CN109369800A - The extracting method of high-purity collagen in a kind of ox bone - Google Patents
The extracting method of high-purity collagen in a kind of ox bone Download PDFInfo
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- CN109369800A CN109369800A CN201811333903.6A CN201811333903A CN109369800A CN 109369800 A CN109369800 A CN 109369800A CN 201811333903 A CN201811333903 A CN 201811333903A CN 109369800 A CN109369800 A CN 109369800A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07K—PEPTIDES
- C07K14/00—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof
- C07K14/435—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof from animals; from humans
- C07K14/78—Connective tissue peptides, e.g. collagen, elastin, laminin, fibronectin, vitronectin, cold insoluble globulin [CIG]
Abstract
The present invention relates to the technical fields of biological collagen preparation, and in particular to the extracting method of high-purity collagen in a kind of ox bone includes the following steps: that S1 cleans fresh ox bone；Clean ox bone is put into reactor and ethanol solution is added by S2, and ox bone slurry is made after ventilation, confined reaction；S3 high pressure homogenizer handles ox bone slurry, forms uniform ox bone slurry；S4 is added acid solution into ox bone slurry and is uniformly mixed, and hits stream process, closed reactor processing through super-pressure, then after high-pressure pulse electric is handled, closed reactor is handled, and filter press is utilized to carry out solid-liquid separation, obtains extracting solution；Extracting solution through hyperfiltration treatment, is collected ultrafiltrate by S4, spray-dried up to collagen；For the purity of collagen of the present invention 98% or more, the yield of collagen improves the bioactivity of collagen 90% or more, improves absorption of human body utilization rate up to 98.5% or more, and extraction time is short.
Description
Technical field
The present invention relates to the technical fields of biological collagen preparation, and in particular to high-purity collagen in a kind of ox bone
Extracting method.
Background technique
Collagen is a kind of native biopolymer of zooblast synthesis, is widely present in the skin of animal, bone, soft
It is the extremely main structural proteins of connective tissue in bone, tooth, tendon, ligament and blood vessel, plays support structure organ, protection
The effect of body.Collagen has stable property, and general processing temperature and short time heating all difficulties make its decomposition, therefore
Difficulty is absorbed by the body, and it is lower to eat utilization rate.
Currently, common extracting mode has chemical method and enzyme edman degradation Edman.Chemical method is with chemical reagent such as acid, alkali certain
At a temperature of promote protein molecule Fragmentation formed small-molecule substance method.The prior art such as Patent No.
The Chinese invention patent of CN201710823158.2 discloses ox bone collagen protein peptides extracting method, comprises the following steps, one,
It is osteoclastic；Two, feeding cleans；Three, feeding boiling, row's soup；Four, hydrolysed filtrate；Five, it is concentrated；Six, drying is dusted；Make full use of ox
Bone discharges some nutriments for being not easy to be discharged inside it all sufficiently by deep processing, can utilize for human body.Again
Such as the Chinese invention patent of patent No. CN201710904024.3, discloses to combine from animal hard bone using acid-enzyme and extract I
The method of collagen type, comprising the following steps: Step 1: carrying out pre-treatment to collagen material, carried out at decalcification with hydrochloric acid later
Reason, 0.01~0.02mol/L of concentration of hydrochloric acid, soaking time are 10~12h；It cleans after decalcification processing to pH3~5；Step 2:
Heating boiling, 90~95 DEG C of boiling temperature, 2~3h；Step 3: it is cooling, protease hydrolyzed is added, protease is pepsin,
Additive amount is 3~the 5 ‰ of collagen material, and hydrolysis temperature is 50~55 DEG C, and 5~7h of enzymolysis time is maintained at pH5~7；Step 4:
Isolated enzymolysis liquid；Step 5: post-processing, obtains bone I-type collagen powder.The present invention extracts I-type collagen, improves
The utility value of edibility bone；Preparation method of the invention is simple, high production efficiency；Using decoloration desalinating process product color
Pool is pure white, with high purity.
In the prior art, for acid system because strong acid reaction is violent, equipment seriously corroded, alkaline process is uncomfortable because racemization occurs
For industrial applications.Enzymatic Extraction is the certain temperature and PH of control, with protease hydrolyzed raw material, is extracted by removal of impurities refined filtration
Collagen, the period is short, and 1-24h terminates, and protein yield is high, and amino acid destroys less, and environmental-friendly, the disadvantage is that molecular weight distribution
Extensively, at high cost, foreign protein is more.Therefore, the extracting method for studying high-purity collagen in a kind of ox bone is of great significance.
Summary of the invention
The present invention is in order to solve the above technical problems, the present invention provides a kind of extraction sides of high-purity collagen in ox bone
Method.
Specifically realized according to following technical scheme:
The extracting method of high-purity collagen, includes the following steps: in a kind of ox bone
S1 removes the meat slag on its surface after cleaning fresh ox bone with clear water, then cleaned with citric acid solution；
Clean ox bone is put into reactor and ethanol solution is added by S2, after ventilation to temperature is 110-130 DEG C, stops ventilation
And pressure is adjusted as under the conditions of 80-95MPa, after confined reaction 1-2h, then high-speed stirred forms pulpous state, crosses 60 meshes, obtains ox
Pulp；
S3 high pressure homogenizer handles ox bone slurry, and material is sprayed from current restricting slit, turbulent shear, collision, keeps material super
It is refined into minimum particle, forms uniform ox bone slurry；
S4 is added acid solution into ox bone slurry and is uniformly mixed, and after super-pressure hits stream process 10-15min, closed
After reaction kettle handles 20-30min, by mixed solution after high-pressure pulse electric handles 60-90s, closed reactor handles 20-
After 30min, solid-liquid separation is carried out using filter press, obtains extracting solution；
Extracting solution through hyperfiltration treatment, is collected ultrafiltrate by S5, spray-dried up to collagen.
The mass concentration of the citric acid solution is 7-10%.
The additional amount of the ethanol solution is to clean 4-7 times of ox bone quality.
The mass concentration of the ethanol solution is 45-50%.
The ventilation refers to nitrogen and carbon dioxide gas mixture, wherein the amount ratio of nitrogen and carbon dioxide is (3-
5):1。
The acid solution is the organic acid soln that mass concentration is 55-65%.
The organic acid is by following parts by weight meter material composition: 8-11 parts of lactic acid, 4-7 parts of tartaric acid, 1-2 parts of galla turcicas
Acid, 2-5 parts of acetic acid.
The additional amount of the acid solution is to clean 5-6 times of ox bone quality.
It is 180-230MPa that the super-pressure, which hits pressure in stream process, and hitting distance is 2-4mm.
Electric field strength is 10-14kV/cm, umber of pulse 10-15 in the high-pressure pulse electric processing.
The molecular weight of the ultrafiltration membrane is ten thousand dalton of 0.1-0.7.
The beneficial effects of the present invention are:
Collagen is extracted using the method for the present invention, 98% or more, the yield of collagen exists the purity of collagen
90% or more, it improves the bioactivity of collagen, improves absorption of human body utilization rate up to 98.5% or more, and extraction time
It is short.
Firstly, the present invention utilizes citric acid treatment ox bone, ox bone surface grease and calcareous ingredient are removed；Secondly, of the invention
Ethyl alcohol and ventilation treatment are utilized in pulping process, so that the impurity components such as calcium constituent are transferred to organic phase from water phase, improve glue
The yield and purity of former albumen；Finally, collagen is extracted using acid solution, in conjunction with super-pressure percussion flow, effectively destruction glue
The rock-steady structure of former albumen generates galvanomagnetic-effect in conjunction with high-pressure pulse electric, shortens extraction time, and tropocollagen molecule chain is not
It can be interrupted, and then will not tropocollagen molecule be degraded, improve the bioactivity of collagen.
Specific embodiment
Specific embodiments of the present invention will be described in further detail below, but the invention is not limited to these realities
Mode is applied, it is claimed to still fall within the claims in the present invention for any improvement or replacement on the present embodiment essence spirit
Range.
Embodiment 1
The extracting method of high-purity collagen, includes the following steps: in a kind of ox bone
S1 removes the meat slag on its surface after cleaning fresh ox bone with clear water, the citric acid for being then 10% with mass concentration
Solution is cleaned；
The ethanol solution that clean ox bone is put into and clean 7 times of ox bone quality is added in reactor by S2, mass concentration is 50%,
After ventilation to temperature is 130 DEG C, stop ventilating and adjust under the conditions of pressure is 95MPa, after confined reaction 2h, then high-speed stirred shape
Pulp crosses 60 meshes, obtains ox bone slurry；
S3 high pressure homogenizer handles ox bone slurry, and material is sprayed from current restricting slit, turbulent shear, collision, keeps material super
It is refined into minimum particle, forms uniform ox bone slurry；
S4 to ox bone starch in be added mass concentration be 65% organic acid soln be uniformly mixed, and through super-pressure percussion flow at
After managing 15min, after closed reactor handles 30min, by mixed solution after high-pressure pulse electric handles 90s, closed reactor
After handling 30min, solid-liquid separation is carried out using filter press, obtains extracting solution；
Extracting solution through hyperfiltration treatment, is collected ultrafiltrate by S5, spray-dried up to collagen；
The ventilation refers to nitrogen and carbon dioxide gas mixture, wherein the amount ratio of nitrogen and carbon dioxide is 5:1；
The organic acid is by following material composition: 11kg lactic acid, 7kg tartaric acid, 2kg gallic acid, 5kg acetic acid；
The additional amount of the organic acid soln is to clean 6 times of ox bone quality；
It is 230MPa that the super-pressure, which hits pressure in stream process, and hitting distance is 4mm；
Electric field strength is 14kV/cm, umber of pulse 15 in the high-pressure pulse electric processing；
The molecular weight of the ultrafiltration membrane is 0.7 ten thousand dalton.
Embodiment 2
The extracting method of high-purity collagen, includes the following steps: in a kind of ox bone
S1 removes the meat slag on its surface after cleaning fresh ox bone with clear water, the citric acid for being then 7% with mass concentration
Solution is cleaned；
The ethanol solution that clean ox bone is put into and clean 4 times of ox bone quality is added in reactor by S2, mass concentration is 45%,
After ventilation to temperature is 110 DEG C, stop ventilating and adjust under the conditions of pressure is 80MPa, after confined reaction 1h, then high-speed stirred shape
Pulp crosses 60 meshes, obtains ox bone slurry；
S3 high pressure homogenizer handles ox bone slurry, and material is sprayed from current restricting slit, turbulent shear, collision, keeps material super
It is refined into minimum particle, forms uniform ox bone slurry；
S4 to ox bone starch in be added mass concentration be 55% organic acid soln be uniformly mixed, and through super-pressure percussion flow at
After managing 10min, after closed reactor handles 20min, by mixed solution after high-pressure pulse electric handles 60s, closed reactor
After handling 20min, solid-liquid separation is carried out using filter press, obtains extracting solution；
Extracting solution through hyperfiltration treatment, is collected ultrafiltrate by S5, spray-dried up to collagen；
The ventilation refers to nitrogen and carbon dioxide gas mixture, wherein the amount ratio of nitrogen and carbon dioxide is 3:1；
The organic acid is by following material composition: 8kg lactic acid, 4kg tartaric acid, 1kg gallic acid, 2kg acetic acid；
The additional amount of the organic acid soln is to clean 5 times of ox bone quality；
It is 180MPa that the super-pressure, which hits pressure in stream process, and hitting distance is 2mm；
Electric field strength is 10kV/cm, umber of pulse 10 in the high-pressure pulse electric processing；
The molecular weight of the ultrafiltration membrane is 0.1 ten thousand dalton.
Embodiment 3
The extracting method of high-purity collagen, includes the following steps: in a kind of ox bone
S1 removes the meat slag on its surface after cleaning fresh ox bone with clear water, the citric acid for being then 8% with mass concentration
Solution is cleaned；
The ethanol solution that clean ox bone is put into and clean 5 times of ox bone quality is added in reactor by S2, mass concentration is 48%,
After ventilation to temperature is 120 DEG C, stop ventilating and adjust under the conditions of pressure is 85MPa, after confined reaction 1.5h, then high-speed stirred
Pulpous state is formed, 60 meshes are crossed, obtains ox bone slurry；
S3 high pressure homogenizer handles ox bone slurry, and material is sprayed from current restricting slit, turbulent shear, collision, keeps material super
It is refined into minimum particle, forms uniform ox bone slurry；
S4 to ox bone starch in be added mass concentration be 60% organic acid soln be uniformly mixed, and through super-pressure percussion flow at
After managing 12min, after closed reactor handles 25min, by mixed solution after high-pressure pulse electric handles 75s, closed reactor
After handling 25min, solid-liquid separation is carried out using filter press, obtains extracting solution；
Extracting solution through hyperfiltration treatment, is collected ultrafiltrate by S5, spray-dried up to collagen；
The ventilation refers to nitrogen and carbon dioxide gas mixture, wherein the amount ratio of nitrogen and carbon dioxide is 4:1；
The organic acid is by following material composition: 9.5kg lactic acid, 5kg tartaric acid, 1.5kg gallic acid, 3kg acetic acid；
The additional amount of the organic acid soln is to clean 5.6 times of ox bone quality；
It is 200MPa that the super-pressure, which hits pressure in stream process, and hitting distance is 3mm；
Electric field strength is 12kV/cm, umber of pulse 12 in the high-pressure pulse electric processing；
The molecular weight of the ultrafiltration membrane is 0.5 ten thousand dalton.
Embodiment 4
The extracting method of high-purity collagen, includes the following steps: in a kind of ox bone
S1 removes the meat slag on its surface after cleaning fresh ox bone 50kg with clear water, the lemon for being then 9% with mass concentration
Lemon acid solution is cleaned；
The ethanol solution that clean ox bone is put into and clean 6 times of ox bone quality is added in reactor by S2, mass concentration is 50%,
After ventilation to temperature is 120 DEG C, stop ventilating and adjust under the conditions of pressure is 90MPa, after confined reaction 1h, then high-speed stirred shape
Pulp crosses 60 meshes, obtains ox bone slurry；
S3 high pressure homogenizer handles ox bone slurry, and material is sprayed from current restricting slit, turbulent shear, collision, keeps material super
It is refined into minimum particle, forms uniform ox bone slurry；
S4 to ox bone starch in be added mass concentration be 60% organic acid soln be uniformly mixed, and through super-pressure percussion flow at
After managing 10min, after closed reactor handles 25min, by mixed solution after high-pressure pulse electric handles 60s, closed reactor
After handling 20min, solid-liquid separation is carried out using filter press, obtains extracting solution；
Extracting solution through hyperfiltration treatment, is collected ultrafiltrate by S5, spray-dried up to collagen；
The ventilation refers to nitrogen and carbon dioxide gas mixture, wherein the amount ratio of nitrogen and carbon dioxide is 3.5:
1；
The organic acid is by following material composition: 10kg lactic acid, 6kg tartaric acid, 2kg gallic acid, 4kg acetic acid；
The additional amount of the organic acid soln is to clean 5.5 times of ox bone quality；
It is 205MPa that the super-pressure, which hits pressure in stream process, and hitting distance is 3mm；
Electric field strength is 13kV/cm, umber of pulse 10 in the high-pressure pulse electric processing；
The molecular weight of the ultrafiltration membrane is 0.4 ten thousand dalton.
Comparative example 1
The extracting method of high-purity collagen, includes the following steps: in a kind of ox bone
S1 removes the meat slag on its surface after cleaning fresh ox bone 50kg with clear water, the lemon for being then 9% with mass concentration
Lemon acid solution is cleaned；
The ethanol solution that clean ox bone is put into and clean 6 times of ox bone quality is added in reactor by S2, mass concentration is 50%,
After ventilation to temperature is 120 DEG C, stop ventilating and adjust under the conditions of pressure is 90MPa, after confined reaction 1h, then high-speed stirred shape
Pulp crosses 60 meshes, obtains ox bone slurry；
S3 high pressure homogenizer handles ox bone slurry, and material is sprayed from current restricting slit, turbulent shear, collision, keeps material super
It is refined into minimum particle, forms uniform ox bone slurry；
The organic acid soln that mass concentration is 60% is added into ox bone slurry and is uniformly mixed by S4, and handles through closed reactor
After 25min, by mixed solution through high-pressure pulse electric handle 60s after, closed reactor handle 20min after, using filter press into
The separation of row solid-liquid, obtains extracting solution；
Extracting solution through hyperfiltration treatment, is collected ultrafiltrate by S5, spray-dried up to collagen；
The ventilation refers to nitrogen and carbon dioxide gas mixture, wherein the amount ratio of nitrogen and carbon dioxide is 3.5:
1；
The organic acid is by following material composition: 10kg lactic acid, 6kg tartaric acid, 2kg gallic acid, 4kg acetic acid；
The additional amount of the organic acid soln is to clean 5.5 times of ox bone quality；
Electric field strength is 13kV/cm, umber of pulse 10 in the high-pressure pulse electric processing；
The molecular weight of the ultrafiltration membrane is 0.4 ten thousand dalton.
Comparative example 2
The extracting method of high-purity collagen, includes the following steps: in a kind of ox bone
S1 removes the meat slag on its surface after cleaning fresh ox bone 50kg with clear water, the lemon for being then 9% with mass concentration
Lemon acid solution is cleaned；
The ethanol solution that clean ox bone is put into and clean 6 times of ox bone quality is added in reactor by S2, mass concentration is 50%,
After ventilation to temperature is 120 DEG C, stop ventilating and adjust under the conditions of pressure is 90MPa, after confined reaction 1h, then high-speed stirred shape
Pulp crosses 60 meshes, obtains ox bone slurry；
S3 high pressure homogenizer handles ox bone slurry, and material is sprayed from current restricting slit, turbulent shear, collision, keeps material super
It is refined into minimum particle, forms uniform ox bone slurry；
S4 to ox bone starch in be added mass concentration be 60% organic acid soln be uniformly mixed, and through super-pressure percussion flow at
After managing 10min, after closed reactor handles 45min, solid-liquid separation is carried out using filter press, obtains extracting solution；
Extracting solution through hyperfiltration treatment, is collected ultrafiltrate by S5, spray-dried up to collagen；
The ventilation refers to nitrogen and carbon dioxide gas mixture, wherein the amount ratio of nitrogen and carbon dioxide is 3.5:
1；
The organic acid is by following material composition: 10kg lactic acid, 6kg tartaric acid, 2kg gallic acid, 4kg acetic acid；
The additional amount of the organic acid soln is to clean 5.5 times of ox bone quality；
It is 205MPa that the super-pressure, which hits pressure in stream process, and hitting distance is 3mm；
The molecular weight of the ultrafiltration membrane is 0.4 ten thousand dalton.
Comparative example 3
The extracting method of high-purity collagen, includes the following steps: in a kind of ox bone
S1 removes the meat slag on its surface after cleaning fresh ox bone 50kg with clear water, the lemon for being then 9% with mass concentration
Lemon acid solution is cleaned；
The ethanol solution that clean ox bone is put into and clean 6 times of ox bone quality is added in reactor by S2, mass concentration is 50%,
After ventilation to temperature is 120 DEG C, stop ventilating and adjust under the conditions of pressure is 90MPa, after confined reaction 1h, then high-speed stirred shape
Pulp crosses 60 meshes, obtains ox bone slurry；
S3 high pressure homogenizer handles ox bone slurry, and material is sprayed from current restricting slit, turbulent shear, collision, keeps material super
It is refined into minimum particle, forms uniform ox bone slurry；
The hydrochloric acid solution that mass concentration is 60% is added into ox bone slurry and is uniformly mixed by S4, and hits stream process through super-pressure
After 10min, after closed reactor handles 25min, by mixed solution after high-pressure pulse electric handles 60s, at closed reactor
After managing 20min, solid-liquid separation is carried out using filter press, obtains extracting solution；
Extracting solution through hyperfiltration treatment, is collected ultrafiltrate by S5, spray-dried up to collagen；
The ventilation refers to nitrogen and carbon dioxide gas mixture, wherein the amount ratio of nitrogen and carbon dioxide is 3.5:
1；
The additional amount of the hydrochloric acid solution is to clean 5.5 times of ox bone quality；
It is 205MPa that the super-pressure, which hits pressure in stream process, and hitting distance is 3mm；
Electric field strength is 13kV/cm, umber of pulse 10 in the high-pressure pulse electric processing；
The molecular weight of the ultrafiltration membrane is 0.4 ten thousand dalton.
Comparative example 4
The extracting method of high-purity collagen, includes the following steps: in a kind of ox bone
S1 removes the meat slag on its surface after cleaning fresh ox bone 50kg with clear water, the lemon for being then 9% with mass concentration
Lemon acid solution is cleaned；
The ethanol solution that clean ox bone is put into and clean 6 times of ox bone quality is added in reactor by S2, mass concentration is 50%,
After ventilation to temperature is 120 DEG C, stop ventilating and adjust under the conditions of pressure is 90MPa, after confined reaction 1h, then high-speed stirred shape
Pulp crosses 60 meshes, obtains ox bone slurry；
S3 high pressure homogenizer handles ox bone slurry, and material is sprayed from current restricting slit, turbulent shear, collision, keeps material super
It is refined into minimum particle, forms uniform ox bone slurry；
The animal protein enzyme solutions that mass concentration is 60% are added into ox bone slurry and are uniformly mixed by S4, and hit through super-pressure
It is closed anti-by mixed solution after high-pressure pulse electric handles 60s after closed reactor handles 25min after stream process 10min
After answering kettle to handle 20min, solid-liquid separation is carried out using filter press, obtains extracting solution；
Extracting solution through hyperfiltration treatment, is collected ultrafiltrate by S5, spray-dried up to collagen；
The ventilation refers to nitrogen and carbon dioxide gas mixture, wherein the amount ratio of nitrogen and carbon dioxide is 3.5:
1；
The additional amount of the animal protein enzyme solutions is to clean 5.5 times of ox bone quality；
It is 205MPa that the super-pressure, which hits pressure in stream process, and hitting distance is 3mm；
Electric field strength is 13kV/cm, umber of pulse 10 in the high-pressure pulse electric processing；
The molecular weight of the ultrafiltration membrane is 0.4 ten thousand dalton.
Test example
The hydroxyproline for accurately weighing 5.0mg is dissolved in a small amount of water, is settled to 100mL, and concentration is the standard of 0.05mg/mL
Then solution takes standard solution 0.05,0.125,0.25,0.375,0.5mL, be separately added into 0.1mol/L sodium acetate to 1mL, benefit
With high effective liquid chromatography for measuring absorbance, standard curve is drawn；
Then then the sample 5.0mg of Example 4 and comparative example 1-4 configures the sample solution of 0.05mg/mL, benefit
With high effective liquid chromatography for measuring absorbance and combined standard curve, collagen content is obtained, and calculate collagen and mention
Take rate and purity, wherein collagen recovery rate=(collagen weight × example weight in sample)/(ox bone collagen albumen
Weight × ox bone weight)；Collagen weight/example weight in collagen purity=sample；The results are shown in Table 1:
Table 1
| Embodiment 4 | Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 | |
| Recovery rate (%) | 93.2 | 86.5 | 80.3 | 95.4 | 90.5 |
| Purity (%) | 98.6 | 94.1 | 95.7 | 89.4 | 88.3 |
Test example 2
The measurement of content of beary metal is carried out to embodiment 1- embodiment 4: inorganic arsenic, total arsenic are according to GB/T5009.11 " food
In total arsenic and inorganic arsenic measurement " detected, lead (in terms of Pb) is examined according to GB5009.12 " measurement of Pb in food "
It surveys, cadmium (in terms of Cd) is detected according to GB/T5009.15 " measurement of cadmium in foods ", and mercury (in terms of methyl mercury) is according to GB/
T5009.17 " measurement of total mercury and organic mercury in food " is detected, and the results are shown in Table 2:
Table 2
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | |
| Inorganic arsenic (mg/kg) | 0.12 | 0.08 | 0.10 | 0.07 |
| Total arsenic (mg/kg) | 0.23 | 0.18 | 0.20 | 0.15 |
| Cadmium (mg/kg) | <0.01 | <0.01 | <0.01 | <0.01 |
| Lead (mg/kg) | 0.03 | 0.05 | 0.05 | 0.04 |
| Mercury (mg/kg) | <0.01 | <0.01 | <0.01 | <0.01 |
Claims (10)
1. the extracting method of high-purity collagen in a kind of ox bone, which comprises the steps of:
S1 removes the meat slag on its surface after cleaning fresh ox bone with clear water, then cleaned with citric acid solution；
Clean ox bone is put into reactor and ethanol solution is added by S2, after ventilation to temperature is 110-130 DEG C, stops ventilating and adjust
Under the conditions of seamless power is 80-95MPa, after confined reaction 1-2h, then high-speed stirred forms pulpous state, crosses 60 meshes, obtains ox bone slurry；
S3 high pressure homogenizer handles ox bone slurry, and material is sprayed from current restricting slit, turbulent shear, and collision makes material fining
At minimum particle, uniform ox bone slurry is formed；
S4 is added acid solution into ox bone slurry and is uniformly mixed, and after super-pressure hits stream process 10-15min, confined reaction
After kettle handles 20-30min, by mixed solution after high-pressure pulse electric handles 60-90s, closed reactor handles 20-30min
Afterwards, solid-liquid separation is carried out using filter press, obtains extracting solution；
Extracting solution through hyperfiltration treatment, is collected ultrafiltrate by S5, spray-dried up to collagen.
2. the extracting method of high-purity collagen in ox bone as described in claim 1, which is characterized in that the citric acid solution
Mass concentration is 7-10%.
3. the extracting method of high-purity collagen in ox bone as described in claim 1, which is characterized in that the ethanol solution adds
Entering amount is to clean 4-7 times of ox bone quality.
4. the extracting method of high-purity collagen in ox bone as described in claim 1, which is characterized in that the matter of the ethanol solution
Amount concentration is 45-50%.
5. the extracting method of high-purity collagen in ox bone as described in claim 1, which is characterized in that the ventilation refers to nitrogen
With carbon dioxide gas mixture, wherein the amount ratio of nitrogen and carbon dioxide is (3-5): 1.
6. the extracting method of high-purity collagen in ox bone as described in claim 1, which is characterized in that the acid solution is matter
Measure the organic acid soln that concentration is 55-65%.
7. the extracting method of high-purity collagen in ox bone as described in claim 1, which is characterized in that the organic acid is by as follows
Parts by weight meter material composition: 8-11 parts of lactic acid, 4-7 parts of tartaric acid, 1-2 parts of gallic acids, 2-5 parts of acetic acid.
8. the extracting method of high-purity collagen in ox bone as described in claim 1, which is characterized in that the super-pressure percussion flow
Pressure is 180-230MPa in processing, and hitting distance is 2-4mm.
9. the extracting method of high-purity collagen in ox bone as described in claim 1, which is characterized in that the high-pressure pulse electric
Electric field strength is 10-14kV/cm, umber of pulse 10-15 in processing.
10. the extracting method of high-purity collagen in ox bone as described in claim 1, which is characterized in that point of the ultrafiltration membrane
Son amount is ten thousand dalton of 0.1-0.7.
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| CN106939325A (en) * | 2016-01-05 | 2017-07-11 | 许昌学院 | A kind of preparation method of ox bone collagen albumen |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5138030A (en) * | 1989-10-10 | 1992-08-11 | Pachence James M | Process for extracting type I collagen form an avian source, and applications therefor |
| CN101792382A (en) * | 2010-03-10 | 2010-08-04 | 宋艳 | Method for preparing disinfected-decolorized fish-squamosum organic acid calcium and non-denatured collagen |
| CN106939325A (en) * | 2016-01-05 | 2017-07-11 | 许昌学院 | A kind of preparation method of ox bone collagen albumen |
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