CN117946254A - Extraction process of chondroitin sodium sulfate, elastin peptide and collagen peptide - Google Patents
Extraction process of chondroitin sodium sulfate, elastin peptide and collagen peptide Download PDFInfo
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- CN117946254A CN117946254A CN202410151486.2A CN202410151486A CN117946254A CN 117946254 A CN117946254 A CN 117946254A CN 202410151486 A CN202410151486 A CN 202410151486A CN 117946254 A CN117946254 A CN 117946254A
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- 229920002549 elastin Polymers 0.000 title claims abstract description 69
- 102000016942 Elastin Human genes 0.000 title claims abstract description 68
- 108010014258 Elastin Proteins 0.000 title claims abstract description 68
- 102000008186 Collagen Human genes 0.000 title claims abstract description 54
- 108010035532 Collagen Proteins 0.000 title claims abstract description 54
- 229920001436 collagen Polymers 0.000 title claims abstract description 54
- 238000000605 extraction Methods 0.000 title claims abstract description 39
- 229920002567 Chondroitin Polymers 0.000 title claims abstract description 20
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 title claims abstract description 20
- DLGJWSVWTWEWBJ-HGGSSLSASA-N chondroitin Chemical compound CC(O)=N[C@@H]1[C@H](O)O[C@H](CO)[C@H](O)[C@@H]1OC1[C@H](O)[C@H](O)C=C(C(O)=O)O1 DLGJWSVWTWEWBJ-HGGSSLSASA-N 0.000 title claims abstract description 20
- 229910052938 sodium sulfate Inorganic materials 0.000 title claims abstract description 18
- 235000011152 sodium sulphate Nutrition 0.000 title claims abstract description 18
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Abstract
The invention discloses an extraction process of chondroitin sodium sulfate, elastin peptide and collagen peptide, which relates to the technical field of processing of compact connective tissues and comprises the following steps of: pretreating, degreasing, separating, carrying out enzymolysis, purifying, concentrating, drying and the like on the beef tendon. The process aims at the characteristics of toughness and difficult processing of the beef tendon, adds pretreatment steps, and improves the extraction process in a low-cost mode. The method simultaneously extracts the chondroitin sulfate sodium, the elastin peptide and the collagen peptide, and has high product yield (1.1 to 1.3 percent of the chondroitin sulfate sodium, 5.3 to 16.5 percent of the elastin peptide and 8.1 to 15.6 percent of the collagen peptide), high quality and high purity; wherein, the content of desmin and isodesmin in the elastin peptide is 0.32-1.13%, and the content of peptides below 5000Da is more than 90%, thus improving the comprehensive utilization value of the beef tendon.
Description
Technical Field
The invention belongs to the technical field of dense connective tissue processing, and particularly relates to an extraction process of chondroitin sodium sulfate, elastin peptide and collagen peptide.
Background
The beef tendon comprises beef tendon, beef ligament and the like, is compact connective tissue, mainly comprises water, collagen fiber, elastic fiber, fibroblasts and matrixes, wherein the water content of fresh beef tendon is more than 70%, the content difference of the elastic fiber of the beef tendon at different positions is large, the beef tendon accounts for about 20% -30% of the dry basis, the beef tendon accounts for 1% -3%, the proteoglycan containing chondroitin sulfate accounts for only 1% -5%, the plasma of copper, manganese and calcium accounts for about 0.2%, and the collagen fiber accounts for about 70% -90%, and is mainly type I collagen. The production of the source chondroitin sulfate sodium generally selects costal cartilage, nasal bone cartilage, scapular cartilage, tracheal cartilage and the like with higher chondroitin content.
Chondroitin Sulfate (CS) is an acidic mucopolysaccharide widely existing in bovine bones, pig bones, chicken bones, shark bones and squid bones, belongs to one of glycosaminoglycans, is a natural biological macromolecule, and is mostly composed of polysaccharide chains and proteins in tissues, and the bonding mode is covalent bonding of the polysaccharide chains and core proteins. The chondroitin sulfate sodium consists of 50-70 disaccharide units, wherein the disaccharide units are formed by glucuronic acid and N-acetylgalactosamine through beta (1-3) glycosidic bond, disaccharide is polymerized into macromolecules through beta (1-4) glycosidic bond connection, and part of C-6 or C-4 position of N-acetylgalactosamine is sulfated and combined with sodium ions through sulfate groups or hydroxy acid groups. The chondroitin sulfate sodium has the physiological functions of reducing blood fat, anticoagulating blood, resisting inflammation, resisting tumor and the like. Clinically, the eye drops are mainly used for treating diseases such as osteoarthritis, hyperlipidemia, angina pectoris, atherosclerosis and the like, and the eye drops have the function of treating cornea injury, cornea ulcer or keratitis; sodium chondroitin sulfate is classified on food by the us FDA as a dietary supplement that australia uses as a nutraceutical to improve or prevent arthropathy. At present, the industrial production of the sodium chondroitin sulfate adopts an enzymolysis method to extract from animal cartilage, and mainly comprises the steps of impurity removal, cleaning, material boiling, enzymolysis, deproteinization, filtration, centrifugation, ion exchange, ultrafiltration, alcohol precipitation, drying and the like.
Collagen is an animal protein with the largest content in mammals, mainly exists in tissues such as bones, tendons, ligaments, skin and the like, and is an important structural protein in connective tissues. Collagen consists of three peptide chains which form a complex helix in a characteristic manner, and can be hydrolyzed by protease after denaturation. The collagen peptide is a hydrolysate of bovine bones, is rich in hydroxyproline, is composed of more than 2 amino acids, and can be used in various fields such as foods, health-care foods, cosmetics, biological materials, microorganism culture mediums, high-end feeds and the like. The collagen peptide has low molecular weight and is easy to absorb, and the national food standard of the collagen peptide requires more than 90 percent of the relative molecular weight below 10000.
Elastin is the major component of elastane fiber. Elastic fibers are mainly present in ligaments and vascular walls, and are also present in small amounts in tendons and skin. The presence of elastic fibers in combination with collagen fibers imparts elasticity and tensile capabilities to the tissue. The extracted elastin peptide takes desmin and isodesmin as characteristic components. It is particularly emphasized that small molecule elastin peptides are more readily absorbed, industry requires greater than 80% relative molecular mass below 5000.
In the prior art, the problems of poor rehydration, long time, easy rancidity, low efficiency and the like of the dried beef tendon are faced in the beef tendon extraction process, the beef tendon is directly extracted to remove elastin peptide beef tallow, the odor is not influenced, the odor is also influenced due to insufficient removal of other peculiar smell substances in the product, and the color is influenced due to insufficient removal of chromogenic substances, such as sugar, hemoglobin and fatty acid. The existing enterprise records that standard elastin peptide and collagen peptide have similar detection indexes, and is difficult to evaluate the purity of varieties, and researches show that desmin and isodesmin are characteristic components of elastin peptide, and the process for extracting high-purity elastin peptide by using compact connective tissues containing collagen and elastin such as cowhells and the like as the purity standard of elastin peptide is yet to be researched.
Disclosure of Invention
The method solves the technical problem that sodium chondroitin sulfate, elastin peptide and collagen peptide cannot be extracted from the beef tendon simultaneously in the prior art, solves the problems of low extraction purity, low comprehensive benefit and large pollution of the elastin peptide in the beef tendon in the prior art, and promotes the green and energy-saving steady development of industry and the continuous expansion of scale. The invention aims to provide an extraction process of chondroitin sodium sulfate, elastin peptide and collagen peptide, which has the advantages of low process modification cost, high raw material utilization rate, good comprehensive benefit and environmental protection; the quality of the product reaches national standard, exceeds line standard, such as high content of chain element in elastin peptide, and low molecular weight of peptide.
The invention provides an extraction process of chondroitin sodium sulfate, elastin peptide and collagen peptide, which comprises the following steps:
S1, preprocessing beef tendons;
S2, subcritical extraction degreasing is carried out on the beef tendon;
s3, alkaline water leaching, and carrying out solid-liquid separation to obtain filter residues and alkaline water extract;
S3.1, collecting filter residues obtained in the step S3, steaming the filter residues, carrying out enzymolysis on the filter residues by composite protease, regulating pH, standing and filtering to obtain filtrate;
s3.2, respectively passing the filtrate through strong acid type cation exchange resin, strong base type anion exchange resin and weak base type macroporous resin, and collecting effluent;
s3.3, performing precise filtration, nanofiltration, double-effect concentration, sterilization and spray drying on the effluent liquid to obtain elastin peptide;
s4, collecting the alkaline water extract solution after solid-liquid separation in the S3;
S4.1, carrying out enzymolysis, filter pressing, cation exchange resin, anion exchange resin and weak base type macroporous resin on the alkaline water extract, and collecting effluent;
s4.2, performing precise filtration, nanofiltration, double-effect concentration, sterilization and spray drying on the effluent to obtain collagen peptide;
s5, eluting the adsorbate on the anion exchange resin in the step S4.1 to obtain eluent;
S5.1, precisely filtering, ultrafiltering, precipitating with ethanol, dehydrating and drying the eluent to obtain the chondroitin sulfate sodium.
In the invention, the types of the beef tendons comprise beef tendons, beef plate tendons and beef ligaments.
In the step S1, the pretreatment is carried out by removing impurities from fresh beef tendon, washing with water, soaking in acid water, freezing and slicing, washing, filtering, dehydrating with alcohol and drying in vacuum; wherein, aiming at the characteristics of large toughness and wet skid and difficult processing of the cowhells, a pretreatment step is specially added; the freeze-thawing method can influence the size of ice crystals in animal tissues by controlling the freezing rate, so as to puncture tissue cells; frozen slices, cut into transverse slices, are particularly suitable for mechanical slicing of fresh animal tissues such as muscles, tendons, ligaments and the like; the two methods can improve the efficiency of removing impurities such as heme, nucleic acid, sugar, lactic acid, etc.
In the step S1, the acid water is hydrochloric acid water with a pH value of 1 or acetic acid water solution, preferably acetic acid water solution with a pH value of 1; wherein, the acid soaking water can fix protein in the cowhells tissue.
In the step S1, the addition amount of the acid water is 1 to 2 times of the mass of the beef tendon.
In the step S1, the time of the acid soaking water is 20-30 hours.
In the step S1, the soaked acid water is soaked and washed for 2-3 times by reverse osmosis water, and then frozen and fixed along the direction of the tendon fiber by water with the mass of 0.5 times of that of the tendon; the adding amount of the reverse osmosis water is 2-3 times of the mass of the cowhells.
In the step S1, the section is a slice obtained by cutting cowhells into 0.5-1.0 mm thick slices.
In the step S1, the washing is performed three times by using reverse osmosis water at the temperature of below 10 ℃.
In the step S1, the alcohol is 95% alcohol.
In the step S1, the times of alcohol dehydration are 2 to 4 times, preferably 3 times; wherein, the alcohol can denature and dehydrate animal tissue protein, effectively avoid the adhesion and blocking of slices in the drying process, reduce the drying efficiency and influence the later crushing, and remove part of peculiar smell components with slightly low hydrophilicity.
In the step S1, the temperature of the vacuum drying is 40-60 ℃, preferably 50-60 ℃.
In the further step S1, ethanol recovery equipment is adopted for the vacuum drying.
In a further step S1, the crushing is performed to form particles or fibers.
In S2, the solvent used in the subcritical extraction is a solvent conventionally used in oil extraction, preferably a compound extractant, more preferably a nonpolar solvent such as butane; ethanol can be added into the solvent used for subcritical extraction.
S2, subcritical extraction adopts the temperature which is conventional in the art; the subcritical extraction is a common efficient oil extraction process, has good beef tendon odor removal effect, and can extract fat-soluble components such as beef tallow and remove partial semi-hydrophilic components.
In S2, the working pressure of the subcritical extraction is 0.3-0.6 MPa, and the subcritical extraction temperature is 35-50 ℃.
In S3, the alkaline water is an aqueous sodium hydroxide solution having ph=9.
And S3, the addition amount of the alkaline water is 8-10 times of the mass of the cowhells.
S3, the temperature of the alkaline water leaching is 95-100 ℃; the method comprises the steps of extracting collagen and proteoglycan by using alkaline water to obtain elastin, hydrolyzing, separating, purifying and drying to obtain elastin peptide, and extracting chondroitin sulfate sodium and collagen peptide by using the extracting solution to hydrolyze, separating, purifying and drying to obtain elastin peptide, wherein the purity of the obtained elastin peptide is high, the content of characteristic components of desmin (isodesmin) is higher than that of bonito elastin peptide, and the chondroitin sulfate sodium and collagen peptide reach or exceed the national standard.
And S3, leaching the alkaline water for 2-3 hours.
In S3, the number of times of the alkaline water leaching is 2 to 4, preferably 3.
In S3.1, the heating temperature of the cooking is 120 ℃.
In S3.1, the cooking time is 3-5 hours, preferably 4 hours.
In S3.1 and S4.1, the complex protease is an alkaline protease and a neutral protease, preferably 25wt% alkaline protease and 75wt% neutral protease.
In S3.1 and S4.1, the mass of the compound protease is 0.5% of the mass of the filter residue; wherein, the protease hydrolysis is a hydrolysis method with stronger specificity, and peptides with more concentrated molecular weight can be obtained by enzyme combination.
S3.1 and S4.1, the enzymolysis further comprises the operation of inactivating the enzyme for 0.5 to 1 hour at the temperature of 75 to 80 ℃.
S3.1, performing enzymolysis by adding reverse osmosis water with the mass 4-6 times that of filter residues and adding compound protease.
S3.1, the enzymolysis is carried out for 8-10 hours under the conditions that the pH is 7-8 and the temperature is 40-45 ℃.
In S3.1, the pH value is adjusted to be 4.0-5.0.
S3.1, the filter aid used for filtering is diatomite with a medium-fine ratio of 3/1; the diatomite is generally classified into coarse soil, medium soil and fine soil, and the diatomite is mixed by 3 times of the medium soil and 1 time of the fine soil.
The usage amount of the filter aid used for filtering in the S3.1 is 0.5-1% of the weight of the cowhells.
In S3.3, S4.2 and S5.1, the pore size of the fine filtration was 5. Mu.m.
S3.3 and S4.2 and S5, wherein the aperture of the nanofiltration membrane used for nanofiltration is 150Da.
S3.3 and S4.2, wherein the solid content of the effluent after nanofiltration is 20-25%, and the conductivity is less than or equal to 5mS/cm.
S3.3 and S4.2, wherein the double-effect concentration is to concentrate to a specific gravity of 1.15-1.25 at 50-60 ℃.
S3.3 and S4.2, said sterilization being a routine procedure in the art.
S3.3 and S4.2, wherein the air inlet temperature of spray drying is 160-190 ℃, the air outlet temperature of spray drying is 80-85 ℃, the pressure of spray drying is 12-15 mpa, and the aperture of a spray drying nozzle is 1.2-1.5 mm.
S4.1, the enzymolysis is carried out for 5 to 8 hours under the conditions that the pH is 7 to 9 and the temperature is 50 to 60 ℃.
In S5, the eluent used in the elution is 10% sodium chloride aqueous solution.
S5.1, the aperture of an ultrafiltration membrane used for ultrafiltration is 5000Da.
In S5.1, the alcohol precipitation degree is 60-65%.
In S5.1, the degree of dehydration is 92% or more.
S5.1, wherein the drying temperature is 60-80 ℃.
In the invention, the nanofiltration and ultrafiltration both keep trapped fluid, and the trapped fluid is subjected to the next operation; and the filtrate is reserved in both the precise filtration and the filtration.
Compared with the prior art, the invention has the beneficial effects that:
1. Aiming at the characteristics of toughness and difficult processing of the beef tendon, the pretreatment step is added. Firstly, innovation is carried out from the angles of being convenient for drying, degreasing and removing beef tallow taste, increasing leaching rate, comprehensively utilizing beef tendon and improving utilization rate, and physiological tissue slice acid soaking and solidifying technology, freezing and slicing and puncturing tissue cells to release internal impurities, alcohol dehydration, anti-bonding, drying convenience and vacuum drying are introduced to realize low-temperature puffing and nonpolar solvent oil extraction. The improvement measures improve the efficiency of subcritical extraction of fat-soluble components, effectively remove water-soluble and fat-soluble impurities in the beef tendon, and improve the extraction efficiency and the product quality of the product. In addition, the invention also uses special anion exchange adsorption resin to enrich the sodium chondroitin sulfate, thereby realizing effective extraction effect. It is worth mentioning that the method of the invention is compatible with most production equipment for extracting the chondroitin sodium sulfate and collagen peptide of cow cartilage by the existing enzyme method, and has lower transformation cost.
2. The invention utilizes the cowhells to extract the chondroitin sulfate sodium, the elastin peptide and the collagen peptide, and the product has high extraction yield (1.1 to 1.3 percent of the chondroitin sulfate sodium, 5.3 to 16.5 percent of the elastin peptide, 8.1 to 15.6 percent of the collagen peptide and1 to 1.5 percent of the beef tallow), good quality, high purity and no peculiar smell. Wherein, the content of the desmin and the isodesmin in the elastin peptide is 0.32-1.13%, which exceeds the raw material purchasing standard of elastin peptide of a certain enterprise in China; the peptide content below 5000Da reaches more than 90%, the chondroitin sulfate sodium reaches pharmacopoeia standard, the collagen peptide reaches food standard, and the comprehensive utilization value of the beef tendon is improved.
3. Compared with a single elastin peptide extraction process, the method provided by the invention has the advantages that elastin peptide, collagen peptide and chondroitin sulfate sodium are extracted at the same time, so that the comprehensive utilization rate of the beef tendon is greatly improved, the content of organic matters in wastewater is obviously reduced, the treatment cost is reduced, and the comprehensive utilization value of the beef tendon is obviously improved.
Drawings
Fig. 1 is a flow chart of an extraction process of chondroitin sodium sulfate, elastin peptide and collagen peptide.
Detailed Description
The present invention will be described more fully hereinafter with reference to the preferred embodiments for the purpose of facilitating understanding of the present invention, but the scope of the present invention is not limited to the following specific embodiments.
Unless defined otherwise, all technical and scientific terms used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the scope of the present invention.
The diatomite is generally classified into coarse diatomite, medium diatomite and fine diatomite, different manufacturers slightly differentiate the classification of the diatomite, the diatomite used in the embodiment of the invention is purchased from Jilin Yuantong mining Co Ltd, the medium diatomite model is ZBS300#, the fine diatomite model is BS30#, and the diatomite in the embodiment of the invention is mixed diatomite, and the medium-fine mass ratio is 3/1.
The composite extractant is special for grease equipment manufacturers, the main component is butane, and ethanol is added into some extractants to adjust the polarity of the solvent.
In the invention S3.2, strong acid type cation exchange resin and strong base type anion exchange resin can be used as Rogowski brand; the anion exchange resin in S4.1 requires the use of a special chondroitin adsorption resin for enriching sodium chondroitin sulfate, typically of the rombin brand.
In the following examples, sodium chondroitin sulfate was tested against pharmacopoeia standards; collagen peptide is detected by referring to national standard GB 31645; the elastin peptide is detected by a national standard, and can be referred to as QBT 5936-2023-elastin peptide (the public stage is not approved yet), wherein a content determination method of the desmin/isodesmin is involved (specifically, the desmin/isodesmin is cyclic peptide consisting of 4 lysines and usually appears in the elastin peptide in the form of polypeptide combined with other amino acids, the desmin/isodesmin in the elastin peptide is released from a polypeptide chain by acid hydrolysis treatment, and the released desmin/isodesmin is mixed with ninhydrin at 135 ℃ to form a bluish purple compound after being separated by a sulfonic acid type cation exchange column of an amino acid analyzer, and a derivative product is detected at 570nm wavelength, and the retention time is qualitative and the quantitative analysis is carried out by an external standard method.
Other substances can be referred to Q/HTSW 0004S-2021, the reference standard for bovine ligament elastin peptide in the food safety Enterprise Standard of Guangdong province.
Example 1
Raw materials: northeast fresh cowhells
(1) And taking a certain amount of beef tendon qualified by inspection and quarantine, and carrying out primary screening. Pretreatment of cowhells: removing impurities from fresh beef tendon, soaking in 1 times of acetic acid solution (prepared from reverse osmosis water) with pH=1 for 24 hr, washing with 2 times of water for 2 times, freezing with 0.5 times of beef tendon mass water to form strips, slicing with frozen transverse slice method to obtain 0.5-1.0 mm thick slices, washing with reverse osmosis water below 10deg.C for three times, soaking in 95% ethanol for 3 times, vacuum drying at 50deg.C in ethanol recovery device, and pulverizing to obtain granule. (the multiple in this step means a multiple of the weight of the cowhells)
(2) Degreasing: subcritical extraction of beef tallow, using butane compound extraction solvent for extraction, wherein the extraction working pressure is about 0.5MPa, and the working temperature is 35-50 ℃.
(3) Leaching and separating with alkali water: extracting collagen and proteoglycan with sodium hydroxide aqueous solution with pH=9, wherein filter residue contains elastin; the three times of leaching are carried out, the total amount of sodium hydroxide aqueous solution required by the three times is 8-10 times of the weight of the beef tendon pieces, the first leaching is carried out for 3 hours, the second leaching is carried out for 2 hours, and the third leaching is carried out for 2 hours; the extraction temperature is 95-100 ℃, and the filter residue and alkaline water extract are obtained after solid-liquid separation.
(4) Enzymolysis: collecting residue, and decocting in water (120deg.C) for 4 hr; adding reverse osmosis water with the mass 4-6 times of that of the filter residue, and hydrolyzing with compound enzyme with the mass 0.5% of that of the filter residue (the compound enzyme contains 25wt% of alkaline protease and 75wt% of neutral protease), wherein the enzymolysis is carried out for 8-10 hours under the conditions of pH of 7-8 and temperature of 40-45 ℃; enzyme inactivation is carried out at 75 ℃ for 0.5 hour; the pH value is regulated to 4.0-5.0, and the weight of filter residues used for filtering is 0.5-1% of diatomite. Wherein, the yield is lost when the filter aid is excessively added, so that diatomite accounting for 0.5 to 1 percent of the weight of the filter residue is added for assisting filtration
(5) Purifying: the filtrate sequentially passes through strong acid cation exchange resin, strong base anion exchange resin and weak base macroporous resin, and flows out after collection and passes through a precision filter (aperture is 5 mu m) and nanofiltration (membrane aperture is 150 Da), and is concentrated and desalted until the solid content is 20% -25%, and the conductivity is less than or equal to 3mS/cm.
(6) Concentrating: double-effect vacuum concentration at 50-60 deg.c to 45-50%.
(7) Sterilizing and drying: spray drying at 160-190 deg.c and 80-85 deg.c to obtain elastin peptide.
(8) Extraction of sodium chondroitin sulfate: carrying out enzymolysis on the alkaline aqueous extract liquid of the step (3) [ the same type and quality of enzyme used in the step (4), carrying out enzymolysis for 5-8 h under the conditions of pH of 7-9 and temperature of 50-60 ℃, and then carrying out enzyme inactivation for 1h at 75-80 ℃; filtering by press filtration [ filter aid with step (4), eluting with 10% sodium chloride aqueous solution water ], passing through cation exchange resin, anion exchange resin, weak base macroporous resin, eluting sodium chondroitin sulfate of the retentate of anion exchange resin with 10% sodium chloride aqueous solution water, filtering the eluent by press filtration [ filter aid with step (4), removing impurities such as broken resin, ultrafiltering with 5000Da membrane, processing until ultrafiltrate contains 0.5% -0.8%, solid content is 10% -12%, precipitating the retentate with 3 times of alcohol, controlling alcohol degree in feed liquid to 60% -65%, dehydrating the precipitate with alcohol, dehydrating for 2 times, adding alcohol to ensure that alcohol degree is greater than 92%, drying the dehydrated precipitate with hot air oven, and drying at 75deg.C.
(9) Extraction of collagen peptide: and (3) performing precise filtration, nanofiltration, double-effect concentration, sterilization and spray drying treatment on the effluent liquid of the anion exchange resin adsorbed with the chondroitin sulfate in the step (8) to obtain the collagen peptide. In the step, specific parameters of precise filtration, nanofiltration, double-effect concentration, sterilization and spray drying are the same as those in the steps (5) to (7).
Example 2
Raw materials used northeast fresh beef tendon, and other steps were the same as in example 1.
Example 3
Raw materials used were fresh beef neck ligaments in northeast, and the other steps were the same as in example 1.
The yields of sodium chondroitin sulfate, elastin peptide and collagen peptide obtained in examples 1 to 3 are shown in Table 1.
Comparative example 1
In the embodiment, the beef tendon pretreatment (1) is only washed, dried and crushed; the other steps were the same as in example 1. The yields of the substances are respectively as follows: chondroitin sulfate 0.1%, elastin peptide 14.7%, collagen peptide 1.8%, beef tallow; the content of desmin and isodesmin in the elastin peptide is 0.12%, the color of elastin peptide and collagen peptide is yellow, the fishy smell and the acid smell are heavy, the filtering is smooth, and the diatomite consumption is increased by nearly 5 times compared with that of the example 1.
Comparative example 2
In the embodiment, the beef tendon pretreatment (1) is only washed, dried and crushed; the other steps are the same as in example 1, and the activated carbon decolorization and deodorization treatment process for injection is added, wherein the amount of the activated carbon is 0.5-1wt% of that of elastin peptide hydrolysate and collagen peptide hydrolysate, and the amount of diatomite is almost equal to that of comparative example 1.
The yields of the substances are respectively as follows: chondroitin sulfate 0.1%, elastin peptide 8.7%, collagen peptide 1.5%, beef tallow; the content of desmin and isodesmin in the elastin peptide is 0.18%, and the color of the elastin peptide and collagen peptide is white, so that no obvious peculiar smell is generated.
TABLE 1
| Project | Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 |
| Chondroitin sulfate sodium salt | 1.3％ | 1.1％ | 1.2％ | 0.1％ | 0.1％ |
| Elastin peptides | 5.3％ | 9.3％ | 16.5％ | 14.7％ | 8.7％ |
| Collagen peptide | 15.6％ | 13.5％ | 8.1％ | 1.8％ | 1.5％ |
| Beef tallow | 1.5％ | 1.2％ | 1.0％ | 0％ | 0％ |
The properties of the sodium chondroitin sulfate obtained in examples 1 to 3 were measured, and the data are shown in the summary of the sodium chondroitin sulfate measurement data in Table 2.
TABLE 2
Table 3 is a summary of several enterprise elastin peptide food records standards section indicators.
TABLE 3 Table 3
The elastin peptides obtained in examples 1 to 3 were tested by referring to the standard method of collagen peptide GB31645-2018, and the desmin and isodesmin projects were added (the test index of the raw material of the bonito elastin by referring to a certain health food enterprise in China should be more than 0.1%) and the data are shown in Table 4.
TABLE 4 Table 4
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As can be seen from the data in Table 1, the yields of chondroitin sulfate sodium and collagen peptide in examples 1 to 3 are both stable, and the yield of elastin peptide has a large correlation with the raw material; from the data in tables 2 to 4, it can be seen that the quality of the chondroitin sulfate sodium and the collagen peptide obtained in examples 1 to 3 all reach the quality of the national standard, and the elastin peptide reaches the requirement of the national enterprise record standard, wherein the content of the desmin and the isodesmin exceeds the raw material purchasing standard of the elastin peptide of a certain enterprise in China.
As can be seen from comparative example 1, the elastin peptide extracted from untreated cowhells has low purity, and has heavy yellow color and smell, and can not meet the industry requirements; as can be seen from comparative example 2, the addition of the decolorization and deodorization treatment to the elastin peptide extracted from untreated beef tendon gives a color and smell acceptable product, but the yield is lower and the purity is still smaller than that of the example. It can be seen from table 1 that the total extraction of the non-pretreated cowhells was lower than that of the treated cowhells.
Unless otherwise specifically indicated, the various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or may be prepared by existing methods. While the foregoing is directed to embodiments of the present invention, other and further details of the invention may be had by the present invention, it should be understood that the foregoing description is merely illustrative of the present invention and that no limitations are intended to the scope of the invention, except insofar as modifications, equivalents, improvements or modifications are within the spirit and principles of the invention.
Claims (10)
1. An extraction process of chondroitin sodium sulfate, elastin peptide and collagen peptide is characterized by comprising the following steps:
S1, preprocessing beef tendons;
S2, subcritical extraction degreasing is carried out on the beef tendon;
s3, alkaline water leaching, and carrying out solid-liquid separation to obtain filter residues and alkaline water extract;
S3.1, collecting filter residues obtained in the step S3, steaming the filter residues, carrying out enzymolysis on the filter residues by composite protease, regulating pH, standing and filtering to obtain filtrate;
s3.2, respectively passing the filtrate through strong acid type cation exchange resin, strong base type anion exchange resin and weak base type macroporous resin, and collecting effluent;
s3.3, performing precise filtration, nanofiltration, double-effect concentration, sterilization and spray drying on the effluent liquid to obtain elastin peptide;
s4, collecting the alkaline water extract solution after solid-liquid separation in the S3;
s4.1, carrying out enzymolysis, filter pressing, cation exchange resin, anion exchange resin and weak base type macroporous resin on the alkaline water extract, and collecting effluent;
s4.2, performing precise filtration, nanofiltration, double-effect concentration, sterilization and spray drying on the effluent to obtain collagen peptide;
s5, eluting the adsorbate on the anion exchange resin in the step S4.1 to obtain eluent;
S5.1, precisely filtering, ultrafiltering, precipitating with ethanol, dehydrating and drying the eluent to obtain the chondroitin sulfate sodium.
2. The process for extracting chondroitin sodium sulfate, elastin peptide and collagen peptide according to claim 1, wherein the types of beef tendons comprise beef tendons, beef tendons and beef ligaments.
3. The process for extracting chondroitin sodium sulfate, elastin peptide and collagen peptide according to claim 1, wherein in S1, the pretreatment is performed by removing impurities from fresh beef tendon, washing with water, soaking in acid water, freezing, slicing, washing, draining, dehydrating with alcohol, vacuum drying, and pulverizing;
s2, extracting agent adopted by subcritical extraction is a nonpolar solvent;
in S2, the working pressure of the subcritical extraction is 0.3-0.6 MPa, and the subcritical extraction temperature is 35-50 ℃.
4. The process for extracting chondroitin sodium sulfate, elastin peptide and collagen peptide according to claim 3, wherein in S1, the acid water is hydrochloric acid water or acetic acid water solution with a pH value of 1;
In the S1, after the acid soaking water is used, reverse osmosis water is used for soaking for 2-3 times, and then water with the mass of 0.5 times of that of the beef tendon is used for freezing and fixing along the fiber direction of the beef tendon;
in S1, the alcohol is 95% alcohol;
In S1, the times of alcohol dehydration are 2-4 times;
s1, the temperature of vacuum drying is 40-60 ℃;
s1, crushing into particles or fibers;
In S2, the extracting agent adopted by the subcritical extraction is butane.
5. The process for extracting chondroitin sodium sulfate, elastin peptide and collagen peptide according to claim 1, wherein in S3, the alkaline water is aqueous sodium hydroxide solution having ph=9;
S3, the addition amount of the alkaline water is 8-10 times of the mass of the cowhells;
s3, the temperature of the alkaline water leaching is 95-100 ℃;
S3, leaching the alkaline water for 2-3 hours;
And S3, the number of times of alkaline water leaching is 2-4.
6. The process for extracting chondroitin sodium sulphate, elastin peptide and collagen peptide according to claim 1, wherein in S3.1, the heating temperature of the cooking is 120 ℃;
S3.1, the cooking time is 3-5 hours;
S3.1 and S4.1, wherein the compound protease is alkaline protease and neutral protease;
in S3.1 and S4.1, the mass of the compound protease is 0.5% of the mass of the filter residue;
s3.1 and S4.1, the enzymolysis further comprises the operation of inactivating enzyme for 0.5 to 1 hour at 75 to 80 ℃;
s3.1, performing enzymolysis by adding reverse osmosis water with the mass 4-6 times that of filter residues and then adding compound protease;
S3.1, performing enzymolysis for 8-10 hours under the conditions of pH of 7-8 and temperature of 40-45 ℃;
in S3.1, the pH value is adjusted to be 4.0-5.0.
7. The process for extracting chondroitin sodium sulfate, elastin peptide and collagen peptide according to claim 1, wherein the filter aid used for filtering in S3.1 is diatomaceous earth with a medium to fine ratio of 3/1;
The usage amount of the filter aid used for filtering in the S3.1 is 0.5-1% of the weight of the cowhells.
8. The process for extracting chondroitin sodium sulphate, elastin peptide and collagen peptide according to claim 1, wherein in S3.3, S4.2 and S5.1, the pore size of the fine filtration is 5 μm;
S3.3 and S4.2, wherein the aperture of a nanofiltration membrane used for nanofiltration is 150Da;
s3.3 and S4.2, wherein the double-effect concentration is to concentrate to a specific gravity of 1.15-1.25 at 50-60 ℃;
s3.3 and S4.2, wherein the air inlet temperature of the spray drying is 160-190 ℃, the air outlet temperature of the spray drying is 80-85 ℃, and the pressure of the spray drying is 12-15 mpa.
9. The process for extracting chondroitin sodium sulfate, elastin peptide and collagen peptide according to claim 1, wherein in S4.1, the enzymolysis is carried out for 5-8 hours under the conditions that the pH is 7-9 and the temperature is 50-60 ℃.
10. The process for extracting chondroitin sodium sulfate, elastin peptide and collagen peptide according to claim 1, wherein in S5, the eluent used for eluting is 10% sodium chloride aqueous solution;
s5.1, the aperture of an ultrafiltration membrane used for ultrafiltration is 5000Da;
s5.1, the alcohol precipitation degree is 60% -65%;
S5.1, the degree of dehydration is more than 92%;
S5.1, wherein the drying temperature is 60-80 ℃.
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