Patents
A kind of casein phosphopeptide preparation method of beta-cyclodextrin and the de- hardship of chitosan Download PDFInfo
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- CN108531531A CN108531531A CN201810283751.7A CN201810283751A CN108531531A CN 108531531 A CN108531531 A CN 108531531A CN 201810283751 A CN201810283751 A CN 201810283751A CN 108531531 A CN108531531 A CN 108531531A
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- 239000005018 casein Substances 0.000 title claims abstract description 41
- BECPQYXYKAMYBN-UHFFFAOYSA-N casein, tech. Chemical compound NCCCCC(C(O)=O)N=C(O)C(CC(O)=O)N=C(O)C(CCC(O)=N)N=C(O)C(CC(C)C)N=C(O)C(CCC(O)=O)N=C(O)C(CC(O)=O)N=C(O)C(CCC(O)=O)N=C(O)C(C(C)O)N=C(O)C(CCC(O)=N)N=C(O)C(CCC(O)=N)N=C(O)C(CCC(O)=N)N=C(O)C(CCC(O)=O)N=C(O)C(CCC(O)=O)N=C(O)C(COP(O)(O)=O)N=C(O)C(CCC(O)=N)N=C(O)C(N)CC1=CC=CC=C1 BECPQYXYKAMYBN-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 235000021240 caseins Nutrition 0.000 title claims abstract description 41
- 229920000858 Cyclodextrin Polymers 0.000 title claims abstract description 19
- WHGYBXFWUBPSRW-FOUAGVGXSA-N beta-cyclodextrin Chemical compound OC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)CO)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1CO WHGYBXFWUBPSRW-FOUAGVGXSA-N 0.000 title claims abstract description 18
- 235000011175 beta-cyclodextrine Nutrition 0.000 title claims abstract description 18
- 229920001661 Chitosan Polymers 0.000 title claims abstract description 17
- 108010001441 Phosphopeptides Proteins 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000001116 FEMA 4028 Substances 0.000 title claims description 17
- 229960004853 betadex Drugs 0.000 title claims description 17
- 239000007788 liquid Substances 0.000 claims abstract description 25
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 18
- 150000001875 compounds Chemical class 0.000 claims abstract description 12
- 239000003463 adsorbent Substances 0.000 claims abstract description 11
- 108090000790 Enzymes Proteins 0.000 claims abstract description 7
- 102000004190 Enzymes Human genes 0.000 claims abstract description 7
- 229940088598 enzyme Drugs 0.000 claims abstract description 7
- 108090000526 Papain Proteins 0.000 claims abstract description 6
- 239000004365 Protease Substances 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 230000009849 deactivation Effects 0.000 claims abstract description 6
- 229940055729 papain Drugs 0.000 claims abstract description 6
- 235000019834 papain Nutrition 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 108010076119 Caseins Proteins 0.000 claims description 37
- 102000011632 Caseins Human genes 0.000 claims description 37
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 20
- 239000000243 solution Substances 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 239000012460 protein solution Substances 0.000 claims description 5
- 239000003643 water by type Substances 0.000 claims description 5
- 230000036760 body temperature Effects 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 12
- 230000000694 effects Effects 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract 1
- 239000000047 product Substances 0.000 description 7
- 235000019658 bitter taste Nutrition 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 3
- 108090000765 processed proteins & peptides Proteins 0.000 description 3
- 238000001694 spray drying Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 150000001413 amino acids Chemical class 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000005538 encapsulation Methods 0.000 description 2
- 230000002209 hydrophobic effect Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000000873 masking effect Effects 0.000 description 2
- 102000004196 processed proteins & peptides Human genes 0.000 description 2
- 235000018102 proteins Nutrition 0.000 description 2
- 102000004169 proteins and genes Human genes 0.000 description 2
- 108090000623 proteins and genes Proteins 0.000 description 2
- XOAAWQZATWQOTB-UHFFFAOYSA-N taurine Chemical compound NCCS(O)(=O)=O XOAAWQZATWQOTB-UHFFFAOYSA-N 0.000 description 2
- 241000583281 Sugiura Species 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 108010079058 casein hydrolysate Proteins 0.000 description 1
- 230000002255 enzymatic effect Effects 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 230000001339 gustatory effect Effects 0.000 description 1
- 235000013402 health food Nutrition 0.000 description 1
- 125000001165 hydrophobic group Chemical group 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 150000003904 phospholipids Chemical class 0.000 description 1
- 229920001184 polypeptide Polymers 0.000 description 1
- HFHDHCJBZVLPGP-UHFFFAOYSA-N schardinger α-dextrin Chemical compound O1C(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(O)C2O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC2C(O)C(O)C1OC2CO HFHDHCJBZVLPGP-UHFFFAOYSA-N 0.000 description 1
- 235000012976 tarts Nutrition 0.000 description 1
- 210000001779 taste bud Anatomy 0.000 description 1
- 229960003080 taurine Drugs 0.000 description 1
Classifications
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- 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
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07K—PEPTIDES
- C07K1/00—General methods for the preparation of peptides, i.e. processes for the organic chemical preparation of peptides or proteins of any length
- C07K1/14—Extraction; Separation; Purification
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Zoology (AREA)
- Molecular Biology (AREA)
- Engineering & Computer Science (AREA)
- Genetics & Genomics (AREA)
- General Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Wood Science & Technology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Microbiology (AREA)
- Bioinformatics & Cheminformatics (AREA)
- General Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Biotechnology (AREA)
- Analytical Chemistry (AREA)
- Biophysics (AREA)
- Medicinal Chemistry (AREA)
- Proteomics, Peptides & Aminoacids (AREA)
- Peptides Or Proteins (AREA)
- Cosmetics (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The present invention relates to a kind of beta cyclodextrins and chitosan to take off bitter casein phosphopeptide preparation method, and this approach includes the following steps：(1) be added NaOH solution in casein, it is agitated uniformly after, obtain the casein solution that mass concentration is 15%；(2) for the casein solution tune pH value to papain is added after 5.5 ~ 6.5,15 ~ 25min of enzyme deactivation after water bath with thermostatic control enzymolysis obtains enzymolysis liquid through natural cooling；(3) the enzymolysis liquid tune pH value is to compound adsorbent is added after 6.5 ~ 7.5, and stirring and adsorbing takes off 50 ~ 70min of hardship under 35 ~ 45 DEG C of water-baths, obtains the enzymolysis liquid after de- hardship；(4) the enzymolysis liquid after the de- hardship is spray-dried, obtains product casein phosphopeptide.The method of the present invention is simple and practicable, and economic and de-bittering effect is splendid.
Description
Technical field
The present invention relates to casein production technical fields more particularly to a kind of beta-cyclodextrin and chitosan to take off bitter casein
Phosphoeptide preparation method.
Background technology
Casein generation bitter taste during enzymolysis is at polypeptide is mainly the peptide of some hydrophobic amino acids contained by it
Caused, hydrophobic residue is exposed to molecular surface, and gradually generates bitter taste with gustatory, and hydrophobic amino acid content is got over
Height, bitter taste are stronger.The presence of bitter taste affects the quality and its mouthfeel of product, limits casein phosphopeptide in industry such as food
In application, it is therefore necessary to de- suffering reason is carried out to casein hydrolysate.
Currently used debitterizing method is mainly the following：Select absorption method, partition method, encapsulation method, enzyme process, microorganism
Debittering france etc., wherein absorption method and encapsulation method use more.De- hardship is carried out to enzymolysis liquid for example, by using immobilization cyclodextrin column,
Masking agent can recycle in this way, but also result in the loss of Partial Protein nitrogen simultaneously.For another example Sugiura is to protein enzymatic hydrolyzate
The de- hardship of the health food of preparation is studied, it is found that addition acidic phospholipid and lysophosphatide can reduce the bitter of product.
But certain tart flavour can also be brought while reducing bitter taste to product by adding these masking agents.Using the side of addition taurine solution
This problem is not present in method, but it is expensive, is not suitable for industrialized production.
Invention content
Technical problem to be solved by the invention is to provide a kind of a kind of simple and practicable, effective beta-cyclodextrin and shells
Glycan takes off bitter casein phosphopeptide preparation method.
It is prepared to solve the above problems, a kind of beta-cyclodextrin of the present invention and chitosan take off bitter casein phosphopeptide
Method includes the following steps：
(1) be added the NaOH solution of a concentration of 1mol/L in casein, it is agitated uniformly after, obtain the junket that mass concentration is 15%
Protein solution；
(2) in the casein solution plus the hydrochloric acid tune pH value of a concentration of 0.1mol/L is to after 5.5 ~ 6.5, by initial casein protein
Papain is added in the 0.4 ~ 0.8% of amount, the enzymolysis of 140 ~ 160min of progress in 55 ~ 65 DEG C of waters bath with thermostatic control, after the completion of enzymolysis
Then at 90 ~ 100 DEG C of 15 ~ 25min of enzyme deactivation, enzymolysis liquid is obtained through natural cooling；
(3) in the enzymolysis liquid plus the hydrochloric acid tune pH value of a concentration of 0.1mol/L is to after 6.5 ~ 7.5, by initial casein quality
15 ~ 25% are added compound adsorbent, and stirring and adsorbing takes off 50 ~ 70min of hardship under 35 ~ 45 DEG C of water-baths, obtain the enzymolysis liquid after de- hardship；
The compound adsorbent refers to by beta-cyclodextrin and water-soluble chitosan by 4 ~ 6：The mixture that 1 mass ratio is obtained by mixing；
(4) the enzymolysis liquid after the de- hardship is spray-dried, obtains product casein phosphopeptide.
The step (4) in the condition that is spray-dried refer to steam pressure ＞ 0.75MPa, 160 DEG C of tower body inlet air temperature ＞,
In tower temperature be 65 ~ 75 DEG C, 63 DEG C of tower body temperature of outgoing air ＞, in tower negative pressure be -20 ~ -100Pa, high pressure pump pressure be 10 ~
25MPa。
Compared with the prior art, the present invention has the following advantages：
1, for the present invention using beta-cyclodextrin and chitosan to being in that bitter peptides have carried out absorption embedding, which is embedded in compound suction
In attached dose of gap, the contact with taste bud is reduced, to make bitterness value reduce.
2, beta cyclodextrin is cheap and easy to get in the present invention, and water-soluble chitosan is slightly expensive but dosage is less, overall entirely to prepare
Cheng Chengben is relatively low.
3, enzymolysis time of the present invention totally expends time about 4h with the de- bitter time, time saving compared with prior art.
4, almost color keep is constant for solution in whole preparation process by the present invention, and de- bitter process need to only control temperature.
5, the method for the present invention is simple and practicable, and economic and de-bittering effect is splendid.
Specific implementation mode
A kind of 1 beta-cyclodextrin of embodiment and chitosan take off bitter casein phosphopeptide preparation method, include the following steps：
(1) be added the NaOH solution of a concentration of 1mol/L in casein, it is agitated uniformly after, obtain the junket that mass concentration is 15%
Protein solution.
(2) in casein solution plus the hydrochloric acid tune pH value of a concentration of 0.1mol/L is to after 5.5, by initial casein quality
0.4% is added papain, the enzymolysis of progress 160min in 55 DEG C of waters bath with thermostatic control, then at 90 DEG C of enzyme deactivations after the completion of enzymolysis
25min obtains enzymolysis liquid through natural cooling.
(3) in enzymolysis liquid plus the hydrochloric acid tune pH value of a concentration of 0.1mol/L is to after 6.5, add by the 15% of initial casein quality
Enter compound adsorbent, stirring and adsorbing takes off hardship 70min under 35 DEG C of water-baths, obtains the enzymolysis liquid after de- hardship.
Wherein：Compound adsorbent refers to by beta-cyclodextrin and water-soluble chitosan by 4：1 mass ratio（g/g）Mixing and
The mixture obtained.
(4) the enzymolysis liquid taken off after hardship is spray-dried, obtains product casein phosphopeptide.
Wherein：The condition of spray drying refers to steam pressure ＞ 0.75MPa, 160 DEG C of tower body inlet air temperature ＞, temperature in tower
It it is 65 ~ 75 DEG C, 63 DEG C of tower body temperature of outgoing air ＞, negative pressure is -20 ~ -100Pa in tower, and high pressure pump pressure is 10 ~ 25MPa.
A kind of 2 beta-cyclodextrin of embodiment and chitosan take off bitter casein phosphopeptide preparation method, include the following steps：
(1) be added the NaOH solution of a concentration of 1mol/L in casein, it is agitated uniformly after, obtain the junket that mass concentration is 15%
Protein solution.
(2) in casein solution plus the hydrochloric acid tune pH value of a concentration of 0.1mol/L is to after 6.5, by initial casein quality
0.8% is added papain, the enzymolysis of progress 140min in 65 DEG C of waters bath with thermostatic control, then at 100 DEG C of enzyme deactivations after the completion of enzymolysis
15min obtains enzymolysis liquid through natural cooling.
(3) in enzymolysis liquid plus the hydrochloric acid tune pH value of a concentration of 0.1mol/L is to after 7.5, add by the 25% of initial casein quality
Enter compound adsorbent, stirring and adsorbing takes off hardship 50min under 45 DEG C of water-baths, obtains the enzymolysis liquid after de- hardship.
Wherein：Compound adsorbent refers to by beta-cyclodextrin and water-soluble chitosan by 6：1 mass ratio（g/g）Mixing and
The mixture obtained.
(4) the enzymolysis liquid taken off after hardship is spray-dried, obtains product casein phosphopeptide.
Wherein spray drying condition is the same as embodiment 1.
A kind of 3 beta-cyclodextrin of embodiment and chitosan take off bitter casein phosphopeptide preparation method, include the following steps：
(1) be added the NaOH solution of a concentration of 1mol/L in casein, it is agitated uniformly after, obtain the junket that mass concentration is 15%
Protein solution.
(2) in casein solution plus the hydrochloric acid tune pH value of a concentration of 0.1mol/L is to after 6.0, by initial casein quality
0.6% is added papain, the enzymolysis of progress 150min in 60 DEG C of waters bath with thermostatic control, then at 95 DEG C of enzyme deactivations after the completion of enzymolysis
20min obtains enzymolysis liquid through natural cooling.
(3) in enzymolysis liquid plus the hydrochloric acid tune pH value of a concentration of 0.1mol/L is to after 7.0, add by the 20% of initial casein quality
Enter compound adsorbent, stirring and adsorbing takes off hardship 60min under 40 DEG C of water-baths, obtains the enzymolysis liquid after de- hardship.
Wherein：Compound adsorbent refers to by beta-cyclodextrin and water-soluble chitosan by 5：1 mass ratio（g/g）Mixing and
The mixture obtained.
(4) the enzymolysis liquid taken off after hardship is spray-dried, obtains product casein phosphopeptide.
Wherein spray drying condition is the same as embodiment 1.
Claims (2)
1. a kind of beta-cyclodextrin and chitosan take off bitter casein phosphopeptide preparation method, include the following steps：
(1) be added the NaOH solution of a concentration of 1mol/L in casein, it is agitated uniformly after, obtain the junket that mass concentration is 15%
Protein solution；
(2) in the casein solution plus the hydrochloric acid tune pH value of a concentration of 0.1mol/L is to after 5.5 ~ 6.5, by initial casein protein
Papain is added in the 0.4 ~ 0.8% of amount, the enzymolysis of 140 ~ 160min of progress in 55 ~ 65 DEG C of waters bath with thermostatic control, after the completion of enzymolysis
Then at 90 ~ 100 DEG C of 15 ~ 25min of enzyme deactivation, enzymolysis liquid is obtained through natural cooling；
(3) in the enzymolysis liquid plus the hydrochloric acid tune pH value of a concentration of 0.1mol/L is to after 6.5 ~ 7.5, by initial casein quality
15 ~ 25% are added compound adsorbent, and stirring and adsorbing takes off 50 ~ 70min of hardship under 35 ~ 45 DEG C of water-baths, obtain the enzymolysis liquid after de- hardship；
The compound adsorbent refers to by beta-cyclodextrin and water-soluble chitosan by 4 ~ 6：The mixture that 1 mass ratio is obtained by mixing；
(4) the enzymolysis liquid after the de- hardship is spray-dried, obtains product casein phosphopeptide.
2. a kind of beta-cyclodextrin as described in claim 1 and chitosan take off bitter casein phosphopeptide preparation method, feature
It is：(4) the middle condition being spray-dried refers to steam pressure ＞ 0.75MPa, 160 DEG C of tower body inlet air temperature ＞, in tower to the step
Temperature is 65 ~ 75 DEG C, 63 DEG C of tower body temperature of outgoing air ＞, and negative pressure is -20 ~ -100Pa in tower, and high pressure pump pressure is 10 ~ 25MPa.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112841390A (en) * | 2021-02-04 | 2021-05-28 | 中国海洋大学 | Euphausia superba flavor peptide powder and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101260397A (en) * | 2008-04-28 | 2008-09-10 | 浙江省农业科学院 | Immobilized protease and its application method in preparing milk casein peptide |
| CN103571905A (en) * | 2013-10-30 | 2014-02-12 | 广州绿萃生物科技有限公司 | Preparation method of high-purity casein phosphopeptide |
| US20150093459A1 (en) * | 2004-02-23 | 2015-04-02 | Texas A&M University System | Bioactive complex compositions and methods of use thereof |
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2018
- 2018-04-02 CN CN201810283751.7A patent/CN108531531A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20150093459A1 (en) * | 2004-02-23 | 2015-04-02 | Texas A&M University System | Bioactive complex compositions and methods of use thereof |
| CN101260397A (en) * | 2008-04-28 | 2008-09-10 | 浙江省农业科学院 | Immobilized protease and its application method in preparing milk casein peptide |
| CN103571905A (en) * | 2013-10-30 | 2014-02-12 | 广州绿萃生物科技有限公司 | Preparation method of high-purity casein phosphopeptide |
Non-Patent Citations (2)
| Title |
|---|
| NAKANO T等: "Preparation of micellar calcium phosphate-casein phosphopeptide complex from rennet casein using ultrafiltration", 《MILK SCIENCE》 * |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112841390A (en) * | 2021-02-04 | 2021-05-28 | 中国海洋大学 | Euphausia superba flavor peptide powder and preparation method thereof |
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