CN109929055A - A method of passing through milling and extracting chondroitin sulfate - Google Patents

A method of passing through milling and extracting chondroitin sulfate Download PDF

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Publication number
CN109929055A
CN109929055A CN201711350762.4A CN201711350762A CN109929055A CN 109929055 A CN109929055 A CN 109929055A CN 201711350762 A CN201711350762 A CN 201711350762A CN 109929055 A CN109929055 A CN 109929055A
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CN
China
Prior art keywords
cartilage
chondroitin sulfate
reagent
milling
dismembyator
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Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201711350762.4A
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Chinese (zh)
Inventor
刘乃山
迟培升
李先英
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Qingdao Jiulong Biological Medicine Group Co Ltd
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Qingdao Jiulong Biological Medicine Group Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
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Publication date
Application filed by Qingdao Jiulong Biological Medicine Group Co Ltd filed Critical Qingdao Jiulong Biological Medicine Group Co Ltd
Priority to CN201711350762.4A priority Critical patent/CN109929055A/en
Publication of CN109929055A publication Critical patent/CN109929055A/en
Pending legal-status Critical Current

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Abstract

The present invention relates to one kind to pass through milling and extracting chondroitin sulfate, using cartilage as raw material, it is crushed after being pre-processed and is ground into ultra-fine cartilage powder, it is uniformly mixed again with solid base reagent, grinding agent, it is placed in dismembyator and is fully ground, the mixture of powders ground sufficiently dissolves with salt water and adjust pH value, is filtered to remove insoluble matter, filtrate passes through alcohol precipitation, is drying to obtain chondroitin sulfate.Simple production process of the present invention, with short production cycle, high income, low energy consumption, few to the pollution of environment, easy to industrialized production.

Description

A method of passing through milling and extracting chondroitin sulfate
Technical field
The present invention relates to biochemistry, especially a kind of polishing extracts chondroitin sulfate.
Background technique
Chondroitin sulfate is to be covalently attached a kind of glycosaminoglycan that proteoglycans is formed on protein, is distributed widely in dynamic The extracellular matrix and cell surface of object tissue mainly treat the drug of rheumatism and rheumatism, also serve as functional food Primary raw material, also have the effects that anticancer, antithrombotic, reducing blood lipid.It is many that US and European is exported to as bulk pharmaceutical chemicals now Country, the market demand are vigorous.
Summary of the invention
In order to overcome in the prior art cartilage extract chondroitin sulfate alkali carries-enzymatic hydrolysis -ol sink method there are process energy consumptions it is big, The deficiency of pollution weight, complex production process, the present invention provide a kind of simple process, with short production cycle, at low cost, environmental pollution Less, the high polishing of recovery rate extracts chondroitin sulfate.
The technical solution adopted by the present invention to solve the technical problems is: one kind passing through milling and extracting chondroitin sulfate, Be characterized in that: it is ultra-fine cartilage powder to be crushed and be ground into after being pre-processed, then try with solid base using cartilage as raw material Agent, grinding agent are uniformly mixed, and are placed in dismembyator and are fully ground, the mixture of powders ground is sufficiently dissolved and adjusted with salt water PH value is saved, is filtered to remove insoluble matter, filtrate passes through alcohol precipitation, up to chondroitin sulfate after drying.
One kind passing through milling and extracting chondroitin sulfate, it is characterised in that: passes through following specific process step:
(1) pretreatment of raw material
It is spare with clear water cleaning, drying by cartilage degreasing, meat slag;By the cartilage after drying according to chondrigen Liao ︰ water=1 ︰ 4 ~6,10~40min is handled under the conditions of 60~100 DEG C;Cartilage is taken out, is put into baking oven, is dried under the conditions of 70~140 DEG C 4~9h of roasting processing;It is milled into cartilage powder with dismembyator, 120~400 mesh screens is crossed, obtains cartilage superfine powder, it is spare;
(2) reagent is produced
Solid base reagent is mixed with silica and is placed in dismembyator, 5~15min is ground, obtains reagent;Wherein, solid base tries The mass ratio of agent and silica is 0.4~1.5 ︰ 6;
(3) it extracts
Weigh cartilage superfine powder obtained in step (1), reagent obtained in step (2) 1 ︰ 0.8~3.3 in mass ratio addition is ground In grinder, it is co-mulled and made into 2~12min at room temperature, obtains mixture;It is 4~12% that obtained mixture, which is dissolved in concentration, In sodium chloride solution, pH value is adjusted to 5.0~7.5, centrifugation obtains supernatant;
(4) alcohol precipitation
95% ethyl alcohol will be added in supernatant obtained in step (3), the final volume score of ethyl alcohol is made to reach total liquid volume 70~90%, 6~14h is staticly settled, sediment is obtained;
(5) it is dried in vacuo
Sediment in step (4) is fitted into sack, 10~15min is centrifuged, it is small that 6~15 are dried in vacuo at 45~70 DEG C When, it crushes, obtains chondroitin sulfate finished product.
The solid base reagent is flaky sodium hydrate.
The sodium hydroxide solution with 2mol/L adjusts pH value.
The present invention be ultra-fine cartilage powder using cartilage as raw material, will be ground into after being pre-processed, then with solid base reagent, Grinding agent is uniformly mixed, and is placed in dismembyator and is fully ground, the mixture of powders ground is sufficiently dissolved and adjusted with salt water PH value, is filtered to remove insoluble matter, and filtrate passes through alcohol precipitation, is drying to obtain chondroitin sulfate.It is soft that polishing of the invention extracts sulfuric acid Low energy consumption for ossein, simple production process.Chondroitin sulfate is extracted using base reagent, with short production cycle, extracted amount is big, and it is at low cost, And other protein are not introduced in process of production.The purification of chondroitin sulfate is carried out using ethanol precipitation, sulfuric acid is soft The ossein rate of recovery is higher, while alleviating the consummate difficulty in downstream, alleviates the pollution to environment, easy to industrialized production.Through Measuring the polishing and extracting chondroitin sulfate recovery rate is 94%, and obtaining object purity is 98.6%.
Specific embodiment
Below with reference to embodiment, the present invention will be further described.
Embodiment 1
A kind of Mechanical Method extraction chondroitin sulfate, by following specific process step:
(1) pretreatment of raw material
Choosing fresh hog snout cartilage is raw material, and degreasing, meat slag are spare with clear water cleaning, drying;By the cartilage after drying According to chondrigen Liao ︰ water=1 ︰ 5,20min is handled under the conditions of 95 DEG C;Cartilage is taken out, is put into baking oven, under the conditions of 105 DEG C Baking processing 6h;It is milled into cartilage powder with high-intensitive planetary dismembyator, 200 mesh screens is crossed, obtains cartilage superfine powder, it is spare;
(2) reagent is produced
Flaky sodium hydrate is mixed with silica and is placed in high-intensitive planetary dismembyator, grinds 15min with stainless steel ball, Obtain reagent;Wherein, the mass ratio of flaky sodium hydrate and silica is 1.2 ︰ 6;
(3) it extracts
Weigh cartilage superfine powder obtained in step (1), reagent obtained in step (2) 1:2.5 in mass ratio be added it is high-intensitive In planetary dismembyator, it is co-mulled and made into 8min at room temperature, obtains mixture;It is 10% that obtained mixture, which is dissolved in concentration, Sodium chloride solution in, adjust pH value to 6.5, centrifugation obtains supernatant;
(4) alcohol precipitation
95% ethyl alcohol will be added in supernatant obtained in step (3), the final volume score of ethyl alcohol is made to reach total liquid volume 85%, 8h is staticly settled, sediment is obtained;
(5) it is dried in vacuo
Sediment in step (4) is fitted into sack, 10min is centrifuged, is dried in vacuo 12 hours under the conditions of 55 DEG C, is crushed, Obtain chondroitin sulfate finished product.
Polishing provided by the present embodiment extracts chondroitin sulfate, and low energy consumption, and simple production process is with short production cycle, mentions It takes rate and obtains object purity is high, it is at low cost, the pollution to environment is alleviated, it is easy to industrialized production.
Embodiment 2
A kind of polishing extraction chondroitin sulfate, by following specific process step:
(1) pretreatment of raw material
Choosing fresh bovine nasal cartilage is raw material, and degreasing, meat slag are spare with clear water cleaning, drying;By the cartilage after drying According to material ratio: chondrigen Liao ︰ water=1 ︰ 5 handles 5min under the conditions of 100 DEG C;Cartilage is taken out, is put into baking oven, 120 Baking processing 5h under the conditions of DEG C;It is milled into cartilage powder with high-intensitive planetary dismembyator, 300 mesh screens is crossed, it is ultra-fine to obtain cartilage Powder, it is spare;
(2) reagent is produced
Flaky sodium hydrate is mixed with silica and is placed in high-intensitive planetary dismembyator, grinds 10min with stainless steel ball, Obtain reagent;Wherein, the mass ratio of sodium hydroxide and silica is 0.8 ︰ 6;
(3) it extracts
Weigh cartilage superfine powder obtained in step (1), high-intensitive row is added in reagent obtained in step (2) 1 ︰ 2 in mass ratio In planetary dismembyator, it is co-mulled and made into 5min at room temperature, obtains mixture;It is 10% that obtained mixture, which is dissolved in concentration, In sodium chloride solution, pH value is adjusted to 5.5, centrifugation obtains supernatant;
(4) alcohol precipitation
95% ethyl alcohol will be added in supernatant obtained in step (3), makes the final volume score 83% of ethyl alcohol, staticly settle 10h obtains sediment;
(5) it is dried in vacuo
Sediment in step (4) is fitted into sack, 15min is centrifuged, is dried in vacuo 10 hours at 60 DEG C, crushes, obtains sulphur Aching and limp ossein finished product.It is reasonable by milling and extracting production technique of chondroitin sulfate provided by the present embodiment, recovery rate and object Purity is high, low energy consumption, few to the pollution of environment, easy to industrialized production.

Claims (4)

1. a kind of method by milling and extracting chondroitin sulfate, it is characterised in that: using cartilage as raw material, powder after being pre-processed It is broken and be ground into ultra-fine cartilage powder, then be uniformly mixed with solid base reagent, grinding agent, it is placed in dismembyator and is fully ground, grind It grinds obtained mixture of powders and pH value is sufficiently dissolved and adjusted with salt water, be filtered to remove insoluble matter, filtrate passes through alcohol precipitation, and drying is Obtain chondroitin sulfate.
2. a kind of method by milling and extracting chondroitin sulfate according to claim 1, it is characterised in that: by following Specific process step:
(1) pretreatment of raw material: spare with clear water cleaning, drying by cartilage degreasing, meat slag;By the cartilage after drying according to Chondrigen Liao ︰ water=1 ︰ 4~6 handles 10~40min under the conditions of 60~100 DEG C;Cartilage is taken out, is put into baking oven, 70 4~9h of baking processing under the conditions of~140 DEG C;It is milled into cartilage powder with dismembyator, 120~400 mesh screens is crossed, it is ultra-fine to obtain cartilage Powder, it is spare;
(2) reagent is produced: solid base reagent being mixed with silica and is placed in dismembyator, 5~15min is ground, obtains reagent;Its In, the mass ratio of solid base reagent and silica is 0.4~1.5 ︰ 6;
(3) extract: weigh cartilage superfine powder obtained in step (1), reagent obtained in step (2) 1:0.8 in mass ratio~ 3.3 are added in dismembyator, are co-mulled and made into 2~12min at room temperature, obtain mixture;Obtained mixture is dissolved in concentration In 4~12% sodium chloride solution, to adjust pH value to 5.0~7.5, centrifugation obtains supernatant;
(4) alcohol precipitation: will be added 95% ethyl alcohol in supernatant obtained in step (3), make the final volume score of ethyl alcohol 70~ 90%, 6~14h is staticly settled, sediment is obtained;
(5) it is dried in vacuo: the sediment in step (4) is fitted into sack, be centrifuged 10~15min, the vacuum at 45~70 DEG C It is 6~15 hours dry, it crushes, obtains chondroitin sulfate finished product.
3. a kind of method by milling and extracting chondroitin sulfate according to claim 1 or 2, it is characterised in that: described Solid base reagent be flaky sodium hydrate.
4. a kind of method by milling and extracting chondroitin sulfate according to claim 1 or 2, it is characterised in that: step (3) pH value is adjusted with the sodium hydroxide solution of 2mol/L in.
CN201711350762.4A 2017-12-15 2017-12-15 A method of passing through milling and extracting chondroitin sulfate Pending CN109929055A (en)

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Application Number Priority Date Filing Date Title
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112724279A (en) * 2021-01-13 2021-04-30 四川菲德力制药有限公司 Preparation method of sodium chondroitin sulfate

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112724279A (en) * 2021-01-13 2021-04-30 四川菲德力制药有限公司 Preparation method of sodium chondroitin sulfate

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Application publication date: 20190625