CN101965897B - Processing method for mussel isolated protein - Google Patents
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- CN101965897B CN101965897B CN2010105135562A CN201010513556A CN101965897B CN 101965897 B CN101965897 B CN 101965897B CN 2010105135562 A CN2010105135562 A CN 2010105135562A CN 201010513556 A CN201010513556 A CN 201010513556A CN 101965897 B CN101965897 B CN 101965897B
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- 241000237536 Mytilus edulis Species 0.000 title claims abstract description 74
- 235000020638 mussel Nutrition 0.000 title claims abstract description 74
- 108090000623 proteins and genes Proteins 0.000 title claims abstract description 52
- 102000004169 proteins and genes Human genes 0.000 title claims abstract description 52
- 238000003672 processing method Methods 0.000 title claims abstract description 15
- 239000000843 powder Substances 0.000 claims abstract description 29
- 239000000706 filtrate Substances 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 15
- 238000004108 freeze drying Methods 0.000 claims abstract description 10
- 235000013372 meat Nutrition 0.000 claims abstract description 9
- 239000013049 sediment Substances 0.000 claims abstract description 6
- 230000007935 neutral effect Effects 0.000 claims abstract description 3
- 238000005238 degreasing Methods 0.000 claims description 28
- 239000012141 concentrate Substances 0.000 claims description 14
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 9
- 238000001694 spray drying Methods 0.000 claims description 4
- 238000007654 immersion Methods 0.000 claims description 3
- 238000000194 supercritical-fluid extraction Methods 0.000 claims description 2
- 238000001035 drying Methods 0.000 abstract description 4
- 238000002791 soaking Methods 0.000 abstract 2
- 235000019624 protein content Nutrition 0.000 abstract 1
- 235000018102 proteins Nutrition 0.000 description 44
- 239000000243 solution Substances 0.000 description 10
- 238000000605 extraction Methods 0.000 description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 5
- 238000010612 desalination reaction Methods 0.000 description 4
- 238000004090 dissolution Methods 0.000 description 4
- 230000006872 improvement Effects 0.000 description 4
- 235000016709 nutrition Nutrition 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 235000013305 food Nutrition 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 230000035764 nutrition Effects 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 238000000108 ultra-filtration Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004945 emulsification Methods 0.000 description 2
- 235000020776 essential amino acid Nutrition 0.000 description 2
- 239000003797 essential amino acid Substances 0.000 description 2
- 239000000796 flavoring agent Substances 0.000 description 2
- 235000019634 flavors Nutrition 0.000 description 2
- 238000005187 foaming Methods 0.000 description 2
- 150000002632 lipids Chemical class 0.000 description 2
- 235000013622 meat product Nutrition 0.000 description 2
- 235000008935 nutritious Nutrition 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 235000014102 seafood Nutrition 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 241000251468 Actinopterygii Species 0.000 description 1
- 241000272525 Anas platyrhynchos Species 0.000 description 1
- 241000238557 Decapoda Species 0.000 description 1
- 241000287828 Gallus gallus Species 0.000 description 1
- 108010064851 Plant Proteins Proteins 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 235000013361 beverage Nutrition 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 235000013409 condiments Nutrition 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 235000013365 dairy product Nutrition 0.000 description 1
- 230000007850 degeneration Effects 0.000 description 1
- 238000004925 denaturation Methods 0.000 description 1
- 230000036425 denaturation Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 235000013376 functional food Nutrition 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000002372 labelling Methods 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 230000000050 nutritive effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 235000011837 pasties Nutrition 0.000 description 1
- 235000021118 plant-derived protein Nutrition 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 235000004252 protein component Nutrition 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- Peptides Or Proteins (AREA)
- Meat, Egg Or Seafood Products (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The invention discloses a processing method for mussel isolated protein, which sequentially comprises the following steps of: 1) cutting mussel meat into pieces, performing freeze drying, crushing, and defatting to obtain defatted mussel powder; 2) mixing the defatted mussel powder and water, adjusting pH to be between 10 and 12, soaking, and centrifuging to obtain filtrate I and filter residue; 3) soaking the filter residue in water, and centrifuging to obtain filtrate II and sediment; 4) combining the filtrate I and the filtrate II, and adjusting the pH to neutral to obtain total filtrate; and 5) concentrating and drying the total filtrate to obtain the mussel isolated protein. The mussel isolated protein prepared by the method has the characteristics of good solubility and high proteincontent.
Description
Technical field
The present invention relates to a kind of extraction of protein, particularly a kind of extraction of mussel protein isolate and processing technology thereof.
Background technology
Mussel is common seashells and marine products treasure; Its meat flavour is delicious, and nutritious, especially Protein content is up to 47.8%; 8 kinds of essential amino acids that contain all human bodies, and contents of essential amino acids is higher than egg and food such as chicken, duck, fish, shrimp and meat far away.The mussel protein content of amino acids is seen table 1.
The nutritional labeling tabulation of table 1, mussel (doing) [mussel, mussel] (containing in per 100 grams)
Protein isolate in the market is main with plant protein powder, and seafood protein also rarely has report.Expansion along with China's mussel culture area; Increasing sharply of mussel output because that mussel is not easy to is fresh-keeping, and mainly is that the band shell is freezing or process dry product---mussel etc. for the processing of mussel at present; Lack further intensely processed products; For promoting the economic worth of this cheap marine product, make full use of this resource, people begin to develop the technology of mussel protein isolate.
The preparation method of present existing mussel protein powder is following:
After fresh mussel water cleaned up, byssus was removed in shelling, beater homogenate to pasty state, freeze drying (50 ℃, 72 hours), the mussel powder.The mussel powder under 40 ℃ of conditions, is added the ethanolic solution degreasing 4h of volumetric concentration 95%, triplicate in the ratio of 1g: 4ml; 100 mesh sieves are pulverized and crossed to mussel powder after the above-mentioned ungrease treatment in 40 ℃ of vacuum drying (5h),, get the dried mussel powder of degreasing of moisture≤2.51%.Take by weighing the dried mussel powder of degreasing, utilize the sodium hydroxide solution of pH11.5 to extract albumen, 35 ℃ of temperature; Extraction time is 2.5 hours; Under 4 ℃ of conditions of 3000r/min centrifugal 20 minutes, supernatant used concentration as the hydrochloric acid of 2N the pH value to be transferred to 3.5, precipitates (50 ℃ of centrifugal postlyophilizations; 72 hours), obtain protein content and be about 74% mussel protein powder.
The shortcoming that this method exists is following:
1), use the alcohol degreasing, the alcohol use amount is bigger, step is more loaded down with trivial details, number of repetition is many, though degreasing is cleaner, but the loss of proteins amount is bigger; And repeatedly the organic solvent immersion also can make albuminous degeneration;
2), this method is used the HCl precipitating proteins, the acid that needs consumption is a large amount of;
3), add acid at isoelectric point precipitates albumen, method is easy, cost is low, but often have coprecipitation phenomena, purification efficiency is not high, the purity of protein that is settled out is not high yet;
4), the albumen of deposition obtains albumen powder with freeze drying at last, though freeze drying can keep the original structure and the activity of albumen in theory, the albumen powder that obtains in fact like this is insoluble in water, even under stirring state, also be difficult for dissolving;
5), cryodesiccated albumen powder is deep on color and luster, the outward appearance particle is big, foaming characteristic is also well below spray-dired albumen powder.
Summary of the invention
It is simple that the technical problem that the present invention will solve provides a kind of extraction process, the processing method of free of contamination mussel protein isolate, and the mussel protein isolate dissolubility of gained is good, protein content is high.
In order to solve the problems of the technologies described above, the present invention provides a kind of processing method of mussel protein isolate, may further comprise the steps successively:
1), mussel meat chopping, after the freeze drying, be crushed to 40~60 orders, degreasing, degreasing mussel powder;
2), the w/v of above-mentioned degreasing mussel powder according to 1kg/20~30L mixed with water, regulate pH to 10~12 with NaOH then, soak centrifugal after 1.5~2.5 hours, must filtrate I and filter residue;
3), above-mentioned filter residue is immersed in the water by the w/v of 1kg/2~3L, soak centrifugal after 0.5~2.5 hour, filtrate II and sediment;
4), above-mentioned filtrating I and filtrate II are merged, transfer pH to neutral with HCl; Get filtrating always;
5), the total filtrating with the step 4) gained concentrate, drying; Get mussel protein isolate (being mussel protein).
Improvement as the processing method of mussel protein isolate of the present invention: CO is used in the degreasing in the step 1)
2Supercritical extraction.
Further improvement as the processing method of mussel protein isolate of the present invention: step 2) and the immersion in the step 3) all under stirring condition, carry out.
Further improvement as the processing method of mussel protein isolate of the present invention: step 2) and the centrifugal 5000~10000rmp that is in the step 3), 10~15min.
Further improvement as the processing method of mussel protein isolate of the present invention: the concentrated employing hyperfiltration technique of step 5), and spray-dried pulverous mussel protein isolate.
The present invention adopts CO
2The supercritical extract degreasing not only makes the lipid material of extraction keep original character, can do him in addition and use; Can also keep other components unchanged after the degreasing, and have fast and convenient advantage.
The present invention adopts milipore filter to concentrate, and promptly from big molecular solution, removes salt and little molecule solable matter, and not only step is easy; Mild condition; Need not to add other chemical reagent, no phase transformation improves protein extracting ratio; The purity of protein that makes is high, and the protein liquid after ultrafiltration concentrates carries out drying again and can cut down the consumption of energy greatly.Spray-dried albumen powder, the outward appearance look white, and powder is fine and smooth, and is soluble in water.
In the present invention, adopt PH10~12 alkaline aqueous solutions, make mussel protein stripping preferably as extractant; Simultaneously can not make protein denaturation again; Whole leaching process all carries out under normal temperature or low temperature, can not make the protein component sex change in the extract, has guaranteed the solubility of albumen in normal-temperature water solution; Through Primary Study to the distribution of the component of mussel protein and molecular weight, minimum about tens KD of molecular weight, it is about 5000 milipore filter that the present invention selects molecular cut off for use, concentrates and desalination.The inventive method is easy, and the equipment that needs is simple, and protein extracting ratio high (more than >=83%) separates the mussel protein purity high (>=90%) that obtains.
Adopt the mussel protein isolate of the inventive method gained both to can be used as nutritious supplementary pharmaceutical, be widely used in the nutriment such as health care for the middle and old aged article, child nutrition article, thus enhancement people's nutrition condition; Also can add in various solid beverages and the dairy produce to improve the goods Protein content, enhancing nutrition; More can be used as raw material and process the condiment of seafood flavor through methods such as fermentations.The mussel protein isolate adds meat products to, improves the mouthfeel and the structure of goods as raw-food material; Keep the goods tissue fine and smooth moistening; Promote fatty emulsification and albumen gelling, especially in cooked meat product, can improve texture, taste and cutability, improve the acceptable degree and the nutritive value of goods; In addition, also can excavate the latent effect of mussel protein, also can from mussel protein, isolate a kind of molecule and derive its a kind of or several kinds of molecules by it again; Utilize its some physicochemical properties; Or the characteristic that is used for food processing that obtains of method of modifying through physics or chemistry, for example: emulsification, gel, foaming characteristic, retentiveness, oil absorption etc., as the source of novel functional food; Therefrom obtain functional and the biologically active batching, be applied to a plurality of fields of food processing.
The specific embodiment
The processing method of embodiment 1, a kind of mussel protein isolate, carry out following steps successively:
1), mussel meat chopping, after the freeze drying (60 ℃, 24 hours), be crushed to 60 orders, CO
2Supercritical extract degreasing (lipid uses it for anything else in addition) obtains the degreasing mussel powder of moisture≤2.5%.
CO
2The process conditions of supercritical extract degreasing for example can be:
Material (mussel meat after the pulverizing) thickness 5-10mm, freeze-off time 5 hours freezes outlet temperature-25 ℃, condenser temperature 50-60 ℃, vacuum 25-50pa, 25 ℃ of freeze-drying final temperatures, drying time 20h.The pressure of separation reactor I is 7-8MPa, 60 ℃ of temperature; The pressure of separation reactor I I is 4-6MPa, 35 ℃ of temperature; Extraction kettle pressure is 30MPa, and temperature is 45 ℃; CO
2Flow is 15 times/h of extraction kettle capacity; The extraction time is 2h.
Above-mentioned degreasing mussel powder adopts Kjeldahl to detect, and protein content is 45%.
2), above-mentioned 0.85 kilogram of degreasing mussel powder is mixed with 20L water, NAOH solution (for example, molar concentration is 2N) is regulated pH to 10 then; Stirring condition soaked 2.5 hours down, the centrifugal 15min of 10000rmp, must filtrate I and filter residue.
3), according to the amount ratio of the corresponding 2.5L water of 1kg filter residue, in above-mentioned filter residue, add water and in stirring condition under, soaked 1 hour, the centrifugal 15min of 10000rmp must filtrate II and sediment.
4), above-mentioned filtrating I and filtrate II are merged, transfer pH to neutrality with HCl solution (for example, molar concentration is 2N); Get filtrating always.
5), the total filtrating of step 4) gained is used molecular cut off is 6000 ultrafiltration membrance filter, thereby concentrate also desalination; Get concentrate.
6), the concentrate of step 5) gained is carried out spray-drying, 150 ℃ of inlet temperatures, outlet temperature are 80 ℃.
Obtain the pulverous mussel protein of 350g, protein extracting ratio is 84.4%, and protein content is 92.2%.Dissolution rate is 52.3%.
The processing method of embodiment 2, a kind of mussel protein isolate, carry out following steps successively:
1), mussel meat chopping, after the freeze drying, be crushed to 50 orders, CO
2The supercritical extract degreasing makes the degreasing mussel powder of moisture≤2.5%.This degreasing mussel powder adopts Kjeldahl to detect, and protein content is 45%.
2), above-mentioned 1.5 kilograms of degreasing mussel powder are mixed with 45L water, regulate PH to 10 with NAOH solution, stirring condition soaked down after 2 hours, the centrifugal 15min of 10000rmp, must filtrate I and filter residue.
3), according to the amount ratio of the corresponding 2L water of 1kg filter residue, in above-mentioned filter residue, add water and in stirring condition under, soaked 0.5 hour, the centrifugal 15min of 10000rmp must filtrate II and sediment.
4), above-mentioned filtrating I and filtrate II are merged, transfer pH to neutrality with HCl solution; Get filtrating always.
5), above-mentioned total filtrating is used molecular cut off is 4000 ultrafiltration membrance filter, thereby concentrate also desalination; Get concentrate.
6), above-mentioned concentrate is carried out spray-drying, 150 ℃ of inlet temperatures, outlet temperature are 80 ℃.
Obtain the pulverous mussel protein of 630g, protein extracting ratio is 86.2%, and protein content is 92.4%.Dissolution rate is: 48.21%.
The processing method of embodiment 3, a kind of mussel protein isolate, carry out following steps successively:
1), mussel meat chopping, after the freeze drying, be crushed to 40 orders, CO
2Degreasing mussel powder is processed in the supercritical extract degreasing.Above-mentioned degreasing mussel powder adopts Kjeldahl to detect, and protein content is 44.5%.
2), 1 kilogram in above-mentioned degreasing mussel powder is mixed with 20L water, regulate pH to 11.5 with NAOH solution.Stirring condition soaked down after 1.5 hours, the centrifugal 15min of 10000rmp, must filtrate I and filter residue.
3), according to the amount ratio of the corresponding 2.9L water of 1kg filter residue, in above-mentioned filter residue, add water and in stirring condition under, soaked 0.5 hour, the centrifugal 15min of 10000rmp must filtrate II and sediment.
4), above-mentioned filtrating I and filtrate II are merged, transfer pH to neutrality with HCl solution; Get filtrating always.
5), above-mentioned total filtrating is used molecular cut off is 5000 milipore filter, thereby concentrate also desalination; Get concentrate.
6), above-mentioned concentrate is carried out spray-drying, 150 ℃ of inlet temperatures, outlet temperature are 80 ℃.
Obtain the pulverous mussel protein of 412g, protein extracting ratio is 83.8%, and protein content is 90.5%.Dissolution rate is 53.43%.
Comparative Examples: adopt the method for distilling of informing in the background technology to extract mussel protein, protein extracting ratio is 58.48%, and protein content is 74.32%.Dissolution rate is<30%.
At last, it is also to be noted that what more than enumerate only is several specific embodiments of the present invention.Obviously, the invention is not restricted to above embodiment, many distortion can also be arranged.All distortion that those of ordinary skill in the art can directly derive or associate from content disclosed by the invention all should be thought protection scope of the present invention.
Claims (3)
1. the processing method of mussel protein isolate is characterized in that may further comprise the steps successively:
1), mussel meat chopping, after the freeze drying, be crushed to 40~60 orders, degreasing, degreasing mussel powder;
CO is used in said degreasing
2Supercritical extraction;
2), the w/v of above-mentioned degreasing mussel powder according to 1kg/20~30L mixed with water, regulate pH to 10~12 with NaOH then, soak centrifugal after 1.5~2.5 hours, must filtrate I and filter residue;
3), above-mentioned filter residue is immersed in the water by the w/v of 1kg/2~3L, soak centrifugal after 0.5~2.5 hour, filtrate II and sediment;
4), above-mentioned filtrating I and filtrate II are merged, transfer pH to neutral with HCl; Get filtrating always;
5), adopt hyperfiltration technique to concentrate spray-drying total filtrating of step 4) gained; Get pulverous mussel protein isolate.
2. the processing method of mussel protein isolate according to claim 1 is characterized in that: step 2) and step 3) in immersion all under stirring condition, carry out.
3. the processing method of mussel protein isolate according to claim 2 is characterized in that: step 2) and step 3) in the centrifugal 5000~10000rpm that is, 10~15min.
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CN102524645B (en) * | 2012-01-19 | 2013-12-11 | 广西还珠海洋生物科技有限公司 | Method for extracting pearl foetal sac liquid from pearl foetal sac of mother pearl shellfish, product and application of product |
CN106928332A (en) * | 2017-01-10 | 2017-07-07 | 大连工业大学 | A kind of preparation method of different deliquescent mussel proteins and polypeptide |
CN109007233A (en) * | 2018-09-06 | 2018-12-18 | 大连工业大学 | A kind of extracting method of stichopus japonicus intestines protein isolate |
CN109265528A (en) * | 2018-09-19 | 2019-01-25 | 南方医科大学 | A kind of preparation method of sea-mussel mucin |
CN109593599A (en) * | 2018-12-28 | 2019-04-09 | 大连工业大学 | A kind of extracting method of clam quasi-grease and protein |
CN113604531A (en) * | 2021-08-23 | 2021-11-05 | 大连工业大学 | Method for simultaneously preparing mussel functional lipid and active polypeptide |
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