CN102199229A

CN102199229A - Method for preparing chondroitin sulfate

Info

Publication number: CN102199229A
Application number: CN 201110087026
Authority: CN
Inventors: 刘榜惠
Original assignee: HUAI'AN MAIDESEN PHARMACEUTICAL CO Ltd
Current assignee: HUAI'AN MAIDESEN PHARMACEUTICAL CO Ltd
Priority date: 2011-04-08
Filing date: 2011-04-08
Publication date: 2011-09-28

Abstract

The invention discloses a method for preparing chondroitin sulfate, which comprises the following steps of: boiling a cartilage raw material at the temperature of between 80 and 100DEG C for 16 to 24 hours, steaming a cartilage tissue in a steam box at the temperature of between 100 and 150DEG C for more than 16 hours, and performing enzymolysis, oxidation and alcohol precipitation on the cartilage tissue to obtain the chondroitin sulfate product. The cartilage raw material is boiled and steamed, most impurities are recycled, and the pollution is reduced; meanwhile, operation such as enzymolysis, filtration and the like is simple, the obtained chondroitin sulfate product has stable quality, and the content of the chondroitin sulfate is over 90 percent.

Description

A kind of preparing chondroitin sulfates

Technical field

The invention belongs to biological technical field, be specifically related to a kind of preparing chondroitin sulfates.

Background technology

Chondroitin sulfate, English name chondroitin sulfate, be that cartilage with animal (pig, ox, horse, sheep, chicken, shark etc.) is a kind of polymeric acidic mucopolysaccharide of raw material, its molecular structure is the polysaccharide chain that repetition disaccharide unit that β-D-glucuronic acid and N-acetylamino galactosamine form by β 1 → 3 glycosidic link is formed.It is a kind of white or micro-yellow powder, and water-absorbent is strong, and the thick liquid that forms soluble in water is insoluble to organic solvents such as alcohol, acetone, EC, and its esters is more stable to heat.

At present, chondroitin sulfate adopts alkali-zymohydrolysis extracting method usually, mainly may further comprise the steps:

1) alkali is carried enzymolysis: raw material (cartilage) is added water to submerge, and transfers pH8.5 with sodium hydroxide, is warming up to 55-60 ℃, is incubated 4-6 hour, add 2% Sumizyme MP again, keep pH8.5, be incubated 55-60 ℃ of stirring 6-8 hour, be warming up to boiling about 15 minutes, filter, get filtrate;

2) alcohol precipitation: add the sodium-chlor of 3% weight in the filtrate, be cooled to room temperature, by volume 2.5 extraordinarily go into 95% alcohol, static 8 hours, get precipitation;

3) oxidation: the weight ratio by precipitation and water is the mixed water of 1:10, adds the sodium-chlor of 3% weight simultaneously, transfers pH10-12, adds 2% weight percent hydrogen peroxide oxidation 8 hours, filters, and gets filtrate;

4) alcohol precipitation drying: filtrate is transferred pH6, adds 2.5 times of amount alcohol secondary sedimentation of volume, and precipitation is used 95% dehydration of alcohol twice again, and drying and crushing obtains the chondroitin sulfate finished product.

Because many fat of cartilage raw material surface attachment or muscle tissue, these tissues are the major impurities in the chondroitin sulfate production process, and the chondroitin sulfate cellulose solution compares thickness, impurity is too much in the solution, filters very difficulty, when making scale produce chondroitin sulfate, filtration efficiency is very low, many producers use the manger of original backwardness to filter, and cause production efficiency not high, the follow-up purifying of infiltrating of impurity effect product; Secondly owing to impurity in the chondroitin sulfate cellulose solution is too much, make purification process become complicated, impurity too disperses to be unfavorable for to recycle, and causes environmental pollution.

Summary of the invention

The objective of the invention is to: a kind of preparing chondroitin sulfates is provided, and this preparation method makes the chondroitin sulfate production process simple, and impurities in raw materials can effectively be handled and recycle, good product quality.

Technical solution of the present invention is that this preparation method comprises the following steps:

(1) poach: the cartilage raw material is added water to submerge, and is warming up to 80-100 ℃, boils 12-24 hour, and the muscle tissue that is attached to cartilage surface is peeled off, and pulls cartilage out;

(2) gas steams: the cartilage that step (1) obtains is put into food steamer, and 100-150 ℃ steamed is more than 16 hours, and vapour outlet is established in the food steamer upper end, carries out oily water separation after the exhaust vapour condensation, and water is got back to food steamer, and oil is collected;

(3) enzymolysis: the cartilage that step (2) is handled is added water to submerge, by volume add 3% sodium-chlor, with adjusting PH with base to 8-9, be warming up to 55-60 ℃, add 2709 Sumizyme MPs by cartilage raw material weight 1-3% again, keep pH8-9, be incubated 55-60 ℃ and stirred 4-6 hour, be warming up to boiling 12-18 minute;

(4) oxidation: with the solution that step (3) obtains, be cooled to 35-40 ℃, transfer pH to 10-12, the 1-3% hydrogen peroxide oxidation that adds liquor capacity filtered to get filtrate more than 6 hours;

(5) alcohol precipitation: with the filtrate that step (4) obtains, transfer pH6-7, add alcohol and make the solution ethanol concn reach 60%, precipitation is more than 16 hours;

(6) dewatered drying: precipitation discards upper strata alcohol after finishing, and collecting precipitation dehydrates, and gets the chondroitin sulfate finished product.

The effect that the present invention obtains is:

One, the present invention passes through only remaining pure white cartilaginous tissue of cartilage and a small amount of grease in surface that poach obtains, and other animal tissues all peels off, and poach, other tissue that strips down can be recycled, and water can be reused;

Two, cartilage steams through gas again, the grease high temperature of the overwhelming majority in the cartilage can be steamed, and carries out oily water separation behind the vapor condensation, recycles;

Three, the production filter operation is simple, and no grease and filter residue are few in the enzymolysis solution, the filtration efficiency height;

Four, constant product quality, the content of chondroitin sulfate reaches more than 90%.

Embodiment

Further specify technical solution of the present invention below in conjunction with specific embodiment, these embodiment can not be interpreted as it is restriction to technical solution.

Embodiment 1: prepare chondroitin sulfate according to following steps

(1) poach: 100 kilograms of cartilage raw materials are added water to submerge, and are warming up to 80 ℃, boil 24 hours, and the muscle tissue that is attached to cartilage surface is peeled off, and pull cartilage out;

(2) gas steams: the cartilage that step (1) obtains is put into food steamer, and 100 ℃ steamed is more than 16 hours, and vapour outlet is established in the food steamer upper end, carries out oily water separation after the exhaust vapour condensation, and water is got back to food steamer, and oil is collected;

(3) enzymolysis: the cartilage that step (2) is handled is added water to submerge, by volume add 3% sodium-chlor,, be warming up to 55 ℃, add the 1Kg2709 Sumizyme MP again, keep pH8, be incubated 55 ℃ and stirred 6 hours, be warming up to boiling 12 minutes with adjusting PH with base to 8;

(4) oxidation: with the solution that step (3) obtains, be cooled to 35 ℃, transfer pH to 10,1% hydrogen peroxide oxidation that adds liquor capacity filtered to get filtrate more than 6 hours;

(5) alcohol precipitation: with the filtrate that step (4) obtains, transfer pH6, add alcohol and make the solution ethanol concn reach 60%, precipitation is more than 16 hours;

(6) dewatered drying: precipitation discards upper strata alcohol after finishing, and collecting precipitation dehydrates, and gets 14.3 kilograms of chondroitin sulfate finished products, and the chondroitin sulfate cellulose content is 92.5%.

Embodiment 2: prepare chondroitin sulfate according to following steps

(1) poach: 100 kilograms of cartilage raw materials are added water to submerge, and are warming up to 90 ℃, boil 18 hours, and the muscle tissue that is attached to cartilage surface is peeled off, and pull cartilage out;

(2) gas steams: the cartilage that step (1) obtains is put into food steamer, and 125 ℃ steamed is more than 16 hours, and vapour outlet is established in the food steamer upper end, carries out oily water separation after the exhaust vapour condensation, and water is got back to food steamer, and oil is collected;

(3) enzymolysis: the cartilage that step (2) is handled is added water to submerge, by volume add 3% sodium-chlor,, be warming up to 58 ℃, add the 2Kg2709 Sumizyme MP again, keep pH8.5, be incubated 58 ℃ and stirred 5 hours, be warming up to boiling 15 minutes with adjusting PH with base to 8.5;

(4) oxidation: with the solution that step (3) obtains, be cooled to 37 ℃, transfer pH to 11,2% hydrogen peroxide oxidation that adds liquor capacity filtered to get filtrate more than 6 hours;

(5) alcohol precipitation: with the filtrate that step (4) obtains, transfer pH6.5, add alcohol and make the solution ethanol concn reach 60%, precipitation is more than 16 hours;

(6) dewatered drying: precipitation discards upper strata alcohol after finishing, and collecting precipitation dehydrates, and gets 14.5 kilograms of chondroitin sulfate finished products, and the chondroitin sulfate cellulose content is 92.8%.。

Embodiment 3: prepare chondroitin sulfate according to following steps

(1) poach: 100 kilograms of cartilage raw materials are added water to submerge, and are warming up to 100 ℃, boil 12 hours, and the muscle tissue that is attached to cartilage surface is peeled off, and pull cartilage out;

(2) gas steams: the cartilage that step (1) obtains is put into food steamer, and 150 ℃ steamed is more than 16 hours, and vapour outlet is established in the food steamer upper end, carries out oily water separation after the exhaust vapour condensation, and water is got back to food steamer, and oil is collected;

(3) enzymolysis: the cartilage that step (2) is handled is added water to submerge, by volume add 3% sodium-chlor,, be warming up to 60 ℃, add the 3Kg2709 Sumizyme MP again, keep pH9, be incubated 60 ℃ and stirred 6 hours, be warming up to boiling 18 minutes with adjusting PH with base to 9;

(4) oxidation: with the solution that step (3) obtains, be cooled to 40 ℃, transfer pH to 12,3% hydrogen peroxide oxidation that adds liquor capacity filtered to get filtrate more than 6 hours;

(5) alcohol precipitation: with the filtrate that step (4) obtains, transfer pH7, add alcohol and make the solution ethanol concn reach 60%, precipitation is more than 16 hours;

(6) dewatered drying: precipitation discards upper strata alcohol after finishing, and collecting precipitation dehydrates, and gets 14.8 kilograms of chondroitin sulfate finished products, and the chondroitin sulfate cellulose content is 93.2%.

Claims

1. a preparing chondroitin sulfates is characterized in that comprising the following steps:

(3) enzymolysis: the cartilage that step (2) is handled is added water to submerge, by volume add 3% sodium-chlor, with adjusting PH with base to 8-9, be warming up to 55-60 ℃, add 2709 Sumizyme MPs by cartilage raw material weight 1%-3% again, keep pH8-9, be incubated 55-60 ℃ and stirred 4-6 hour, be warming up to boiling 12-18 minute;