CN106319011A - Method for preparing compound amino acid chelated calcium by sea cucumber intestine enzymatic hydrolysate - Google Patents
Method for preparing compound amino acid chelated calcium by sea cucumber intestine enzymatic hydrolysate Download PDFInfo
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- CN106319011A CN106319011A CN201610685873.XA CN201610685873A CN106319011A CN 106319011 A CN106319011 A CN 106319011A CN 201610685873 A CN201610685873 A CN 201610685873A CN 106319011 A CN106319011 A CN 106319011A
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- Prior art keywords
- intestinum stichopi
- stichopi japonici
- amino acid
- enzymolysis
- compound amino
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- -1 compound amino acid Chemical class 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 24
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 229910052791 calcium Inorganic materials 0.000 title claims abstract description 18
- 239000011575 calcium Substances 0.000 title claims abstract description 18
- 241000251511 Holothuroidea Species 0.000 title abstract description 7
- 210000000936 intestine Anatomy 0.000 title abstract 4
- 230000002255 enzymatic effect Effects 0.000 title abstract 2
- 239000000413 hydrolysate Substances 0.000 title abstract 2
- 238000000108 ultra-filtration Methods 0.000 claims abstract description 26
- 238000001728 nano-filtration Methods 0.000 claims abstract description 18
- 238000003756 stirring Methods 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- 150000003751 zinc Chemical class 0.000 claims abstract description 8
- 239000007787 solid Substances 0.000 claims abstract description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 34
- IHBCFWWEZXPPLG-UHFFFAOYSA-N [Ca].[Zn] Chemical compound [Ca].[Zn] IHBCFWWEZXPPLG-UHFFFAOYSA-N 0.000 claims description 31
- 102000004190 Enzymes Human genes 0.000 claims description 29
- 108090000790 Enzymes Proteins 0.000 claims description 29
- 239000013522 chelant Substances 0.000 claims description 28
- 239000000243 solution Substances 0.000 claims description 23
- 239000007788 liquid Substances 0.000 claims description 20
- 108091005804 Peptidases Proteins 0.000 claims description 18
- 239000004365 Protease Substances 0.000 claims description 18
- 102100037486 Reverse transcriptase/ribonuclease H Human genes 0.000 claims description 18
- 239000012528 membrane Substances 0.000 claims description 15
- 239000012466 permeate Substances 0.000 claims description 15
- 239000006228 supernatant Substances 0.000 claims description 15
- 229920001503 Glucan Polymers 0.000 claims description 12
- 230000000694 effects Effects 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 102000004882 Lipase Human genes 0.000 claims description 11
- 108090001060 Lipase Proteins 0.000 claims description 11
- 239000004367 Lipase Substances 0.000 claims description 11
- 235000019421 lipase Nutrition 0.000 claims description 11
- 238000010792 warming Methods 0.000 claims description 11
- 238000000502 dialysis Methods 0.000 claims description 10
- 239000012530 fluid Substances 0.000 claims description 10
- 235000013305 food Nutrition 0.000 claims description 10
- 239000000725 suspension Substances 0.000 claims description 9
- 108090000145 Bacillolysin Proteins 0.000 claims description 8
- 102000035092 Neutral proteases Human genes 0.000 claims description 8
- 108091005507 Neutral proteases Proteins 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 8
- 150000001875 compounds Chemical class 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 6
- 108090000765 processed proteins & peptides Proteins 0.000 claims description 6
- 239000012141 concentrate Substances 0.000 claims description 5
- 235000009508 confectionery Nutrition 0.000 claims description 5
- 238000010790 dilution Methods 0.000 claims description 5
- 239000012895 dilution Substances 0.000 claims description 5
- RWSXRVCMGQZWBV-WDSKDSINSA-N glutathione Chemical compound OC(=O)[C@@H](N)CCC(=O)N[C@@H](CS)C(=O)NCC(O)=O RWSXRVCMGQZWBV-WDSKDSINSA-N 0.000 claims description 5
- 229960003180 glutathione Drugs 0.000 claims description 5
- 235000003969 glutathione Nutrition 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 230000002779 inactivation Effects 0.000 claims description 5
- 230000004044 response Effects 0.000 claims description 5
- 238000012423 maintenance Methods 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 4
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- 239000004246 zinc acetate Substances 0.000 claims description 3
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 2
- 229960001763 zinc sulfate Drugs 0.000 claims description 2
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 2
- 235000016709 nutrition Nutrition 0.000 abstract description 8
- 239000012535 impurity Substances 0.000 abstract description 7
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 6
- 238000010521 absorption reaction Methods 0.000 abstract description 5
- 239000003513 alkali Substances 0.000 abstract 1
- 238000005119 centrifugation Methods 0.000 abstract 1
- 238000001816 cooling Methods 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 238000000265 homogenisation Methods 0.000 abstract 1
- 239000004615 ingredient Substances 0.000 abstract 1
- 230000035484 reaction time Effects 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- 235000001014 amino acid Nutrition 0.000 description 30
- 150000001413 amino acids Chemical class 0.000 description 10
- 238000002360 preparation method Methods 0.000 description 6
- 230000000050 nutritive effect Effects 0.000 description 5
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 4
- TWNIBLMWSKIRAT-VFUOTHLCSA-N levoglucosan Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@H]2CO[C@@H]1O2 TWNIBLMWSKIRAT-VFUOTHLCSA-N 0.000 description 4
- 230000035764 nutrition Effects 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 239000000796 flavoring agent Substances 0.000 description 3
- 235000019634 flavors Nutrition 0.000 description 3
- 230000000968 intestinal effect Effects 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000011701 zinc Substances 0.000 description 3
- 229910052725 zinc Inorganic materials 0.000 description 3
- QCVGEOXPDFCNHA-UHFFFAOYSA-N 5,5-dimethyl-2,4-dioxo-1,3-oxazolidine-3-carboxamide Chemical compound CC1(C)OC(=O)N(C(N)=O)C1=O QCVGEOXPDFCNHA-UHFFFAOYSA-N 0.000 description 2
- 241000965254 Apostichopus japonicus Species 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 102000002322 Egg Proteins Human genes 0.000 description 2
- 108010000912 Egg Proteins Proteins 0.000 description 2
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 description 2
- 239000002775 capsule Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 238000011033 desalting Methods 0.000 description 2
- 235000014103 egg white Nutrition 0.000 description 2
- 210000000969 egg white Anatomy 0.000 description 2
- 230000036039 immunity Effects 0.000 description 2
- 238000002372 labelling Methods 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 229910052720 vanadium Inorganic materials 0.000 description 2
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 2
- 241000040710 Chela Species 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000000259 anti-tumor effect Effects 0.000 description 1
- 230000000840 anti-viral effect Effects 0.000 description 1
- 230000010100 anticoagulation Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 229940106635 calcium amino acid chelate Drugs 0.000 description 1
- 210000000078 claw Anatomy 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 208000000718 duodenal ulcer Diseases 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 230000036737 immune function Effects 0.000 description 1
- 210000000987 immune system Anatomy 0.000 description 1
- 210000003734 kidney Anatomy 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003204 osmotic effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000001766 physiological effect Effects 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 229920001184 polypeptide Polymers 0.000 description 1
- 102000004196 processed proteins & peptides Human genes 0.000 description 1
- 235000018102 proteins Nutrition 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007634 remodeling Methods 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 235000014102 seafood Nutrition 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 210000002784 stomach Anatomy 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- WQSRXNAKUYIVET-UHFFFAOYSA-N sulfuric acid;zinc Chemical compound [Zn].OS(O)(=O)=O WQSRXNAKUYIVET-UHFFFAOYSA-N 0.000 description 1
- 230000003867 tiredness Effects 0.000 description 1
- 208000016255 tiredness Diseases 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
- RZLVQBNCHSJZPX-UHFFFAOYSA-L zinc sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Zn+2].[O-]S([O-])(=O)=O RZLVQBNCHSJZPX-UHFFFAOYSA-L 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
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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
- C07K1/107—General methods for the preparation of peptides, i.e. processes for the organic chemical preparation of peptides or proteins of any length by chemical modification of precursor peptides
-
- 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
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- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Molecular Biology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Genetics & Genomics (AREA)
- Engineering & Computer Science (AREA)
- Wood Science & Technology (AREA)
- Zoology (AREA)
- Biochemistry (AREA)
- Bioinformatics & Cheminformatics (AREA)
- General Engineering & Computer Science (AREA)
- Biotechnology (AREA)
- Microbiology (AREA)
- Analytical Chemistry (AREA)
- Biophysics (AREA)
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- Proteomics, Peptides & Aminoacids (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
Abstract
The invention provides a method for preparing compound amino acid chelated calcium by sea cucumber intestine enzymatic hydrolysate. The method comprises the following steps: (1) sea cucumber intestine pretreatment; (2) sea cucumber intestine homogenization; (3) primary enzymolysis; (4) secondary enzymolysis; (5) ultrafiltration; (6) nanofiltration; (7) chelating: under the condition of 35-45 DEG C, appropriate amounts of soluble zinc salt and inorganic calcium are added to a nanofiltration concentrated solution while stirring, the mass ratio of the soluble zinc salt and the inorganic calcium is 1:(2-1), at the same time, appropriate amount of alkali is added slowly to adjust the pH to be 7.0-7.5, the reaction time is 2-3 h, the system pH value is kept stable in the reaction process, cooling and centrifugation are performed after reaction, and the compound amino acid chelated calcium is prepared after a solid content is subjected to washing, drying and smashing. The compound amino acid chelated calcium is rich in nutritional ingredient, easy to absorb and utilize, high in absorption and utilization, low in impurity and heavy metal content and high in nutritional value.
Description
Technical field
The present invention relates to a kind of method preparing compound amino acid chelate calcium zinc.
Background technology
Stichopus japonicus belongs to one of precious seafood, and it is internal contains more than the 50 kind of nutritional labeling useful to human physiological activity, wherein
Protein content is higher, trace element abundant species, it is possible to continuity human senility, tonifies Qi of the kidney, essence-replenishing and marrow-strengthening, allaying tiredness,
Have more anticoagulation, antitumor, antibacterial, antiviral and improve the effect of immunity.In recent years, the enterprise of processing sea cucumber the most more comes
The most, contained in the leftover bits and pieces-Intestinum Stichopi japonici during Holothurian machining nutritional labelings, no less than body wall.Its dry intestinal rate Han vanadium
It is 12 parts of million parts, higher than the rate Han vanadium in its body 3 times.It has effect of warming middle-Jiao and tonifying deficiency pain relieving, can treat stomach and ten
Two Duodenalulcers.
The utilization of Intestinum Stichopi japonici resource day by day causes attention, after Intestinum Stichopi japonici is manually removed sand by a lot of enterprises, cleans, cold air drying
Dry or lyophilization, then polishing or micronizing, make capsule product.But Intestinum Stichopi japonici is not done life by this kind of capsule product
Thing processes, and absorption rate is low, and nutritive value is had a greatly reduced quality.It addition, there is also in the process of raw material: manually going of Intestinum Stichopi japonici
Husky mud efficiency is low and silt is thorough, thorough with water cleaning, desalting, causes what content of beary metal and salinity in product exceeded standard to ask
Topic.
Calcium amino acid chelate and zinc are a kind of calcium and the zinc structures that calcium and zinc ion are entrenched in two amino acid moleculars centres
Form.Two amino acid moleculars clamp a calcium or zinc ion as " crab claw ", form overstable chelate structure, then pass through
Aminoacid passage is transported to calcium and zinc in blood, makes calcium, zinc be absorbed by the body together with aminoacid, can be greatly improved absorption
Rate.The present invention provides a kind of method that Intestinum Stichopi japonici enzymolysis solution prepares compound amino acid chelate calcium zinc.
Summary of the invention
It is an object of the invention to solve the deficiencies in the prior art, it is provided that a kind of side preparing compound amino acid chelate calcium zinc
Method, compound amino acid chelate calcium zinc nutrition composition prepared by the method enriches, it is easy to absorb, impurity and content of beary metal
Low.
The technical solution adopted for the present invention to solve the technical problems is:
Intestinum Stichopi japonici enzymolysis solution prepares the method for compound amino acid chelate calcium zinc, and described method comprises the steps:
(1) Intestinum Stichopi japonici pretreatment: collect fresh Intestinum Stichopi japonici, uses pretreating agent A and B to carry out pretreatment, pretreating agent A
For the water-insoluble glucan suspension of mass fraction 8-12%, described pretreating agent B is the reduction of mass fraction 0.5-1.5%
Type glutathion aqueous solution, concrete pretreatment operation is: first using pretreating agent A pretreatment 1-2h under room temperature, solid-liquid ratio is
1:2-3, then under room temperature, stir pretreatment 2-3h with pretreating agent B, then standing 45min-1h, solid-liquid ratio is 1:1-2, or
Pretreating agent A is mixed homogeneously with volume ratio 1:1 with pretreating agent B, is subsequently adding fresh Intestinum Stichopi japonici, under room temperature at stirring
Reason 2-2.5h, then stands 0.5-1h, and solid-liquid ratio 1:2, after pretreatment, solid-liquid separation is standby；
Rich in silt, heavy metal, salinity in Intestinum Stichopi japonici, want to obtain the compound amino acid chelate calcium zinc of high-quality, need
Fully removing above-mentioned impurity, the design concept of the present invention is as follows: (1) water-insoluble glucan suspension is the water suspendible of macromole
Liquid, macromole glucosan itself has the effect of flocculation of reuniting, and can fully adsorb or the mud that flocculates in Intestinum Stichopi japonici and heavy metal
The removal effect of the impurity such as impurity, especially heavy metal is splendid, after using glucosan suspension pretreating agent pretreatment, and Stichopus japonicus
The extensibility of intestinal is the most excellent, and follow-up homogenizing, the effect of enzymolysis are substantially improved, it addition, glucosan safety non-toxic, the glucosan of residual
There is the effect increasing immunity, improving immunologic function on the contrary, it is provided that the nutritive value of compound amino acid chelate calcium zinc；(2) reduction
Type glutathion aqueous solution has the function of good activating cell and tissue, can improve active oxygen in cell or tissue and
Osmotic pressure, maintains Intestinum Stichopi japonici cell and the fresh and healthy state of tissue long period, is substantially improved the effect of follow-up ferment treatment, paddy
Guang sweet peptide also safety non-toxic, the glutathion of residual has the function improving immune system, removing toxic substances on the contrary, improves aminoacids complex chela
Close the nutritive value of calcium zinc, improve the quality of finished product, by Heavy Metal Pollution wind that may be present in compound amino acid chelate calcium zinc
Danger reduces further or eliminates.
(2) homogenizing of Intestinum Stichopi japonici: step (1) pretreated Intestinum Stichopi japonici is placed in high pressure homogenizer, adds appropriate
Water, carries out homogenizing, obtains Intestinum Stichopi japonici homogenizing fluid；
(3) primary enzymolysis: step (2) gained Intestinum Stichopi japonici homogenizing fluid is warming up to 35-45 DEG C, adjusts pH value to 6.5-7.5, adds
Enter appropriate food-grade lipase, stir, enzymolysis 0.5-1h, Intestinum Stichopi japonici is carried out defat, then heats to 75 DEG C of inactivation 3-
5min, is subsequently cooled to room temperature and stands 1-2h, remove supernatant oil layer；The fat in Intestinum Stichopi japonici is removed by lipase enzymolysis
Fat, can improve the quality of compound amino acid chelate calcium zinc, extends the shelf-life of compound amino acid chelate calcium zinc.
(4) secondary enzymolysis: the primary enzymolysis liquid after step (3) being processed is warming up to 40-50 DEG C, adjusts pH value 6.5-7.0, adds
Entering appropriate complex food level protease hydrolyzed 2-3h, described complex food level protease is by compound protease and neutral egg
White enzyme composition, enzymolysis post-heating to 80 DEG C enzyme denaturing 10-15min, it is then centrifuged for separating, obtains Intestinum Stichopi japonici secondary enzymolysis supernatant；Logical
Cross enzymolysis and the protein in Intestinum Stichopi japonici is fully degraded into aminoacid and micromolecule polypeptide, it is simple to compound amino acid chelate calcium zinc
Absorbing and utilize, utilization rate is high, is of high nutritive value.
(5) ultrafiltration: the ultrafilter membrane ultrafiltration that Intestinum Stichopi japonici secondary enzymolysis supernatant molecular cut off is 5000-8000Da is obtained
Ultrafiltration permeate；
(6) nanofiltration: diluted with appropriate pure water by the ultrafiltration permeate of step (6), then carries out dialysis by NF membrane and concentrates,
The dialysis of ultrafiltration permeate be concentrated into dilution 0.25-0.35 times of front volume nanofiltration concentrated solution, described NF membrane retain molecule
Amount is 150-300Da；By nanofiltration to compound amino acid chelate calcium zinc desalting processing, it is thus achieved that compound amino acid chelate calcium zinc salt
Divide low, in good taste；
(7) chelating: under conditions of 35-45 DEG C, while stirring toward nanofiltration concentrated solution adds appropriate soluble zinc salt and
Inorganic calcium, being slowly added appropriate bases regulation system pH is 7.0～7.5, and the response time is 2～3h, maintains in course of reaction
System pH is stable, and reaction cools down after terminating, is centrifuged, and solid content is scrubbed, dry and pulverizes, and prepares compound amino acid chelate calcium
Zinc.
Preferably, during described soluble zinc salt is zinc sulfate and crystalline hydrate thereof or zinc acetate and crystalline hydrate thereof
Any one or a few, the addition mass ratio of soluble zinc salt and inorganic calcium is 1～2:1.
Preferably, in step (1), pretreating agent A is the water-insoluble glucan suspension of mass fraction 10%, described pre-
Inorganic agent B is the reduced glutathion aqueous solution of mass fraction 1.0%.
Preferably, temperature 35-65 DEG C of step (2) mesohigh homogenizing, pressure 120-400Mpa, circulates homogenizing at least two
Secondary.
Preferably, the enzyme work of described food-grade lipase is 20,000 U/g, and enzyme dosage is the 0.2-of fresh Intestinum Stichopi japonici quality
0.8%.
Preferably, in described step (4), the enzyme activity of compound protease and neutral protease is than for 2-3:1, and enzyme is total
Consumption is the 0.6-1.0% of fresh Intestinum Stichopi japonici quality.
The invention has the beneficial effects as follows: compound amino acid chelate calcium zinc nutrition composition prepared by the present invention enriches, it is easy to inhale
Receiving and utilize, absorption rate is high, and impurity and content of beary metal are low, are of high nutritive value.
Detailed description of the invention
Below by specific embodiment, technical scheme is described in further detail.
Embodiment 1:
Intestinum Stichopi japonici enzymolysis solution prepares the preparation method of the method for compound amino acid chelate calcium zinc, described preparation method include as
Lower step:
(1) Intestinum Stichopi japonici pretreatment: collect fresh Intestinum Stichopi japonici, uses pretreating agent A and B to carry out pretreatment, pretreating agent A
For the water-insoluble glucan suspension of mass fraction 8%, described pretreating agent B is the reduced form paddy Guang of mass fraction 0.5%
Sweet peptide aqueous solution, concrete pretreatment operation is: first using pretreating agent A pretreatment 2h under room temperature, solid-liquid ratio is 1:2, then uses
Pretreating agent B stirs pretreatment 2h under room temperature, then stands 45minh, and solid-liquid ratio is 1:1；
(2) homogenizing of Intestinum Stichopi japonici: step (1) pretreated Intestinum Stichopi japonici is placed in high pressure homogenizer, adds appropriate
Water, carries out homogenizing, obtains Intestinum Stichopi japonici homogenizing fluid, high pressure homogenize temperature 35-45 DEG C, pressure 120Mpa, circulation homogenizing 3 twice；
(3) primary enzymolysis: step (2) gained Intestinum Stichopi japonici homogenizing fluid is warming up to 35 DEG C, adjusts pH value to 6.5, adds appropriate
Food-grade lipase, stirs, enzymolysis 1h, and Intestinum Stichopi japonici is carried out defat, then heats to 75 DEG C of inactivation 3min, then cools down
Standing 1h to room temperature, remove supernatant oil layer, the enzyme work of described food-grade lipase is 20,000 U/g, and enzyme dosage is new fresh sea cucumber
The 0.2% of intestinal quality；
(4) secondary enzymolysis: the primary enzymolysis liquid after step (3) being processed is warming up to 40 DEG C, adjusts pH value 6.5, adds appropriate
Complex food level protease hydrolyzed 2h, described complex food level protease is by compound protease and neutral protease group
Become, enzymolysis post-heating to 80 DEG C enzyme denaturing 10min, be then centrifuged for separating, obtain Intestinum Stichopi japonici secondary enzymolysis supernatant, composite flavor albumen
The enzyme activity of enzyme and neutral protease is than for 2:1, and the total consumption of enzyme is the 0.6% of fresh Intestinum Stichopi japonici quality；
(5) ultrafiltration: the ultrafilter membrane ultrafiltration that Intestinum Stichopi japonici secondary enzymolysis supernatant molecular cut off is 5000-2000Da is obtained
Ultrafiltration permeate；
(6) nanofiltration: diluted with appropriate pure water by the ultrafiltration permeate of step (6), then carries out dialysis by NF membrane and concentrates,
The dialysis of ultrafiltration permeate be concentrated into dilution 0.25 times of front volume nanofiltration concentrated solution, the molecular cut off of described NF membrane is
150-200Da；
(7) chelating: under conditions of 35 DEG C, adds moderate amount of sulfuric acid zinc and inorganic calcium while stirring in nanofiltration concentrated solution,
The two mass ratio is 1:1, and being slowly added appropriate bases regulation system pH is 7.0～7.1, and the response time is 3h, course of reaction
Middle maintenance system pH stable, reaction cools down after terminating, is centrifuged, and solid content is scrubbed, dry and pulverizes, and prepares aminoacids complex
Chelating calcium zinc.
Embodiment 2
Intestinum Stichopi japonici enzymolysis solution prepares the preparation method of the method for compound amino acid chelate calcium zinc, described preparation method include as
Lower step:
(1) Intestinum Stichopi japonici pretreatment: collect fresh Intestinum Stichopi japonici, uses pretreating agent A and B to carry out pretreatment, pretreating agent A
For the water-insoluble glucan suspension of mass fraction 12%, described pretreating agent B is the reduced form paddy Guang of mass fraction 1.5%
Sweet peptide aqueous solution, concrete pretreatment operation is: first using pretreating agent A pretreatment 1h under room temperature, solid-liquid ratio is 1:3, then uses
Pretreating agent B stirs pretreatment 3h under room temperature, then stands 45min, and solid-liquid ratio is 1:1；
(2) homogenizing of Intestinum Stichopi japonici: step (1) pretreated Intestinum Stichopi japonici is placed in high pressure homogenizer, adds appropriate
Water, carries out homogenizing, obtains Intestinum Stichopi japonici homogenizing fluid, temperature 60-65 DEG C of high pressure homogenize, pressure 400Mpa, circulation homogenizing twice；
(3) primary enzymolysis: step (2) gained Intestinum Stichopi japonici homogenizing fluid is warming up to 45 DEG C, adjusts pH value to 7.5, adds appropriate
Food-grade lipase, stirs, enzymolysis 1h, and Intestinum Stichopi japonici is carried out defat, then heats to 75 DEG C of inactivation 5min, then cools down
Stand 2h to room temperature, remove supernatant oil layer；The enzyme work of food-grade lipase is 20,000 U/g, and enzyme dosage is fresh Intestinum Stichopi japonici matter
The 0.8% of amount；
(4) secondary enzymolysis: the primary enzymolysis liquid after step (3) being processed is warming up to 40-50 DEG C, adjusts pH value 6.5-7.0, adds
Entering appropriate complex food level protease hydrolyzed 2-3h, described complex food level protease is by compound protease and neutral egg
White enzyme composition, enzymolysis post-heating to 80 DEG C enzyme denaturing 10-15min, it is then centrifuged for separating, obtains Intestinum Stichopi japonici secondary enzymolysis supernatant；Multiple
Closing the enzyme activity of flavor protease and neutral protease ratio for 3:1, the total consumption of enzyme is the 1.0% of fresh Intestinum Stichopi japonici quality；
(5) ultrafiltration: the ultrafilter membrane ultrafiltration that Intestinum Stichopi japonici secondary enzymolysis supernatant molecular cut off is 6000-8000Da is obtained
Ultrafiltration permeate；
(6) nanofiltration: diluted with appropriate pure water by the ultrafiltration permeate of step (6), then carries out dialysis by NF membrane and concentrates,
The dialysis of ultrafiltration permeate be concentrated into dilution 0.35 times of front volume nanofiltration concentrated solution, the molecular cut off of described NF membrane is
200-300Da；
(7) chelating: under conditions of 45 DEG C, while stirring toward adding appropriate zinc sulphate heptahydrate and inorganic in nanofiltration concentrated solution
Calcium, the two mass ratio is 1:1, and being slowly added appropriate bases regulation system pH is 7.4～7.5, and the response time is 2h, reacts
Maintenance system pH stable in journey, reaction cools down after terminating, is centrifuged, and solid content is scrubbed, dry and pulverizes, and prepares compounded amino
Acid chelating calcium zinc.
Embodiment 3:
Intestinum Stichopi japonici enzymolysis solution prepares the preparation method of the method for compound amino acid chelate calcium zinc, described preparation method include as
Lower step:
(1) Intestinum Stichopi japonici pretreatment: collect fresh Intestinum Stichopi japonici, uses pretreating agent A and B to carry out pretreatment, pretreating agent A
For the water-insoluble glucan suspension of mass fraction 10%, described pretreating agent B is the reduced form paddy Guang of mass fraction 1.0%
Sweet peptide aqueous solution, concrete pretreatment operation is: is mixed homogeneously with volume ratio 1:1 with pretreating agent B by pretreating agent A, then adds
Enter fresh Intestinum Stichopi japonici, stir process 2.5h under room temperature, then stand 1h, solid-liquid ratio 1:2, solid-liquid separation after pretreatment
Standby；
(2) homogenizing of Intestinum Stichopi japonici: step (1) pretreated Intestinum Stichopi japonici is placed in high pressure homogenizer, adds appropriate
Water, carries out homogenizing, obtains Intestinum Stichopi japonici homogenizing fluid, temperature 40-45 DEG C of high pressure homogenize, pressure 180Mpa, circulation homogenizing three times；
(3) primary enzymolysis: step (2) gained Intestinum Stichopi japonici homogenizing fluid is warming up to 40 DEG C, adjusts pH value to 7.0, adds appropriate
Food-grade lipase, stirs, enzymolysis 1h, and Intestinum Stichopi japonici is carried out defat, then heats to 75 DEG C of inactivation 5min, then cools down
Stand 2h to room temperature, remove supernatant oil layer；The enzyme work of food-grade lipase is 20,000 U/g, and enzyme dosage is fresh Intestinum Stichopi japonici matter
The 0.5% of amount；
(4) secondary enzymolysis: the primary enzymolysis liquid after step (3) being processed is warming up to 45 DEG C, adjusts pH value 6.8, adds appropriate
Complex food level protease hydrolyzed 2.5h, described complex food level protease is by compound protease and neutral protease group
Become, enzymolysis post-heating to 80 DEG C enzyme denaturing 12min, be then centrifuged for separating, obtain Intestinum Stichopi japonici secondary enzymolysis supernatant；Composite flavor albumen
The enzyme activity of enzyme and neutral protease is than for 2.5:1, and the total consumption of enzyme is the 0.75% of fresh Intestinum Stichopi japonici quality；
(5) ultrafiltration: the ultrafilter membrane ultrafiltration that Intestinum Stichopi japonici secondary enzymolysis supernatant molecular cut off is 6000Da is obtained ultrafiltration
Permeate；
(6) nanofiltration: diluted with appropriate pure water by the ultrafiltration permeate of step (6), then carries out dialysis by NF membrane and concentrates,
The dialysis of ultrafiltration permeate be concentrated into dilution 0.3 times of front volume nanofiltration concentrated solution, the molecular cut off of described NF membrane is
220Da；
(7) chelating: under conditions of 40 DEG C, add appropriate zinc acetate and inorganic calcium in nanofiltration concentrated solution while stirring,
The two mass ratio is 3:2, and being slowly added appropriate bases regulation system pH is 7.2～7.3, and the response time is 2.5h, reacts
Maintenance system pH stable in journey, reaction cools down after terminating, is centrifuged, and solid content is scrubbed, dry and pulverizes, and prepares compounded amino
Acid chelating calcium zinc.
Compound amino acid chelate calcium zinc nutrition composition prepared by the present invention enriches, and amino acid nitrogen content is the highest, nutrition
Being worth height, it is easy to absorb, absorption rate is high, and impurity content is low, and heavy metal does not detects.Embodiment described above is simply
The one of the present invention preferably scheme, not makees any pro forma restriction, described in claim to the present invention
Technical scheme on the premise of also have other variant and remodeling.
Claims (6)
1. the method that Intestinum Stichopi japonici enzymolysis solution prepares compound amino acid chelate calcium zinc, it is characterised in that: described method includes walking as follows
Rapid:
(1) Intestinum Stichopi japonici pretreatment: collect fresh Intestinum Stichopi japonici, uses pretreating agent A and B to carry out pretreatment, and pretreating agent A is matter
The water-insoluble glucan suspension of amount mark 8-12%, described pretreating agent B is the reduced form paddy of mass fraction 0.5-1.5%
Guang sweet peptide aqueous solution, concrete pretreatment operation is: first using pretreating agent A pretreatment 1-2h under room temperature, solid-liquid ratio is 1:2-
3, then under room temperature, stir pretreatment 2-3h with pretreating agent B, then standing 45min-1h, solid-liquid ratio is 1:1-2, or will be pre-
Inorganic agent A is mixed homogeneously with volume ratio 1:1 with pretreating agent B, is subsequently adding fresh Intestinum Stichopi japonici, stir process 2-under room temperature
2.5h, then stands 0.5-1h, and solid-liquid ratio 1:2, after pretreatment, solid-liquid separation is standby；
(2) homogenizing of Intestinum Stichopi japonici: step (1) pretreated Intestinum Stichopi japonici is placed in high pressure homogenizer, adds appropriate water, enter
Row homogenizing, obtains Intestinum Stichopi japonici homogenizing fluid；
(3) primary enzymolysis: step (2) gained Intestinum Stichopi japonici homogenizing fluid is warming up to 35-45 DEG C, adjusts pH value to 6.5-7.5, adds suitable
Amount food-grade lipase, stirs, and enzymolysis 0.5-1h carries out defat to Intestinum Stichopi japonici, then heats to 75 DEG C of inactivation 3-5min,
It is subsequently cooled to room temperature and stands 1-2h, remove supernatant oil layer；
(4) secondary enzymolysis: the primary enzymolysis liquid after step (3) being processed is warming up to 40-50 DEG C, adjusts pH value 6.5-7.0, adds suitable
The complex food level protease hydrolyzed 2-3h of amount, described complex food level protease is by compound protease and neutral protease
Composition, enzymolysis post-heating to 80 DEG C enzyme denaturing 10-15min, it is then centrifuged for separating, obtains Intestinum Stichopi japonici secondary enzymolysis supernatant；
(5) ultrafiltration: the ultrafilter membrane ultrafiltration that Intestinum Stichopi japonici secondary enzymolysis supernatant molecular cut off is 5000-8000Da is obtained ultrafiltration
Permeate；
(6) nanofiltration: diluted with appropriate pure water by the ultrafiltration permeate of step (6), then carries out dialysis by NF membrane and concentrates, ultrafiltration
Permeate dialysis be concentrated into dilution 0.25-0.35 times of front volume nanofiltration concentrated solution, the molecular cut off of described NF membrane is
150-300Da；
(7) chelating: under conditions of 35-45 DEG C, while stirring toward adding appropriate soluble zinc salt and inorganic in nanofiltration concentrated solution
Calcium, being slowly added appropriate bases regulation system pH is 7.0～7.5, and the response time is 2～3h, maintenance system in course of reaction
PH stable, reaction cools down after terminating, is centrifuged, and solid content is scrubbed, dry and pulverizes, and prepares compound amino acid chelate calcium zinc.
The method that Intestinum Stichopi japonici enzymolysis solution the most according to claim 1 prepares compound amino acid chelate calcium zinc, it is characterised in that:
Described soluble zinc salt be in zinc sulfate and crystalline hydrate thereof or zinc acetate and crystalline hydrate thereof any one or several
Kind, the addition mass ratio of soluble zinc salt and inorganic calcium is 1～2:1.
The method that Intestinum Stichopi japonici enzymolysis solution the most according to claim 1 prepares compound amino acid chelate calcium zinc, it is characterised in that:
In step (1), pretreating agent A is the water-insoluble glucan suspension of mass fraction 10%, and described pretreating agent B is that quality is divided
The reduced glutathion aqueous solution of several 1.0%.
The method that Intestinum Stichopi japonici enzymolysis solution the most according to claim 1 prepares compound amino acid chelate calcium zinc, it is characterised in that:
Temperature 35-65 DEG C of step (2) mesohigh homogenizing, pressure 120-400Mpa, circulation homogenizing is at least twice.
The method that Intestinum Stichopi japonici enzymolysis solution the most according to claim 1 prepares compound amino acid chelate calcium zinc, it is characterised in that:
The enzyme work of described food-grade lipase is 20,000 U/g, and enzyme dosage is the 0.2-0.8% of fresh Intestinum Stichopi japonici quality.
The method that Intestinum Stichopi japonici enzymolysis solution the most according to claim 1 prepares compound amino acid chelate calcium zinc, it is characterised in that:
In described step (4), the enzyme activity of compound protease and neutral protease is than for 2-3:1, and the total consumption of enzyme is fresh Intestinum Stichopi japonici
The 0.6-1.0% of quality.
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|---|---|---|---|---|
| CN103230020A (en) * | 2013-04-15 | 2013-08-07 | 武汉工业学院 | Preparation method of protein short peptide chelated calcium |
| KR20150132704A (en) * | 2014-05-16 | 2015-11-26 | 시원해양 주식회사 | Extract of sea cucumber and sea urchin, preparing thereof, functional foods and cosmetics using the same |
| CN105325851A (en) * | 2015-11-26 | 2016-02-17 | 威海新异生物科技有限公司 | Trepang composite flour capable of nourishing kidney and strengthening essence, and tonifying Yang to cure impotence |
| CN105361153A (en) * | 2015-11-18 | 2016-03-02 | 山东省海洋资源与环境研究院 | Processing method of sea cucumber glycopeptides chelated calcium |
| CN105455145A (en) * | 2016-01-06 | 2016-04-06 | 威海特伦斯生物工程有限公司 | Selenium-enriched trepang pulp |
| CN105595224A (en) * | 2015-12-30 | 2016-05-25 | 威海力元海洋生物科技有限公司 | Sea cucumber dunaliella salina glucosan selenium preparation and preparation process |
-
2016
- 2016-08-17 CN CN201610685873.XA patent/CN106319011A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103230020A (en) * | 2013-04-15 | 2013-08-07 | 武汉工业学院 | Preparation method of protein short peptide chelated calcium |
| KR20150132704A (en) * | 2014-05-16 | 2015-11-26 | 시원해양 주식회사 | Extract of sea cucumber and sea urchin, preparing thereof, functional foods and cosmetics using the same |
| CN105361153A (en) * | 2015-11-18 | 2016-03-02 | 山东省海洋资源与环境研究院 | Processing method of sea cucumber glycopeptides chelated calcium |
| CN105325851A (en) * | 2015-11-26 | 2016-02-17 | 威海新异生物科技有限公司 | Trepang composite flour capable of nourishing kidney and strengthening essence, and tonifying Yang to cure impotence |
| CN105595224A (en) * | 2015-12-30 | 2016-05-25 | 威海力元海洋生物科技有限公司 | Sea cucumber dunaliella salina glucosan selenium preparation and preparation process |
| CN105455145A (en) * | 2016-01-06 | 2016-04-06 | 威海特伦斯生物工程有限公司 | Selenium-enriched trepang pulp |
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