CN101225104B - Method for preparing tilapia fishskin small molecular peptide chelate zinc salt - Google Patents
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- 108090000765 processed proteins & peptides Proteins 0.000 title claims abstract description 28
- 241000276707 Tilapia Species 0.000 title claims abstract description 20
- 150000003751 zinc Chemical class 0.000 title claims abstract description 12
- 239000013522 chelant Substances 0.000 title claims description 14
- 238000000034 method Methods 0.000 title abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000002360 preparation method Methods 0.000 claims abstract description 11
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims abstract description 10
- 229960001763 zinc sulfate Drugs 0.000 claims abstract description 10
- 229910000368 zinc sulfate Inorganic materials 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 6
- 238000000108 ultra-filtration Methods 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 238000012545 processing Methods 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 9
- 102000004196 processed proteins & peptides Human genes 0.000 claims description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- 239000000047 product Substances 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 102000004169 proteins and genes Human genes 0.000 claims description 6
- 108090000623 proteins and genes Proteins 0.000 claims description 6
- 238000011084 recovery Methods 0.000 claims description 6
- 239000000796 flavoring agent Substances 0.000 claims description 5
- 235000019634 flavors Nutrition 0.000 claims description 5
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- 239000011701 zinc Substances 0.000 description 32
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- 229910052725 zinc Inorganic materials 0.000 description 17
- 235000015961 tonic Nutrition 0.000 description 12
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- 241000251468 Actinopterygii Species 0.000 description 6
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- 239000002699 waste material Substances 0.000 description 4
- 238000003926 complexometric titration Methods 0.000 description 3
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- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
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- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 2
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 1
- FPIPGXGPPPQFEQ-UHFFFAOYSA-N 13-cis retinol Natural products OCC=C(C)C=CC=C(C)C=CC1=C(C)CCCC1(C)C FPIPGXGPPPQFEQ-UHFFFAOYSA-N 0.000 description 1
- 108090000145 Bacillolysin Proteins 0.000 description 1
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- 102100037486 Reverse transcriptase/ribonuclease H Human genes 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
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- CANRESZKMUPMAE-UHFFFAOYSA-L Zinc lactate Chemical compound [Zn+2].CC(O)C([O-])=O.CC(O)C([O-])=O CANRESZKMUPMAE-UHFFFAOYSA-L 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
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- ORZHVTYKPFFVMG-UHFFFAOYSA-N xylenol orange Chemical compound OC(=O)CN(CC(O)=O)CC1=C(O)C(C)=CC(C2(C3=CC=CC=C3S(=O)(=O)O2)C=2C=C(CN(CC(O)=O)CC(O)=O)C(O)=C(C)C=2)=C1 ORZHVTYKPFFVMG-UHFFFAOYSA-N 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
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- Peptides Or Proteins (AREA)
Abstract
The invention discloses a preparation method for tilapia skin small peptide chelating zinc salt, using the tilapia skin as materials, preparing the tilapia skin small peptide (TSP-II) by means of a combination of the enzyme method and the ultrafiltration method. The tilapia skin small peptide chelating zinc salt is prepared with tilapia skin small peptide liquor and zinc sulfate by a water bath heating method. The preparation method for the tilapia skin small peptide chelating zinc salt has the advantages of scientific and rational technique, easy operation, low cost, and providing a zinc supplement preparation easy to be absorbed.
Description
Technical field
The present invention relates to a kind of preparation method of tilapia fishskin small molecular peptide chelate zinc salt.
Background technology
Zinc is the essential trace element of animal, owing in vivo widely biochemical functions be called as " bioelement "., it can cause the generation of a series of untoward reaction and disease when lacking.Mainly show as: (1) skin lesion; (2) anorexia (with the sense of taste, the responsive variation of sense of smell); (3) cessation of growth cessation; (4) poor wound healing or protein metabolism are suppressed; (5) sexual hypofunction; (6) immunologic function changes; (7) night vision infringement, Vitamin A Metabolism changes; (8) diarrhoea; (9) depression; (10) deformity.At present, zn deficiencie is the urgency of a China and many developing countries public health problem to be solved, and the most of children of China, pregnant woman and patient exist the trophicity zn deficiencie to some extent.In order to improve these crowds' zinc nutrition situation, people have developed multiple zinc tonic.
First-generation zinc tonic is inorganic tonics such as zinc sulfate, and is simple in structure, cheap, but the zinc chloride that the reaction of itself and hydrochloric acid in gastric juice generates is the stronger etching reagent of toxicity, behind the clothes often with spinoffs such as gastrointestinal irritations; In addition, the biological value of inorganic tonic is lower.
S-generation zinc tonic is organic tonic, as: Zinc Gluconate, zinc lactate etc.Its performance is superior to first-generation zinc tonic, but absorbs not as good as third generation zinc tonic.
Third generation zinc tonic is zinc-amino acid chelate tonic and polypeptide chelate zinc tonic, and the absorption that this huge legendary turtle is closed zinc is through amino acid (little peptide) absorption approach, have be prone to absorb, characteristics such as, good stability low to external excretion rate, toxicity are little, biology utilization ratio height.
There are some researches show at present: the human protein of taking in is not only to absorb with amino acid whose form after the digestive ferment effect, more is the form absorption with little peptide, and the ratio that absorbs with the total free aminoacids form is very little.And the digestion of the amino acid of peptide specific ionization is faster, absorption is more.This shows that the biological value of peptide and nutritive value specific ionization amino acid are higher, so polypeptide chelate zinc tonic is the zinc supplementation focus of research and development at present.
No matter the fresh water fishery of China at home or in the water industry in the world, all has consequence and effect.So, the processing of fresh-water fishes is seemed particularly important, should pay attention to the processing of fishery products main part, make full use of the sub product part again, make no waste on the body of fish.China is tilapia producing country the biggest in the world, and YO accounts for the world and produces the half the of total amount per year.Along with riseing year by year of fresh fish sheet, frozen fish fillet and bar frozen fish export volume, a large amount of fish-skins, fish-bone, the first-class tankage of fish have been produced.These tankage not only can cause great waste if effectively do not utilize, and also can cause environmental pollution.
For the wasting of resources that solves leftovers of tilapia and problems such as a kind of preparation of zinc supplementation efficiently are provided; Characteristics and former study in conjunction with fish-skin protein-high; We are attempting the employing enzyme process and the ultrafiltration process coupling prepares fish-skin protein zymolyte ultrafiltrated, and fish-skin protein zymolyte ultrafiltrated and zinc sulfate are equipped with tilapia fishskin small molecular peptide chelate zinc with the heating in water bath legal system.High performance fishskin small molecular peptide chelate zinc salt is not only a kind of natural health functional food of favoring, and also is a kind of good food auxiliary material and foodstuff additive simultaneously, can be used for fields such as beverage, protective foods.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of tilapia fishskin small molecular peptide chelate zinc salt is to overcome the deficiency that traditional zinc supplementation preparation has side effects and be difficult for absorbing.
The present invention realizes that like this its preparation method is:
1, pre-treatment: the fish-skin after the cleaning soaks 1hr with the hydrochloric acid soln of 0.1mol/L and the sodium hydroxide solution of 0.1mol/L successively after degreasing.
2, water is carried: pretreated fish-skin is through washing to neutrality, and under 45 ℃ of conditions, behind the zero(ppm) water constant temperature homogenate 12hr with 10 times of volumes, suction filtration extracts supernatant.
3, enzymolysis:, adopt papoid and neutral protease to carry out enzymolysis, the relatively hydrolysis result of two kinds of enzymes, and definite optimum enzymolysis condition under certain condition.Optimum enzymolysis condition: temperature: 50 ℃-55 ℃, the pH value: 6.0, time: 2hr, enzyme concentration: 0.05%, the degree of hydrolysis under this enzymatic hydrolysis condition is 12.3%.
4, the enzyme that goes out: adopt 100 ℃, the 20min enzyme that goes out.
5, debitterize, decolour, take off flavor: adopt gac and composite decoloring agent (the gac yeast of 3g/L and Schardinger dextrins etc. mix) that enzymolysis solution is carried out debitterize, decolours, takes off flavor and handle respectively, relatively the effect of two kinds of methods.
6, filter: enzymolysis solution through debitterize, decolour, take off flavor and handle after, obtain clear liquid through 4000r/min centrifuging again.
7, IX: the ultrafiltrated of getting certain volume passes through 001*7 (732) strongly acidic styrene type cation exchange resin with the flow velocity of 8 times of column volume/h at normal temperatures; Collect effluent; Measure its nitrogen recovery; Again with the hydrolyzed solution behind the decationized Y sieve with the flow velocity of 8 times of column volume/h through 201*7 (717) strong basicity I type anionite-exchange resin, collect effluent, measure its nitrogen recovery and ratio of desalinization.
8, concentrate: use Rotary Evaporators, thickening temperature is 50 ℃, and evaporating solns is to thick.
9, ultrafiltration: select the tubular fibre material for use, the WP of ultrafiltration apparatus is 28psi, and the membrane permeation flux is 9.98LHM, and the uf processing time is 40min, and feeding temperature is 29 ℃, and material liquid pH value is 6.7.
10, chelating: TSP-II and zinc sulfate chelating, the chelating condition: with content of peptides in the TSP-II solution is index, is 3: 1 by itself and zinc sulfate mass ratio, 60 ℃ of constant temperature water baths, the pH value is 6, the reaction times is 1hr.Gained solution is separated out faint yellow thick fishskin polypeptide chelate zinc salt through absolute ethanol washing repeatedly, and the zinc sulfate chelation percent is 92.31%, and the inner complex yield is 28.39%.
11, measure chelation percent:
(1) accurately pipette chelating zinc liquid concentrator 10mL in the 100mL volumetric flask, constant volume shakes up.Total amount with EDTA complexometric titration trace element.
(2) pipette chelating zinc liquid concentrator 10mL in addition in the 100mL beaker, continue heating and be concentrated near doing.Add the 50mL absolute ethyl alcohol, after water-bath warm (a little less than body temperature) is fully stirred, spinning will precipitate and use water dissolution, be transferred in the 100mL volumetric flask, and constant volume shakes up.Content with EDTA complexometric titration chelated microelements.
EDTA complexometric titration
Accurately pipette the 25mL test solution in the 250mL Erlenmeyer flask, add 50mL water, dropping 2-3 drips xylenol orange and makes indicator, and with 0.02mol/L EDTA standard solution titration, solution colour is titration end point by the purplish red glassy yellow that becomes.
Chelation percent (%)=(total amount of the content/trace element of chelated microelements) * 100
＝(CV
1/CV
0)×100＝(V
1/V
0)×100
The concentration of C-EDTA solution, mol/L;
V
1The EDTA liquor capacity that-titration chelated microelements is consumed, mL;
V
0The EDTA liquor capacity that total amount consumed of-titration trace element, mL.
12, alcohol is washed: inner complex absolute ethanol washing 2-3 time.
13, oven dry: ethanol is washed back inner complex 80 ℃ of dry 30min of constant temperature in the electric heating constant temperature air dry oven and is promptly got product.
14, measure the inner complex yield:
The yield of small molecular peptide chelate zinc salt (%)=W
1/ W
0* 100
W
1: small molecular peptide chelate zinc salt gross weight (g);
W
0: reactant gross weight (g).
Advantage of the present invention is: 1, the prepared fish-skin albumen of the present invention produces small-molecular peptides through behind the protease hydrolyzed, is easy to human body and digests and assimilates fast, and have no side effect, and is safe; 2, raw material of the present invention is the waste of tilapia processing, and technical transform of the present invention is that effective utilization of tilapia waste provides a new way; 3, craft science of the present invention is reasonable, and is simple to operate, with low cost, has stronger industrial implementation property; 4, products obtained therefrom of the present invention can be used as medicine, protective foods, food, foodstuff additive, medicine and increases agent etc.
Embodiment
Below in conjunction with instance the present invention is done further explain.
Case study on implementation:
Take by weighing the tilapia fishskin that 100.0008g rinses well, soak 1hr with the hydrochloric acid soln of 700ml0.1mol/L and the sodium hydroxide solution of 0.1mol/L successively after the skimming treatment, distilled water wash is to neutrality; Under 45 ℃ of conditions, with the zero(ppm) water constant temperature homogenate 12hr of 1000ml, suction filtration extracts supernatant; Be warming up to 50 ℃-55 ℃, regulating the pH value is 6.0, adds 0.04671g papoid constant temperature enzymolysis 2hr; Heating in water bath 20min under 100 ℃ of hot conditionss then; Enzymolysis reaction promptly gets the fish-skin protein enzymatic hydrolyzate, and the tilapia fishskin protein hydrolysis degree is 12.3%.
Adopt composite decoloring agent (the gac yeast of 3g/L and Schardinger dextrins etc. mix) that the fish-skin protein enzymatic hydrolyzate is carried out debitterize, decolours, takes off the flavor processing, supernatant is collected in 4000r/min centrifuging.Flow velocity with 8 times of column volume/h under the normal temperature passes through 001*7 (732) Zeo-karb; Collect effluent; Recording its nitrogen recovery is 95.40%; Again with the hydrolyzed solution behind the decationized Y sieve with the flow velocity of 8 times of column volume/h through 201*7 (717) anionite-exchange resin, collect effluent, record its nitrogen recovery and be 93.31% and ratio of desalinization be 93.15%.Effluent carries out uf processing after concentrating, and the ultrafiltration apparatus WP is 28psi, and feed temperature is 29 ℃, and material liquid pH is 6.7, and it is TSP-II solution that uf processing 40min obtains fishskin polypeptide liquid.
With content of peptides in the TSP-II solution is index; By the mass ratio of itself and zinc sulfate 3: 1, conditioned reaction pH value was 6.0,60 ℃ of constant temperature water baths; Magnetic agitation 1hr obtains chelate solution; Use 5 times absolute ethanol washing 2-3 time again, solution carries out after suction filtration handles, and filter residue is put in 80 ℃ of dry 30min of constant temperature promptly get product I I-Zn in the electric heating constant temperature air dry oven
2+, the chelation percent that records zinc sulfate is 92.31%, the inner complex yield is 28.39%.II-Zn
2+Be respectively 9436.2nm and 485.0nm with the particle size determination result of TSP-II, Zeta potential is-0.31mv and-4.36mv, and the ratio of raw material and water is 1: 5, and 25 ℃ of constant temperatures mensuration viscosity down are 3.73cp and 2.33cp.
Product performance is analyzed
Get TSP-II and II-Zn respectively
2+Compare analysis, analytical results is following:
1, color and luster
The TSP-II powder that is white in color, II-Zn
2+Be pale yellow powder.
2, rheological
Water=1: 5) and II-Zn adopt DV-III ULTRA rheometer (U.S. BROOKFIELD) respectively to TSP-II solution (raw material:
2+Solution (raw material: measure, and selects CP52 type rotor for use, and constant temperature is measured down at 25 ± 0.5 ℃ by rheological characteristics water=1: 5).Mensuration result shows: TSP-II and II-Zn
2+Be Newtonian fuid, II-Zn
2+The viscosity of solution is greater than TSP-II solution, and viscosity number is respectively: 3.73cp and 2.33cp.
3, size-grade distribution and Zeta potential
Adopt laser granulometry (U.S. pss company) respectively to TSP-II solution and II-Zn
2+The size-grade distribution of solution is measured, and can find out that from particle size distribution figure the particle diameter of TSP-II is 485.0nm, II-Zn
2+Particle diameter is 9436.2nm, and size distribution is even.
4, MWD
Adopt high performance liquid chromatograph (Waters company) that TSP-II is carried out molecular-weight determination, 66.56% is distributed in 2068-275Da, belongs to small-molecule peptide.
5, TSP-II and II-Zn
2+The infrared scan result
With 2mgII-Zn
2+Put into agate mortar, put into exsiccant spectroscopically pure KBr 200mg, mixed grinding is (carrying out under ir lamp) evenly, makes its particle diameter below 2.5um, the compression mold of packing into, and the pressurization of bleeding, pressure is about 600kg/cm
2, keep 3-5min, lay down pressure and then can get transparent KBr sample strip, utilize infrared spectrophotometer to carry out qualitative analysis, aforesaid method is also adopted in the detection of TSP-II.Infared spectrum scanning shows, compares II-Zn with TSP-II
2+At 2086.8cm
-1Place's one strong absorption peak disappears.
The above survey generated the novel substance that is different from TSP-II, TSP-II and II-Zn after each item index shows TSP-II and zinc sulfate chelating
2+Character relatively see table 1.
Table 1TSP-II and II-Zn
2+Character relatively
| Raw material | Color and luster | Particle diameter (nm) | Zeta potential (mv) | Viscosity (cp) |
| TSP-II II-Zn 2+ | White is faint yellow | 485.0 9436.2 | -4.36 -0.31 | 2.33 3.73 |
Claims (1)
1. the preparation method of a tilapia fishskin small molecular peptide chelate zinc salt is characterized in that the preparation method is:
Take by weighing the tilapia fishskin that 100.0008g rinses well, soak 1hr with the hydrochloric acid soln of 700ml0.1mol/L and the sodium hydroxide solution of 0.1mol/L successively after the skimming treatment, distilled water wash is to neutrality; Under 45 ℃ of conditions, with the zero(ppm) water constant temperature homogenate 12hr of 1000ml, suction filtration extracts supernatant; Be warming up to 50 ℃-55 ℃, regulating the pH value is 6.0, adds 0.04671g papoid constant temperature enzymolysis 2hr; Heating in water bath 20min under 100 ℃ of hot conditionss then; Enzymolysis reaction promptly gets the fish-skin protein enzymatic hydrolyzate, and the tilapia fishskin protein hydrolysis degree is 12.3%; The composite decoloring agent that gac, yeast and the Schardinger dextrins of employing 3g/L mixes carries out debitterize, decolours, takes off the flavor processing the fish-skin protein enzymatic hydrolyzate, and supernatant is collected in 4000r/min centrifuging, and the flow velocity with 8 times of column volume/h under the normal temperature passes through 001*7 (732) Zeo-karb; Collect effluent, recording its nitrogen recovery is 95.40%, again with the hydrolyzed solution behind the decationized Y sieve with the flow velocity of 8 times of column volume/h through 201*7 (717) anionite-exchange resin; Collect effluent; Record its nitrogen recovery and be 93.31% and ratio of desalinization be 93.15%, effluent carries out uf processing after concentrating; The ultrafiltration apparatus WP is 28psi; Feed temperature is 29 ℃, and material liquid pH is 6.7, and it is TSP-II solution that uf processing 40min obtains fishskin polypeptide liquid; With content of peptides in the TSP-II solution is index, and by the mass ratio of itself and zinc sulfate 3: 1, conditioned reaction pH value was 6.0; 60 ℃ of constant temperature water baths; Magnetic agitation 1hr obtains chelate solution, uses 5 times absolute ethanol washing 2-3 time again, and solution carries out after suction filtration handles; Filter residue is put in 80 ℃ of dry 30min of constant temperature in the electric heating constant temperature air dry oven, promptly gets product.
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| CN102174073A (en) * | 2010-12-17 | 2011-09-07 | 中国海洋大学 | Oyster protein peptide and zinc chelate and method for preparing same |
| CN102687790B (en) * | 2011-03-21 | 2013-09-11 | 汕尾市五丰海洋生物科技有限公司 | Method for preparing freshwater fish collagen peptide |
| CN102286582B (en) * | 2011-06-21 | 2013-07-24 | 华南理工大学 | Method for preparing memory-improving bioactive peptide from deep sea fish |
| CN102688497B (en) * | 2012-03-05 | 2013-12-25 | 浙江省海洋开发研究院 | Preparation method of polypeptide zinc-ferrum supplementary |
| CN103266143A (en) * | 2013-06-05 | 2013-08-28 | 河南工业大学 | Method for preparing compound amino acid chelated zinc by utilizing cold-pressed sesame-seed cake zymolyte |
| CN103626867B (en) * | 2013-06-19 | 2015-08-12 | 中国海洋大学 | A kind of preparation technology of zinc fish-skin collagen polypeptide chelate |
| CN104798980B (en) * | 2015-04-30 | 2019-06-04 | 中国食品发酵工业研究院 | A kind of oyster active peptides chelates of zinc and its preparation method and application |
| CN105146469B (en) * | 2015-07-19 | 2017-09-29 | 中盐榆林盐化有限公司 | A kind of sea food flavor salt and preparation method thereof |
| CN107101883A (en) * | 2017-03-29 | 2017-08-29 | 淄博黄河龙生物工程有限公司 | Collagent casing for sausages longitudinally resists the detection method of disconnected power |
| CN107568467A (en) * | 2017-10-09 | 2018-01-12 | 国家海洋局第三海洋研究所 | A kind of feeding trace meter additive of livestock and poultry for coming from aquatic products processing accessory substance and preparation method thereof |
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