CN113995045B - Method for preparing low-fluorine protein from defatted euphausia superba powder - Google Patents
Method for preparing low-fluorine protein from defatted euphausia superba powder Download PDFInfo
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- 229910052731 fluorine Inorganic materials 0.000 title claims abstract description 43
- 239000011737 fluorine Substances 0.000 title claims abstract description 43
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- 238000000034 method Methods 0.000 title claims abstract description 23
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Classifications
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23J—PROTEIN COMPOSITIONS FOR FOODSTUFFS; WORKING-UP PROTEINS FOR FOODSTUFFS; PHOSPHATIDE COMPOSITIONS FOR FOODSTUFFS
- A23J1/00—Obtaining protein compositions for foodstuffs; Bulk opening of eggs and separation of yolks from whites
- A23J1/04—Obtaining protein compositions for foodstuffs; Bulk opening of eggs and separation of yolks from whites from fish or other sea animals
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L2/00—Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
- A23L2/52—Adding ingredients
- A23L2/66—Proteins
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/17—Amino acids, peptides or proteins
-
- 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
Abstract
The invention discloses a method for preparing low-fluorine protein from defatted antarctic krill powder, which comprises the following steps: ultrasonic alkaline extraction is carried out on the defatted euphausia superba powder, and then solid-liquid separation is carried out, so as to obtain supernatant and precipitate; adding DL-malic acid solution into the supernatant, and performing acid precipitation to obtain acid precipitation supernatant and acid precipitation precipitate; adding calcium citrate into the acid precipitation supernatant, stirring for a set time, taking the supernatant, and drying to obtain protein A powder; precipitating with distilled water, neutralizing, and drying supernatant to obtain protein B powder; adding water to the precipitate after acid precipitation, re-dissolution and neutralization, and drying to obtain protein C powder. No toxic and harmful chemical agent is used, all additives are food grade, and the method is simple and efficient and is suitable for industrial production.
Description
Technical Field
The invention belongs to the technical field of protein resource development, and particularly relates to a method for preparing low-fluorine protein powder from defatted antarctic krill powder.
Background
The statements herein merely provide background information related to the present disclosure and may not necessarily constitute prior art.
At present, the by-product of the euphausia superba after extracting grease, namely defatted euphausia superba powder, is mostly used as a low added value product for animal feed and the like. The protein content in the defatted antarctic krill powder after the grease is extracted by ethanol can reach 60 percent, the fat content is only 8.7 percent, but the fluorine content is as high as 2312 mug/g.
The macromolecular protein in antarctic krill not only can be used as a protein base material for developing natural active peptide, but also can be directly used as a food additive, a protein drink and the like for the food processing field. The osmotic pressure of macromolecular protein is between amino acid/short peptide and integrin, so that other intestinal reactions such as diarrhea caused by higher osmotic pressure are avoided, and the macromolecular protein is easier to absorb than integrin, and can be used as a high-quality raw material of special medical formula food for nutrition supplement of patients suffering from serious diseases such as postoperative body recovery and tumors.
The preparation method of antarctic krill protein is commonly used as an enzymolysis method, an isoelectric dissolution and precipitation technology (isoelectric solubilization/ISP) and the like. The enzymolysis method is suitable for preparing protein peptide, and is mostly applied to products such as medicines, cosmetics, nutritional additives and the like, but the exposure of a large amount of hydrophobic amino acid in the enzymolysis process can cause bitter taste, and the amino acid/short peptide has extremely high osmotic pressure in human intestinal tracts, is easy to cause diarrhea and other intestinal reactions, so the protein peptide cannot be eaten in a large amount as protein drinks and the like.
Most of the proteins extracted by ISP technology or alkali-soluble acid precipitation technology are macromolecular proteins, and the method has the advantages of high extraction rate and simple operation. When the alkali-soluble acid precipitation technology is used for extracting protein, the hydrolysis degree of the protein can be improved and the content of the polypeptide can be increased due to longer action time of alkali solution. In addition, for the raw material with extremely high fluorine content, namely the defatted antarctic krill powder, the protein extracted by using ISP technology and alkali-dissolution and acid-precipitation technology is difficult to reach the limit standard of the fluorine content in food safety. Most researchers often neglect to utilize the supernatant fluid after acid precipitation when using the two methods for protein extraction, and the supernatant fluid is mostly treated as waste liquid, however, the inventor discovers that the supernatant fluid also contains a large amount of protein, has relatively low molecular weight, good solubility and wide pH application range, can be used for preparing liquid beverage and researching and developing other functional foods, and provides a new idea for comprehensively utilizing euphausia superba protein.
Therefore, it is difficult in the prior art to extract low-fat, low-fluorine euphausia superba macromolecular proteins from defatted euphausia superba meal and recover low molecular weight proteins from acid supernatant.
Disclosure of Invention
In view of the above problems in the prior art, it is an object of the present invention to provide a method for preparing low-fluorine proteins from defatted antarctic krill meal.
In order to achieve the above object, the present invention is realized by the following technical scheme:
a method for preparing low fluorine protein from defatted antarctic krill meal, comprising the steps of:
ultrasonic alkaline extraction is carried out on the defatted euphausia superba powder, and then solid-liquid separation is carried out, so as to obtain supernatant and precipitate;
adding DL-malic acid solution into the supernatant to obtain acid precipitation supernatant and acid precipitation precipitate.
Adding calcium citrate into the acid precipitation supernatant with high fluorine content, stirring for a set time, taking the supernatant, and drying to obtain protein A powder.
The inventor compares the common alkali extraction technology, and discovers that the extraction rate of euphausia superba protein extracted by the ultrasonic-assisted alkali extraction technology is improved by 17%, and the hydrolysis degree is improved by 1.5%, so that the ultrasonic-assisted alkali extraction technology is an effective macromolecular protein extraction means.
The inventor finds that more than 95% of fluorine in the antarctic krill protein subjected to alkali extraction is in a water-soluble state, so that most of water-soluble fluorine can be removed by washing the protein subjected to acid precipitation.
In some embodiments, the protein B powder is obtained by precipitation with distilled water, precipitation with acid, neutralization, and drying the supernatant.
Further, the step of ultrafiltration is also included before the supernatant is dried to prepare the protein B powder.
Furthermore, the ultrafiltration adopts a 1000Da ultrafiltration membrane to carry out ultrafiltration so as to desalt, decolor, remove fishy smell and remove soluble impurities of other small molecules, and reduce the loss of euphausia superba protein.
Further, the drying method is spray drying.
Further, the acid precipitation is redissolved, and the neutralized precipitate is dispersed by adding water and centrifuged to carry out water elution of fluorine.
Furthermore, the C protein powder is prepared by spray drying.
In some embodiments, the pH of the ultrasonic alkaline solution is 13-14.
Further, in the ultrasonic alkali extraction solution, the solid-liquid ratio is 1:22-25, g/L.
Further, the ultrasonic density of the ultrasonic alkali extraction is 0.08-0.10W/mL, the ultrasonic temperature is 50-55 ℃, and the ultrasonic time is 70-80min. Too small ultrasonic power can cause the reduction of the protein extraction rate, and too large ultrasonic power can influence the structure of the protein, so that the protein denaturation is easy to cause.
In some embodiments, the pH of the supernatant after adding DL-malic acid is from 4.5 to 5.5.
In some embodiments, the concentration of calcium citrate added to the acid precipitation supernatant is 3.5-4.5g/L. According to the early test, the calcium citrate is a calcium source substance capable of reducing protein loss to a greater extent on the premise of a certain defluorination rate, and other calcium source substances can have a good defluorination effect, but lose more protein, and the calcium citrate is selected under comprehensive consideration.
Further, the pH value of the supernatant fluid after the calcium citrate is added is 8.5-9.5.
Further, after adding calcium citrate into the acid precipitation supernatant, stirring for 100-150min at 35-40deg.C.
Still further, the method further comprises the step of ultrafiltering the supernatant before drying the supernatant to prepare protein A powder.
Still further, the drying is spray drying.
The beneficial effects achieved by one or more embodiments of the present invention are as follows:
DL-malic acid can be used for efficiently precipitating protein to ensure the extraction rate, and can be used for optimizing the defluorination effect of protein precipitation. Using Ca in calcium citrate 2+ And F is equal to - Generation of CaF 2 The precipitate was defluorinated with the acid supernatant.
The invention does not use toxic and harmful chemical agents, all additives are food-grade, and the invention is simple and efficient and is suitable for industrial production. The three proteins are powdery and are easy to dissolve in water, the moisture content is lower than 8%, the purity is higher than 80%, and the fat content is lower than 0.5%, wherein the protein A powder is antarctic krill acid precipitation supernatant protein powder, the fluorine content is lower than 50mg/kg, the protein B powder is antarctic krill redissolution supernatant protein powder, the fluorine content is lower than 10mg/kg, the protein C powder is antarctic krill redissolution precipitation protein powder, the fluorine content is lower than 35mg/kg, and the requirements of the maximum fluorine content of the fish protein concentrate specified by the American FDA are met.
The three euphausia superba protein powders prepared by the method have the advantages of high purity, safety and high nutritive value, and can be used as high-quality raw materials of protein drinks, food additives and formula foods with special medical purposes.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention.
FIG. 1 is a process flow diagram of an embodiment of the present invention.
Detailed Description
It should be noted that the following detailed description is illustrative and is intended to provide further explanation of the invention. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
Example 1
As shown in fig. 1, the defatted antarctic krill powder is crushed by a high-speed multifunctional crusher and is sieved by a 80-mesh sieve; adding purified water into crushed shrimp powder, adding 25 liters of water per kilogram of shrimp powder, stirring and mixing, regulating the pH value to 13.0 by using a food-grade NaOH aqueous solution, and homogenizing for 3min at 16 000 rpm; placing in an ultrasonic instrument, performing ultrasonic treatment at ultrasonic density of 0.08W/mL and ultrasonic temperature of 50deg.C for 80min, centrifuging, and collecting supernatant. Adding DL-malic acid water solution into antarctic krill alkali extract supernatant, adjusting pH to 5.0, centrifuging to obtain acid precipitation supernatant and precipitate. Adding 4.0g of calcium citrate into each liter of acid precipitation supernatant, adjusting pH to 9.0, magnetically stirring at 40 ℃ for 120min, centrifuging to obtain supernatant, ultrafiltering with 1000Da membrane, and spray drying to obtain protein A powder (antarctic krill acid precipitation supernatant protein powder). Precipitating with distilled water with 5% redissolved acid, washing once with 10%, neutralizing, centrifuging, ultrafiltering the supernatant with 1000Da ultrafilter membrane, spray drying to obtain protein B powder (Euphausia superba redissolved supernatant protein powder), adding water into the redissolved precipitate, and spray drying to obtain protein C powder (Euphausia superba redissolved precipitate protein powder).
The protein extraction rate (protein extraction rate=protein mass in alkaline supernatant (g)/protein mass in raw material (g) ×100%) of this example in the ultrasound-assisted alkaline extraction stage was 97.8%, and the total recovery rate of prepared euphausia superba protein powder A, B and C (prepared protein powder mass/protein mass in raw material×100) was 78.3%, a: B: c=19:55:28.
The purity of the protein A powder is 85.43+/-0.09 percent, and the dry weight is realized; the fat content was 0.41.+ -. 0.01% dry weight.
The purity of the protein B powder is 88.41 +/-0.51 percent, and the dry weight is the dry weight; the fat content was 0.28.+ -. 0.03%, dry weight.
The purity of the protein C powder is 83.17+/-0.66 percent, and the dry weight is realized; the fat content was 0.16.+ -. 0.01% dry weight.
The fluorine content in the protein A powder is 46.1mg/kg (dry weight); the fluorine content in the protein B powder is 6.01mg/kg (dry weight); the fluorine content of the protein C powder was 32.5mg/kg (dry weight). Meets the requirements of the U.S. FDA regulation that the fluorine content of the fish protein concentrate is up to 100 mg/kg.
Example 2
Crushing the defatted antarctic krill powder by a high-speed multifunctional crusher, and sieving the defatted antarctic krill powder with a 80-mesh sieve; adding purified water into crushed shrimp powder, adding water with the amount of 22 liters per kilogram of shrimp powder, stirring and mixing, regulating the pH value to 13.5 by using a food-grade NaOH aqueous solution, and homogenizing for 3min at 16 000 rpm; placing in an ultrasonic instrument with ultrasonic density of 0.10W/mL and ultrasonic temperature of 55deg.C for 80min, centrifuging, and collecting supernatant. Adding DL-malic acid water solution into antarctic krill alkali extract supernatant, adjusting pH to 5.0, centrifuging to obtain acid precipitation supernatant and precipitate. Adding 3.5g calcium citrate to each liter of acid precipitation supernatant, adjusting pH to 9.0, magnetically stirring at 35 ℃ for 120min, centrifuging to obtain supernatant, ultrafiltering with 1000Da ultrafiltration membrane, and spray drying to obtain protein A powder (antarctic krill acid precipitation supernatant protein powder). Precipitating with distilled water with 5% redissolved acid, washing once with 10%, neutralizing, centrifuging, ultrafiltering the supernatant with 1000Da ultrafilter membrane, spray drying to obtain protein B powder (Euphausia superba redissolved supernatant protein powder), adding water into the redissolved precipitate, and spray drying to obtain protein C powder (Euphausia superba redissolved precipitate protein powder).
The protein extraction rate (protein mass (g) in alkaline supernatant/protein mass (g) in raw material x 100%) of this example in the ultrasound-assisted alkaline extraction stage was 95.9%, and the total recovery rate (protein mass produced/protein mass in raw material x 100) of prepared euphausia superba protein powder A, B and C was 75.1%, a: B: c=18:59:23.
The purity of the protein A powder is 84.93 +/-0.22 percent, and the dry weight is the dry weight; the fat content was 0.42.+ -. 0.04%, dry weight.
The purity of the protein B powder is 90.10+/-0.21 percent, and the dry weight is the dry weight; the fat content was 0.31.+ -. 0.03%, dry weight.
The purity of the protein C powder is 85.17+/-0.36 percent, and the dry weight is realized; the fat content was 0.20.+ -. 0.01% dry weight.
The fluorine content in the protein A powder is 48.9mg/kg (dry weight); the fluorine content in the protein B powder is 5.8mg/kg (dry weight); the fluorine content of the protein C powder was 35.6mg/kg (dry weight). Meets the requirements of the U.S. FDA regulation that the fluorine content of the fish protein concentrate is up to 100 mg/kg.
Example 3
The same conditions as in example 1 were followed except that 10.0g of chitosan (degree of deacetylation 90%) was added to each liter of acid supernatant, the pH was adjusted to 4.0, and instead of adding 4.0g of calcium citrate to each liter of acid supernatant, the pH was adjusted to 9.0.
The protein extraction rate (=protein mass (g) in alkaline supernatant/protein mass (g) in raw material x 100%) of this example in the ultrasound-assisted alkaline extraction stage reached 96.7%, and the total recovery rate of prepared euphausia superba protein powder A, B and C (prepared protein powder mass/protein mass in raw material x 100) was 65.1%, a: B: c=8:72:20.
The fluorine content in the protein A powder is 30.1mg/kg (dry weight); the fluorine content in the protein B powder is 6.2mg/kg (dry weight); the fluorine content of the protein C powder was 36.7mg/kg (dry weight).
Example 4
The conditions were the same as in example 1 except that the thermostatted oscillator was used instead of the sonicator.
The protein extraction rate (=protein mass in alkaline supernatant (g)/protein mass in raw material (g) ×100%) of this example in the ultrasound-assisted alkaline extraction stage was 66.1%, and the total recovery rate of prepared euphausia superba protein powder A, B and C (prepared protein powder mass/protein mass in raw material×100) was 48.7%, a: B: c=17:60:23.
Example 5
The conditions were the same as in example 1 except that hydrochloric acid was used instead of DL-malic acid.
The protein extraction rate (=protein mass (g) in alkaline supernatant/protein mass (g) in raw material ×100%) of this example in alkaline stage was 95.9%, and the total recovery rate of prepared euphausia superba protein powder A, B and C (prepared protein powder mass/protein mass in raw material ×100) was 73.9%, a: B: c=15:62:23.
The fluorine content in the protein A powder is 46.7mg/kg (dry weight); the fluorine content in the protein B powder is 25.9mg/kg (dry weight); the fluorine content of the protein C powder was 110.7mg/kg (dry weight).
Example 6
The conditions were the same as in example 1 except that the acid precipitated protein was not washed.
The protein extraction rate (=protein mass (g) in alkaline supernatant/protein mass (g) in raw material x 100%) of this example in the ultrasound-assisted alkaline extraction stage reached 97.8%, and the total recovery rate of prepared euphausia superba protein powder A, B and C (prepared protein powder mass/protein mass in raw material x 100) was 78.3%, a: B: c=19:55:28.
The protein A powder prepared in this example had a fluorine content of 46.7mg/kg (dry weight); the fluorine content in the protein B powder is 27.8mg/kg (dry weight); the fluorine content of the protein C powder was 132.1mg/kg (dry weight).
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (6)
1. A method for preparing low-fluorine protein from defatted euphausia superba powder, which is characterized by comprising the following steps: the method comprises the following steps:
ultrasonic alkaline extraction is carried out on the defatted euphausia superba powder, and then solid-liquid separation is carried out, so as to obtain supernatant and precipitate;
adding DL-malic acid solution into the supernatant to obtain acid precipitation supernatant and acid precipitation precipitate;
adding calcium citrate into the acid precipitation supernatant with high fluorine content, stirring for a set time, taking the supernatant, and drying to obtain protein A powder;
precipitating with distilled water, neutralizing, and drying supernatant to obtain protein B powder;
adding water into the precipitate after acid precipitation and re-dissolution and neutralization for dispersion and centrifugation, eluting fluorine by water, and preparing protein C powder by spray drying;
the pH value of the ultrasonic alkali extraction solution is 13-14;
in the ultrasonic alkali extraction solution, the solid-liquid ratio is 1:22-25g/L;
ultrasonic density of ultrasonic alkali extraction is 0.08-0.10W/mL, ultrasonic temperature is 50-55 ℃, and ultrasonic time is 70-80min;
the pH value of the supernatant after adding DL-malic acid is 4.5-5.5;
the concentration of the calcium citrate added into the acid precipitation supernatant is 3.5-4.5g/L;
the pH value of the supernatant fluid after the acid precipitation is added with calcium citrate is 8.5-9.5;
after adding calcium citrate into the acid precipitation supernatant, stirring for 100-150min at 35-40deg.C.
2. The method of producing low fluorine protein from defatted antarctic krill meal of claim 1, wherein: the supernatant is dried to prepare protein B powder, and the method also comprises an ultrafiltration step.
3. The method of producing low fluorine protein from defatted antarctic krill meal according to claim 2, wherein: the ultrafiltration is ultrafiltration by adopting a 1000Da ultrafiltration membrane.
4. The method of producing low fluorine protein from defatted antarctic krill meal of claim 1, wherein: the drying method is spray drying.
5. The method of producing low fluorine protein from defatted antarctic krill meal of claim 1, wherein: the supernatant is subjected to ultrafiltration before being dried to prepare protein A powder.
6. The method of producing low fluorine protein from defatted antarctic krill meal of claim 1, wherein: the drying is spray drying.
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