CN103497261A - Chondroitin sulfate production process - Google Patents
Chondroitin sulfate production process Download PDFInfo
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- CN103497261A CN103497261A CN201310492432.4A CN201310492432A CN103497261A CN 103497261 A CN103497261 A CN 103497261A CN 201310492432 A CN201310492432 A CN 201310492432A CN 103497261 A CN103497261 A CN 103497261A
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- chondroitin sulfate
- enzymolysis
- production technique
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- chondroitin
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Abstract
The invention provides a chondroitin sulfate production process. A raw material is crushed to form particles with a diameter of 3-5mm, the particles are placed into an immersion pool, water which is 7-8 times as heavy as the raw material is added into the immersion pool for immersion, the particles are sent into a pulping machine to form a raw material pulp, the raw material pulp is sent into a reaction kettle, is heated and boils, then heat preservation is carried out for 10-15 minutes, and floating oil is taken out after temperature reduction to obtain collagen thermal denaturation liquid; a PH value of thermal denaturation liquid caustic soda is adjusted, bacterial enzymes are added, heat-preservation enzymolysis is carried out for 5-6 hours, the temperature is reduced to be the same as the temperature of cold water, then the temperature is raised to 70-75 DEG C, and heat-preservation is carried out for 10-15 minutes; materials after enzymolysis are clarified and filtered, and a wet-state chondroitin course product is obtained after alcohol precipitation, dehydration and alcohol removal; decoloration, concentration, alcohol precipitation and alcohol removal are carried out on the wet-state chondroitin course product, and a chondroitin fine product is obtained after drying. Mechanical physical degradation is carried out, the chondroitin is prevented from being degraded under a high temperature, the yield rate is improved, production cost is reduced, the yield is improved, the production efficiency is improved, the production is increased and the process is scientific and environmentally friendly.
Description
Technical field
The present invention relates to a kind of production technique of the chondroitin sulfate that contains chondroitin sulfate B in full, belong to the biological chemistry pharmacy field.
Background technology
At present, known process for extracting chondroitin sulfate is to adopt three grades of gradient method to extract, that is: the high-boiling of 4-8 hours hydrolysis is extracted; The salt alkaline hydrolysis of 5-8 hours sodium-chlor and sodium hydroxide extracts; The enzymolysis and extraction of 6 hours acidity, neutrality or Sumizyme MPs; Extracting solution adds nylon filtering cloth with the stainless steel manger and filters, and hydrogenchloride and sodium hydroxide are done PH value adjusting agent, with hydrogen peroxide oxidation, decolour.In the chondroitin sulfate component finally obtained: the highest 12.6 % that can only reach chrondroitin component in full of chondroitin sulfate B, disappearance is serious.Because the products molecule structure is destroyed by high temperature, highly basic and strong oxidizer, have a strong impact on its chemical property, owing to carrying chlorion in composition, easily produce hydrochloric acid again, hydrochloric acid is easy drugs processed, belongs to the state control item, has mild toxicity, selects and purchase difficult, difficult accumulating.In addition, when producing the byproduct of chondroitin sulfate-bone collagen, because it be food, because of the use of hydrogen peroxide, by eating inspection department doubtful, be easily poisoned food, affect product property, quality and security.
Summary of the invention
The present invention be directed to high temperature, highly basic and the strong oxidizer destruction to product self chemical property in traditional chondroitin sulfate sheet production technique, cause the defects such as in product, chrondroitin B content is low, Product Safety is low, provide that a kind of production cost is low, leaching process is not chloride, the production technique of chondroitin sulfate of each chemical composition perfect performance in chrondroitin.
Realize that the technical scheme that above-mentioned purpose adopts is: a kind of production technique of chondroitin sulfate is generated according to following steps:
A, the immersion of getting the raw materials ready: it is the 3-5mm particle that raw material is pulverized with equipment, then is placed in fermentation vat and adds raw material gross weight 7-8 water doubly to be soaked, and soak time 16-48 hour, then send in pulper and make former slip;
B, hydrolysis are extracted: former slip is sent in reactor, and insulation 10-15 minute after the reactor ebuillition of heated, make the collagen protein thermally denature and separate out grease, pulls oil slick after cooling out, obtains collagen protein thermally denature liquid;
C, enzymolysis and extraction: the thermally denature liquid caustic soda is adjusted to pH value, add bacterial enzyme, control reactor rotating speed 130-150 rev/min, insulation enzymolysis 5-6 hour, then be cooled to cold water temperature, and pH value is adjusted in acid, then is warming up to 70-75 ℃, insulation 10-15 minute;
D, filter alcohol precipitation: first the material after enzymolysis is clarified and filtered, filtrate is concentrated into 1/3rd volumes, through alcohol precipitation-dehydration-after processing except alcohol, obtain hygrometric state chrondroitin crude product;
E, decolouring are dried: first to hygrometric state chrondroitin crude product decoloured-concentrate-ol heavy-process except alcohol, then obtain the chrondroitin elaboration after drying.
The all alcohol precipitation supernatant liquor volumes that filter in the alcohol precipitation process are concentrated into to 1/3rd rear insulation 45-50 ℃, through bamboo charcoal, decolour and take off flavor, mend alcohol to 80-85 °, obtain the food grade bone collagen after pure hypostasis drying.
The bacterial enzyme adopted in the enzymolysis and extraction process is driselase, and hydrolysis temperature is 53-55 ℃, and during enzymolysis, pH value is 8.0-8.5, and the weight ratio of enzyme dosage and thermally denature liquid is 6:100.
In the enzymolysis and extraction process, it is a kind of in acetic acid and phosphoric acid that pH value sour adjusting agent used is adjusted in acid, and it is sodium hydroxide that alkali is adjusted pH value alkali adjusting agent used.
In hydrolytic extraction process, the oil slick of pulling out is made polished fat after melting, filtration.
In filtration procedure, putting-down machine adopts disk centrifugal separator, and strainer adopts 0.22 micron filter.
In the decolouring stoving process, what hygrometric state chrondroitin crude product was decoloured to employing is H103 type resin.
Stoving process is that step is dried, and its bake out temperature is respectively 85 ℃, 75 ℃ and 65 ℃.
Compared with prior art, the invention has the beneficial effects as follows:
1, raw material adopts the mechanical type physical property to decompose, and has avoided chrondroitin by high temperature degradation, has improved yield;
2, decompose with directed bacterial enzyme, got rid of salt solution, alkaline hydrolysis and old enzymolysis process, chrondroitin discharges fully, and decomposition technique shortens to 1/3rd man-hour used, and production cost reduces, and yield improves;
3, on the basis of original reactor capacity, because of work simplification, shorten the treatment time, enhance productivity, increase turnout;
4, replace original oxidative decoloration technique with resin, guarantee that the chrondroitin molecular structure is normal;
5, employing as sour adjusting agent, is avoided the toxicity hidden danger of chlorion existence without chloric acid, and the product safety performance is protected;
6, processing waste is recovered reprocessing, reduces production costs, increases auxiliary income; Discharge the science environmental protection in production without any waste liquid, waste vapour and waste residue.
Embodiment
Below in conjunction with embodiment, the present invention will be further described.
Embodiment mono-
Raw material is prepared: 2 tons, the old hog snout bone dried, be crushed to the 3-5 mm particle size, and disintegrating apparatus is preferred for the crusher of plastics industry; Raw material after pulverizing is placed in fermentation vat, adds wherein the water that is equivalent to 8 times of raw material weights, soak 25 hours, then send in pulper and make former slip, concentration paste roller mill in the preferred paper industry use of pulper.
Hydrolysis, enzymolysis and extraction: first the raw material after soaking is sent in reactor, after heated and boiled, insulation is 15 minutes, makes the collagen protein thermally denature and separates out grease, then with cooling water temperature to 53 ℃, pulls oil slick out to process separately; Thermally denature liquid in reactor is carried out to alkali and adjust pH value to 8.5, add 120 kilograms of driselases, 150 rev/mins of reactor speed governing, insulation enzymolysis 5 hours; Then be cooled to cold water temperature, with acetic acid, adjust pH value to 7.0, reactor is warming up to 70 ℃, and is incubated 15 minutes, in order to accelerate enzymatic reaction.
Filter, alcohol precipitation: the material clarification with disk centrifugal separator after to enzymolysis, clear liquor is crossed 0.22 micron filter, filtrate alkali is adjusted PH to 8.0, ultrafiltration and concentration to three/volume; Add the 90%(volume percent) above ethanol, be stirred to mixed solution ethanol volumetric concentration and reach 65%, precipitate 7 hours; With 90% above ethanol dehydration 2 hours, dehydrate except alcohol, obtained hygrometric state chrondroitin crude product with tripod pendulum type batch centrifugal, this hygrometric state chrondroitin crude product CPC content 83-88.5%, and yield is with the freshness of hog snout cartilage, between 35-45%.
Decolouring is dried: get 0.8 ton of hygrometric state chrondroitin crude product and be placed in container, by the dissolved in purified water of its 50 times of weight, be incubated in 40-45 ℃ of environment; Add 250 kilograms of resins in container, with the resin absorption decolouring, except albumen; The decolouring liquid caustic soda is adjusted to pH value to 8.0, destainer is concentrated into to 1/3rd volumes; 70 ° of alcohol precipitations, pure hypostasis is centrifugal except alcohol; Except the material after alcohol in drying baker respectively with the step temperature oven dry of 85 ℃, 75 ℃, 65 ℃; Obtain the chrondroitin elaboration.
In gained chrondroitin elaboration: alcohol residue≤1.5%; Vitriol≤25.5%; Specific rotation-25; HPLC content 98.5%.The enzymolysis liquid phase records: containing Chondroitin A 58.5%; Chrondroitin B23%; Chrondroitin C18.5%.
Embodiment bis-
Production technique is with embodiment mono-, in filtration, alcohol precipitation process, all precipitation solution are concentrated into 1/3rd volumes, in the environment of 45-50 ℃, be incubated, then with bamboo carbon to the concentrated solution flavor that decoloured, mend alcohol to 85%, then carry out alcohol precipitation, the alcohol hypostasis is sent in drying baker respectively with the step temperature oven dry of 85 ℃, 75 ℃, 65 ℃, obtains 160 kilograms of food grade bone collagens.
In the production technique of this chondroitin sulfate, filter, in the alcohol precipitation process, with whizzer, remove when pure, centrifugal bone slag and the foreign protein gone out, through the sterilizing of large tunnel type micro-wave dryer, oven dry; Through micronizer powder process, obtain 18.8 kilograms of feed grade bone meal again.
In the production technique of this chondroitin sulfate, the oil slick fat of pulling out in reactor in hydrolytic extraction process, through melting, filtration, obtain 15.6 kilograms of polished fats, 12.5 kilograms of dregs of fat flower fertilizers.
Claims (8)
1. a production technique of chondroitin sulfate, is characterized in that, according to following steps, generated:
A, the immersion of getting the raw materials ready: it is the 3-5mm particle that raw material is pulverized with equipment, then is placed in fermentation vat and adds raw material gross weight 7-8 water doubly to be soaked, and soak time 16-48 hour, then send in pulper and make former slip;
B, hydrolysis are extracted: former slip is sent in reactor, and insulation 10-15 minute after the reactor ebuillition of heated, make the collagen protein thermally denature and separate out grease, pulls oil slick after cooling out, obtains collagen protein thermally denature liquid;
C, enzymolysis and extraction: the thermally denature liquid caustic soda is adjusted to pH value, add bacterial enzyme, control reactor rotating speed 130-150 rev/min, insulation enzymolysis 5-6 hour, then be cooled to cold water temperature, and pH value is adjusted in acid, then is warming up to 70-75 ℃, insulation 10-15 minute;
D, filter alcohol precipitation: first the material after enzymolysis is clarified and filtered, filtrate is concentrated into 1/3rd volumes, through alcohol precipitation-dehydration-after processing except alcohol, obtain hygrometric state chrondroitin crude product;
E, decolouring are dried: first to hygrometric state chrondroitin crude product decoloured-concentrate-ol heavy-process except alcohol, then obtain the chrondroitin elaboration after drying.
2. production technique of chondroitin sulfate according to claim 1, it is characterized in that, all alcohol precipitation supernatant liquor volumes that filter in the alcohol precipitation process are concentrated into to 1/3rd rear insulation 45-50 ℃, through the de-flavor of bamboo charcoal decolouring, mend alcohol to 80-85 °, obtain the food grade bone collagen after pure hypostasis drying.
3. production technique of chondroitin sulfate according to claim 1 and 2, it is characterized in that, the bacterial enzyme adopted in the enzymolysis and extraction process is driselase, and hydrolysis temperature is 53-55 ℃, during enzymolysis, pH value is 8.0-8.5, and the weight ratio of enzyme dosage and thermally denature liquid is 6:100.
4. production technique of chondroitin sulfate according to claim 1 and 2, is characterized in that, in the enzymolysis and extraction process, it is a kind of in acetic acid and phosphoric acid that pH value sour adjusting agent used is adjusted in acid, and it is sodium hydroxide that alkali is adjusted pH value alkali adjusting agent used.
5. production technique of chondroitin sulfate according to claim 1 and 2, is characterized in that, in hydrolytic extraction process, the oil slick of pulling out is made polished fat after melting, filtration.
6. production technique of chondroitin sulfate according to claim 1 and 2, is characterized in that, in filtration procedure, putting-down machine adopts disk centrifugal separator, and strainer adopts 0.22 micron filter.
7. production technique of chondroitin sulfate according to claim 1, is characterized in that, in the decolouring stoving process, what hygrometric state chrondroitin crude product was decoloured to employing is H103 type resin.
8. production technique of chondroitin sulfate according to claim 1 and 2, is characterized in that, described stoving process is that step is dried, and its bake out temperature is respectively 85 ℃, 75 ℃ and 65 ℃.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104292363A (en) * | 2014-09-30 | 2015-01-21 | 江苏奇力康皮肤药业有限公司 | Extraction method of shark cartilage for eyedrops |
| CN108043353A (en) * | 2018-01-29 | 2018-05-18 | 湖南伍星生物科技有限公司 | A kind of chondroitin sulfate extractor |
| CN109527499A (en) * | 2018-10-09 | 2019-03-29 | 临沂新程金锣肉制品集团有限公司 | A kind of processing technology that ossein voluptuousness is remarkably reinforced |
Citations (5)
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| EP1557472A1 (en) * | 2002-11-01 | 2005-07-27 | Nippon Barrier Free Co. Ltd. | Sodium chondroitin sulfate, chondroitin sulfate-containing material and processes for producing the same |
| CN1711284A (en) * | 2002-11-13 | 2005-12-21 | 嘉吉有限公司 | Isolating chondroitin sulfate |
| KR20070063096A (en) * | 2005-12-14 | 2007-06-19 | 한국푸디팜 주식회사 | Manufacturing method for chondroitin sulfate from feet of fowl |
| CN101280027A (en) * | 2007-10-18 | 2008-10-08 | 日照众山生物科技有限公司 | Extracting method of chondroitin sulfate |
| CN103320486A (en) * | 2013-06-27 | 2013-09-25 | 青岛贝尔特生物科技有限公司 | Method for producing chondroitin sulfate with coproduction of hydrolyzed collagen by employing fish cartilage |
-
2013
- 2013-10-21 CN CN201310492432.4A patent/CN103497261A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1557472A1 (en) * | 2002-11-01 | 2005-07-27 | Nippon Barrier Free Co. Ltd. | Sodium chondroitin sulfate, chondroitin sulfate-containing material and processes for producing the same |
| CN1711284A (en) * | 2002-11-13 | 2005-12-21 | 嘉吉有限公司 | Isolating chondroitin sulfate |
| KR20070063096A (en) * | 2005-12-14 | 2007-06-19 | 한국푸디팜 주식회사 | Manufacturing method for chondroitin sulfate from feet of fowl |
| CN101280027A (en) * | 2007-10-18 | 2008-10-08 | 日照众山生物科技有限公司 | Extracting method of chondroitin sulfate |
| CN103320486A (en) * | 2013-06-27 | 2013-09-25 | 青岛贝尔特生物科技有限公司 | Method for producing chondroitin sulfate with coproduction of hydrolyzed collagen by employing fish cartilage |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104292363A (en) * | 2014-09-30 | 2015-01-21 | 江苏奇力康皮肤药业有限公司 | Extraction method of shark cartilage for eyedrops |
| CN104292363B (en) * | 2014-09-30 | 2016-08-17 | 江苏奇力康皮肤药业有限公司 | A kind of extracting method of the shark cartilage for collyrium |
| CN108043353A (en) * | 2018-01-29 | 2018-05-18 | 湖南伍星生物科技有限公司 | A kind of chondroitin sulfate extractor |
| CN109527499A (en) * | 2018-10-09 | 2019-03-29 | 临沂新程金锣肉制品集团有限公司 | A kind of processing technology that ossein voluptuousness is remarkably reinforced |
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Application publication date: 20140108 |