CN111041058A - Preparation method of donkey bone collagen powder, donkey bone powder and donkey bone oil - Google Patents
Preparation method of donkey bone collagen powder, donkey bone powder and donkey bone oil Download PDFInfo
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Abstract
本发明提供了一种驴骨胶原粉、驴骨粉和驴骨油的制备方法，包括如下步骤：(1)分骨；(2)冷冻；(3)碎骨；(4)初步脱脂得到粗制骨油；(5)干燥粉碎得到粗制骨粉；(6)二次脱脂得到粗制骨油，与步骤(4)得到的粗制骨油合并经精制得到精制驴骨油；(7)提取得到精制骨粉。本发明所述的驴骨胶原粉速溶性好、分子量小、易吸收，可迅速补充组织流失的胶原蛋白，广泛应用于化妆品、运动饮料、医药保健品行业中。同时，由本发明制得的驴骨油，颜色淡黄、清亮，含有大量人体所必需的不饱和脂肪酸，应用前景广阔；另精制骨粉中尚含有丰富的矿物质及部分驴骨胶原蛋白，可应用于饲料和化肥行业。
The invention provides a preparation method of donkey bone collagen powder, donkey bone powder and donkey bone oil, comprising the following steps: (1) dividing bones; (2) freezing; (3) breaking bones; (4) preliminary degreasing to obtain crude Bone oil; (5) drying and pulverizing to obtain crude bone meal; (6) secondary defatting to obtain crude bone oil, which is combined with the crude bone oil obtained in step (4) and refined to obtain refined donkey bone oil; (7) extraction to obtain Refined bone meal. The donkey bone collagen powder of the invention has good instant solubility, small molecular weight and easy absorption, can quickly replenish the collagen lost by tissue, and is widely used in the industries of cosmetics, sports drinks and medical and health care products. At the same time, the donkey bone oil prepared by the invention is light yellow and clear in color, contains a large amount of unsaturated fatty acids necessary for the human body, and has broad application prospects; in addition, the refined bone meal still contains abundant minerals and part of donkey bone collagen, which can be applied in the feed and fertilizer industry.
Description
Technical Field
The invention belongs to the field of deep processing of animal bone products, and particularly relates to a preparation method of donkey bone collagen powder, donkey bone meal and donkey bone oil.
Background
The influence of the traditional health preserving culture of donkey-hide gelatin, donkey-nourishing and derivative products become a pillar type industry in a chatting place, the traditional donkey-hide gelatin is prepared by decocting donkey skin, and the application of donkey bones has no feasible way at present and is mostly processed in a primary processing mode.
The donkey bone contains rich ossein, mineral substances and unsaturated fatty acid, and has the effects of tonifying kidney, nourishing yin, and strengthening tendons and bones. At present, the donkey bone collagen is extracted in a high-temperature cooking mode, so that the energy consumption is high, more wastes are generated, and the environment is polluted.
Disclosure of Invention
In view of the above, the invention aims to provide a preparation method of donkey bone collagen powder, donkey bone powder and donkey bone oil, which takes fresh donkey bones as raw materials, prepares the donkey bone collagen, the donkey bone powder and the donkey bone oil by an enzyme method, and has the advantages of low energy consumption of a processing mode and green and environment-friendly processing process.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
a method for preparing donkey bone collagen powder, donkey bone meal and donkey bone oil comprises the following steps:
(1) dividing bones, taking fresh donkey bones of adult donkey for standby use, wherein the donkey bones comprise ribs, thighbones and spines;
(2) freezing, namely freezing fresh donkey bones at a low temperature not higher than-4 ℃ for 2-24 h;
(3) crushing bone, namely putting the frozen donkey bone into an osteoclast crusher to crush to obtain bone slices with the length of not more than 0.5cm, the width of not more than 0.3cm and the thickness of not more than 0.1 cm;
(4) and (3) performing primary degreasing, namely degreasing by adopting a hydrothermal degreasing process, wherein the ratio of aggregate to water is not less than 1: 10, the temperature is not lower than 60 ℃, and the extraction time is not lower than 30 min; separating to obtain bone chips and defatted solution, refrigerating the defatted solution at 4 deg.C for 2-24 hr, centrifuging the upper layer to obtain crude bone oil;
(5) drying and crushing, namely drying and crushing the degreased bone chips to obtain crude bone powder;
(6) and (3) carrying out secondary degreasing, namely carrying out secondary degreasing on the crude bone powder by adopting a degreasing reagent, wherein the ratio of aggregate to water is not lower than 1: 10, the temperature is not higher than 40 ℃, and the extraction time is not lower than 1 h; separating and drying to obtain prefabricated bone powder, recovering degreasing liquid to obtain crude bone oil, mixing with the crude bone oil obtained in step (4), and refining to obtain refined donkey bone oil;
(7) extracting, hydrolyzing the pre-prepared bone powder after the secondary degreasing treatment by compound protease, inactivating, centrifuging, collecting supernatant, concentrating, refining, drying to obtain donkey bone collagen powder, drying the lower layer solid, pulverizing, and sieving to obtain refined bone powder.
Preferably, in the preliminary degreasing in the step (4), the ratio of the aggregate to the water is not less than 1: 5, the temperature is not lower than 80 ℃.
Preferably, the refrigerating time in the step (4) is 24 hours.
Preferably, the drying step in the step (5) adopts high-temperature forced air drying, the spread thickness is not higher than 0.3cm, the temperature is not lower than 60 ℃, and the time is not lower than 12 h.
Preferably, the degreasing reagent in the step (6) is an alkane compound.
More preferably, the degreasing reagent in the step (6) is n-hexane, cyclohexane, methylcyclopentane, 2-methylpentane or 3-methylpentane.
Preferably, the ratio of the aggregate to the water in the secondary degreasing in the step (6) is not less than 1: 5, the temperature is not higher than 35 ℃, and the extraction time is not lower than 4 h.
Preferably, the complex protease in step (7) is a degradable protease.
More preferably, the compound protease in step (7) is a mixture of two or more of pepsin, trypsin, cathepsin, alkaline protease, papain, bromelain and acid protease.
Preferably, the ratio of the substrate concentration to the enzyme amount in the protease hydrolysis process in the step (7) is (200) -1500) 1, and the enzymolysis temperature is 35-55 ℃; the enzymolysis time is 1-6 h.
Preferably, the inactivation process in the step (7) is to heat the enzymolysis liquid to 80-100 ℃ within 20min and keep the temperature for 10-30 min.
Preferably, in the step (7), the supernatant drying process is a spray drying, microwave drying or freeze drying process, and the moisture content is not higher than 10%.
Compared with the prior art, the preparation method of the donkey bone collagen powder, the donkey bone powder and the donkey bone oil has the following advantages:
the donkey bone collagen powder, donkey bone powder and donkey bone oil are prepared by adopting the process flow, the energy consumption of the processing mode is low, and the processing process is green and environment-friendly. The produced donkey bone collagen powder has good instant solubility, small molecular weight and easy absorption, can quickly supplement collagen lost by tissues, and is widely applied to the industries of cosmetics, sports drinks and medical health care products; the produced donkey bone oil is light yellow and clear, contains a large amount of unsaturated fatty acid necessary for human bodies, and has wide application prospect; the produced refined bone powder contains rich mineral substances and part of donkey bone collagen, and can be applied to the industries of feed and fertilizer.
Drawings
FIG. 1 is a molecular weight distribution curve of a conventional donkey bone collagen powder on the market;
FIG. 2 is a molecular weight distribution curve of donkey bone collagen powder prepared in example 3 of the present invention.
Detailed Description
In order that those skilled in the art will better understand the technical solutions of the present invention, the present invention will be further described in detail with reference to the following embodiments. It is to be understood by persons skilled in the art that the following detailed description is illustrative and not restrictive, and is not to be taken as limiting the scope of the invention.
Unless defined otherwise, technical terms used in the following examples have the same meanings as commonly understood by one of ordinary skill in the art to which the present invention belongs. The test reagents used in the following examples, unless otherwise specified, are all conventional biochemical reagents; the experimental methods are conventional methods unless otherwise specified.
The present invention will be described in detail with reference to examples.
Example 1
A method for preparing donkey bone collagen powder, donkey bone powder and donkey bone oil comprises preparing donkey bone collagen powder, donkey bone powder and donkey bone oil from fresh donkey bone by enzyme method; the preparation method comprises the following steps:
(1) the bone is divided, the bone of the donkey is mainly the ribs, thighbones and spines of adult donkeys, and the bone of the processed donkeys is broken to 15cm and classified according to the parts.
(2) Freezing, and freezing fresh donkey bone at-18 deg.C for 12 hr.
(3) Crushing bone, and breaking by using a bone breaking machine to obtain bone slices with the length of not more than 0.5cm, the width of not more than 0.3cm and the thickness of not more than 0.1 cm.
(4) And (3) performing primary degreasing, namely degreasing by adopting a hydrothermal degreasing process, wherein the ratio of material to liquid is 1: 5, extracting at 90 ℃ for 20 min; separating to obtain bone chips and defatted solution, refrigerating the defatted solution at 4 deg.C for 12 hr, and centrifuging the upper layer to obtain crude bone oil.
(5) Drying by high-temperature blast air, spreading to a thickness of 0.3cm at 60 deg.C for 24 h.
(6) Pulverizing, drying, pulverizing to obtain coarse bone powder with uniform particle, yellow brown color and no fishy smell.
(7) And (3) carrying out secondary degreasing, wherein the crude bone meal is subjected to secondary degreasing by adopting normal hexane, and the material-liquid ratio is 1: 5, extracting for 24 hours at the temperature of 25 ℃; separating and drying to obtain prefabricated bone powder, recovering degreasing liquid to obtain crude bone oil, mixing the crude bone oil obtained in the step (4), and refining to obtain refined donkey bone oil.
(8) Extracting, hydrolyzing the prepared bone powder with compound protease (papain, trypsin and alkaline protease) at 50 deg.C for 5 hr according to the ratio of substrate concentration to enzyme amount (1500: 1); heating the enzymolysis solution to 90 deg.C within 10min, maintaining for 20min, and inactivating; centrifuging, collecting supernatant, concentrating, refining, and spray drying to obtain donkey bone collagen powder with water content of less than or equal to 5.0%; drying the lower layer solid by high temperature and normal pressure blast, crushing and sieving to obtain refined bone powder with water content not more than 5.0%.
Example 2
A method for preparing donkey bone collagen powder, donkey bone powder and donkey bone oil comprises preparing donkey bone collagen powder, donkey bone powder and donkey bone oil from fresh donkey bone by enzyme method; the preparation method comprises the following steps:
(1) the bone is divided, the bone of the donkey is mainly the ribs, thighbones and spines of adult donkeys, and the bone of the processed donkeys is broken to 20cm and classified according to the parts.
(2) Freezing, and freezing fresh donkey bone at-18 deg.C for 24 hr.
(3) Crushing bone, and breaking by using a bone breaking machine to obtain bone slices with the length of not more than 0.5cm, the width of not more than 0.3cm and the thickness of not more than 0.1 cm.
(4) And (3) performing primary degreasing, namely degreasing by adopting a hydrothermal degreasing process, wherein the ratio of material to liquid is 1: 1, extracting at 100 ℃ for 30 min; separating to obtain bone chips and defatted solution, refrigerating the defatted solution at 4 deg.C for 24 hr, and centrifuging the upper layer to obtain crude bone oil.
(5) Drying by high temperature air blast, spreading to thickness of 0.3cm at 70 deg.C for 24 hr.
(6) Pulverizing, drying, pulverizing to obtain coarse bone powder with uniform particle, yellow brown color and no fishy smell.
(7) And (3) carrying out secondary degreasing, wherein the crude bone meal is subjected to secondary degreasing by adopting normal hexane, and the material-liquid ratio is 1: 1, extracting at 25 ℃ for 24 hours; separating and drying to obtain prefabricated bone powder, recovering degreasing liquid to obtain crude bone oil, mixing the crude bone oil obtained in the step (4), and refining to obtain refined donkey bone oil.
(8) Extracting, hydrolyzing the prepared bone powder with compound protease (papain, trypsin and alkaline protease) at 55 deg.C for 5h according to the ratio of substrate concentration to enzyme amount (1000: 1); heating the enzymolysis solution to 100 deg.C within 10min, maintaining for 30min, and inactivating; centrifuging, collecting supernatant, concentrating, refining, and spray drying to obtain donkey bone collagen powder with water content of less than or equal to 5.0%; drying the lower layer solid by high temperature and normal pressure blast, crushing and sieving to obtain refined bone powder with water content not more than 5.0%.
Example 3
A method for preparing donkey bone collagen powder, donkey bone powder and donkey bone oil comprises preparing donkey bone collagen powder, donkey bone powder and donkey bone oil from fresh donkey bone by enzyme method; the preparation method comprises the following steps:
(1) the bone is divided, the bone of the donkey is mainly the ribs, thighbones and spines of adult donkeys, and the bone of the processed donkeys is broken to 20cm and classified according to the parts.
(2) Freezing, and freezing fresh donkey bone at-60 deg.C for 2 hr.
(3) Crushing bone, and breaking by using a bone breaking machine to obtain bone slices with the length of not more than 0.5cm, the width of not more than 0.3cm and the thickness of not more than 0.1 cm.
(4) And (3) performing primary degreasing, namely degreasing by adopting a hydrothermal degreasing process, wherein the ratio of material to liquid is 1: 2, extracting at 100 ℃ for 20 min; separating to obtain bone chips and defatted solution, refrigerating the defatted solution at 4 deg.C for 12 hr, and centrifuging the upper layer to obtain crude bone oil.
(5) Drying by high-temperature blast air, spreading to a thickness of 0.3cm at 60 deg.C for 12 h.
(6) Pulverizing, drying, pulverizing to obtain coarse bone powder with uniform particle, yellow brown color and no fishy smell.
(7) And (3) carrying out secondary degreasing, wherein the crude bone meal is subjected to secondary degreasing by adopting ethyl acetate, and the material-liquid ratio is 1: 1, extracting at 25 ℃ for 24 hours; separating and drying to obtain prefabricated bone powder, recovering degreasing liquid to obtain crude bone oil, mixing the crude bone oil obtained in the step (4), and refining to obtain refined donkey bone oil.
(8) Extracting, hydrolyzing the prepared bone powder for 4h at 45 ℃ by using compound protease (papain, trypsin and alkaline protease) according to the ratio of substrate concentration to enzyme amount (200: 1); heating the enzymolysis solution to 100 deg.C within 10min, maintaining for 10min, and inactivating; centrifuging, collecting supernatant, concentrating, refining, and spray drying to obtain donkey bone collagen powder with water content of less than or equal to 5.0%; drying the lower layer solid by high temperature and normal pressure blast, crushing and sieving to obtain refined bone powder with water content not more than 5.0%.
The indexes of the donkey bone collagen powder, the donkey bone powder and the donkey bone oil prepared in the example 3 are measured.
(1) The appearance of the donkey bone collagen powder is golden yellow and glossy, and the donkey bone collagen powder has good instant property by measuring the solubility of the donkey bone collagen powder. The content (%) of the components is respectively determined by physical and chemical properties: oil (1.82 + -0.32), protein (78.16 + -3.65), water (5.72 + -0.18) and ash (8.32 + -0.25).
(2) The appearance of the donkey bone powder is light yellow, and the donkey bone powder has the following component contents (%) by measuring the physical and chemical properties of the donkey bone powder: oil (1.02 + -0.03), protein (17.20 + -2.52), water (5.37 + -0.24), and ash (69.79 + -1.53).
(3) The appearance of the donkey bone oil is yellowish and glossy, wherein the peroxide value is 9.13 +/-0.93 g/100 g. The total fatty acid content of the ass bone oil was determined by gas chromatography, and the structure is shown in table 1.
TABLE 1 relative content of fatty acids in donkey bone oil
At present, the preparation method of the donkey bone collagen powder is mainly prepared by high-temperature cooking, filtering and concentrating into glue, and the obtained donkey bone collagen powder has large protein molecular weight, is difficult to be absorbed by human bodies, has poor taste, and has the problems of salty and bitter taste and the like.
The molecular weight distributions of commercially available donkey bone collagen powder and donkey bone collagen powder prepared in example 3 of the present invention were determined by exclusion chromatography, and the results are shown in fig. 1 and 2. The result shows that the molecular weight of the donkey bone collagen powder is obviously lower than that of the traditional donkey bone collagen powder sold in the market.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. A preparation method of donkey bone collagen powder, donkey bone meal and donkey bone oil is characterized by comprising the following steps: the method comprises the following steps:
(1) dividing bones, taking fresh donkey bones of adult donkey for standby use, wherein the donkey bones comprise ribs, thighbones and spines;
(2) freezing, namely freezing fresh donkey bones at a low temperature not higher than-4 ℃ for 2-24 h;
(3) crushing bone, namely putting the frozen donkey bone into an osteoclast crusher to crush to obtain bone slices with the length of not more than 0.5cm, the width of not more than 0.3cm and the thickness of not more than 0.1 cm;
(4) and (3) performing primary degreasing, namely degreasing by adopting a hydrothermal degreasing process, wherein the ratio of aggregate to water is not less than 1: 10, the temperature is not lower than 60 ℃, and the extraction time is not lower than 30 min; separating to obtain bone chips and defatted solution, refrigerating the defatted solution at 4 deg.C for 2-24 hr, centrifuging the upper layer to obtain crude bone oil;
(5) drying and crushing, namely drying and crushing the degreased bone chips to obtain crude bone powder;
(6) and (3) carrying out secondary degreasing, namely carrying out secondary degreasing on the crude bone powder by adopting a degreasing reagent, wherein the ratio of aggregate to water is not lower than 1: 10, the temperature is not higher than 40 ℃, and the extraction time is not lower than 1 h; separating and drying to obtain prefabricated bone powder, recovering degreasing liquid to obtain crude bone oil, mixing with the crude bone oil obtained in step (4), and refining to obtain refined donkey bone oil;
(7) extracting, hydrolyzing the pre-prepared bone powder after the secondary degreasing treatment by compound protease, inactivating, centrifuging, collecting supernatant, concentrating, refining, drying to obtain donkey bone collagen powder, drying the lower layer solid, pulverizing, and sieving to obtain refined bone powder.
2. The method for preparing donkey bone collagen powder, donkey bone meal and donkey bone oil according to claim 1, which is characterized in that: in the preliminary degreasing process in the step (4), the ratio of the aggregate to the water is not less than 1: 5, the temperature is not lower than 80 ℃.
3. The method for preparing donkey bone collagen powder, donkey bone meal and donkey bone oil according to claim 1, which is characterized in that: the refrigerating time in the step (4) is 24 h.
4. The method for preparing donkey bone collagen powder, donkey bone meal and donkey bone oil according to claim 1, which is characterized in that: and (3) drying in the drying step in the step (5) by adopting high-temperature air blasting, wherein the spread thickness is not higher than 0.3cm, the temperature is not lower than 60 ℃, and the time is not lower than 12 h.
5. The method for preparing donkey bone collagen powder, donkey bone meal and donkey bone oil according to claim 1, which is characterized in that: the degreasing reagent in the step (6) is an alkane compound, preferably, the degreasing reagent in the step (6) is n-hexane, cyclohexane, methylcyclopentane, 2-methylpentane or 3-methylpentane.
6. The method for preparing donkey bone collagen powder, donkey bone meal and donkey bone oil according to claim 1, which is characterized in that: the proportion ratio of the aggregate to the water in the secondary degreasing in the step (6) is not less than 1: 5, the temperature is not higher than 35 ℃, and the extraction time is not lower than 4 h.
7. The method for preparing donkey bone collagen powder, donkey bone meal and donkey bone oil according to claim 1, which is characterized in that: the compound protease in the step (7) is a degradable protease, preferably, the compound protease in the step (7) is a mixture of two or more of pepsin, trypsin, cathepsin, alkaline protease, papain, bromelain and acid protease.
8. The method for preparing donkey bone collagen powder, donkey bone meal and donkey bone oil according to claim 1, which is characterized in that: the ratio of the substrate concentration to the enzyme amount in the protease hydrolysis process in the step (7) is (200) -1500) 1, and the enzymolysis temperature is 35-55 ℃; the enzymolysis time is 1-6 h.
9. The method for preparing donkey bone collagen powder, donkey bone meal and donkey bone oil according to claim 1, which is characterized in that: the inactivation process in the step (7) is to heat the enzymolysis liquid to 80-100 ℃ within 20min and keep the temperature for 10-30 min.
10. The method for preparing donkey bone collagen powder, donkey bone meal and donkey bone oil according to claim 1, which is characterized in that: in the step (7), the supernatant drying process is a spray drying, microwave drying or freeze drying process, and the moisture content is not higher than 10%.
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