CN104844731A - Heparin sodium crude product extraction method - Google Patents
Heparin sodium crude product extraction method Download PDFInfo
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- CN104844731A CN104844731A CN201510228781.4A CN201510228781A CN104844731A CN 104844731 A CN104844731 A CN 104844731A CN 201510228781 A CN201510228781 A CN 201510228781A CN 104844731 A CN104844731 A CN 104844731A
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- 229920000669 heparin Polymers 0.000 title claims abstract description 49
- ZFGMDIBRIDKWMY-PASTXAENSA-N heparin Chemical compound CC(O)=N[C@@H]1[C@@H](O)[C@H](O)[C@@H](COS(O)(=O)=O)O[C@@H]1O[C@@H]1[C@@H](C(O)=O)O[C@@H](O[C@H]2[C@@H]([C@@H](OS(O)(=O)=O)[C@@H](O[C@@H]3[C@@H](OC(O)[C@H](OS(O)(=O)=O)[C@H]3O)C(O)=O)O[C@@H]2O)CS(O)(=O)=O)[C@H](O)[C@H]1O ZFGMDIBRIDKWMY-PASTXAENSA-N 0.000 title claims abstract description 49
- 229960001008 heparin sodium Drugs 0.000 title claims abstract description 49
- 238000000605 extraction Methods 0.000 title claims abstract description 12
- 239000012043 crude product Substances 0.000 title claims abstract description 6
- 239000011347 resin Substances 0.000 claims abstract description 99
- 229920005989 resin Polymers 0.000 claims abstract description 99
- 238000003795 desorption Methods 0.000 claims abstract description 85
- 238000001179 sorption measurement Methods 0.000 claims abstract description 54
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 37
- 150000003839 salts Chemical class 0.000 claims abstract description 26
- 238000000354 decomposition reaction Methods 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 19
- 238000001035 drying Methods 0.000 claims abstract description 16
- 238000005406 washing Methods 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 47
- 239000000706 filtrate Substances 0.000 claims description 31
- 239000007788 liquid Substances 0.000 claims description 25
- 238000001556 precipitation Methods 0.000 claims description 25
- 238000003756 stirring Methods 0.000 claims description 25
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 21
- 239000011780 sodium chloride Substances 0.000 claims description 21
- 230000001376 precipitating effect Effects 0.000 claims description 20
- 230000000968 intestinal effect Effects 0.000 claims description 16
- 210000004347 intestinal mucosa Anatomy 0.000 claims description 16
- 238000001914 filtration Methods 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 239000003513 alkali Substances 0.000 claims description 10
- 238000004140 cleaning Methods 0.000 claims description 10
- 239000012535 impurity Substances 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- 210000004877 mucosa Anatomy 0.000 claims description 10
- 239000000047 product Substances 0.000 claims description 10
- 238000005086 pumping Methods 0.000 claims description 10
- 210000000813 small intestine Anatomy 0.000 claims description 10
- 239000006228 supernatant Substances 0.000 claims description 10
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims description 5
- 229920000742 Cotton Polymers 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 239000004744 fabric Substances 0.000 claims description 5
- 239000004519 grease Substances 0.000 claims description 5
- 239000003456 ion exchange resin Substances 0.000 claims description 5
- 229920003303 ion-exchange polymer Polymers 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- 230000007935 neutral effect Effects 0.000 claims description 5
- 102000004169 proteins and genes Human genes 0.000 claims description 5
- 108090000623 proteins and genes Proteins 0.000 claims description 5
- 239000003814 drug Substances 0.000 abstract description 4
- 230000007062 hydrolysis Effects 0.000 abstract description 4
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 4
- 239000002699 waste material Substances 0.000 abstract description 2
- 210000003736 gastrointestinal content Anatomy 0.000 abstract 2
- 235000019441 ethanol Nutrition 0.000 abstract 1
- 239000013049 sediment Substances 0.000 abstract 1
- 238000005185 salting out Methods 0.000 description 6
- 238000002791 soaking Methods 0.000 description 4
- 239000012267 brine Substances 0.000 description 3
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229920002683 Glycosaminoglycan Polymers 0.000 description 1
- 241000124008 Mammalia Species 0.000 description 1
- 241001494479 Pecora Species 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000002785 anti-thrombosis Effects 0.000 description 1
- 239000003146 anticoagulant agent Substances 0.000 description 1
- 230000010100 anticoagulation Effects 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 210000000936 intestine Anatomy 0.000 description 1
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- Polysaccharides And Polysaccharide Derivatives (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a heparin sodium crude product extraction method, which comprises the following steps: (1) salt hydrolysis; (2) adsorption; (3) resin washing; (4) resin desorption; (5) sediment; (6) ethyl alcohol decomposition; (7) drying. The method provided by the invention has the advantage that separated intestinal contents are taken as fodder, and second time desorption filter liquor is recycled at a next first time desorption, so that the pollution problem is solved; according to the method, the salt content is improved, the salt content used by a tradition method is 4 degrees, the salt content of the method provided by the invention is six degrees, and the yield of heparin sodium is increased. By adopting the method, the zymolytic medicine extraction rate can be achieved, and the waste of the intestinal contents is also avoided, so that the highest productive benefit is achieved.
Description
The technical field is as follows:
the invention relates to a heparin sodium extraction method, in particular to a heparin sodium crude product extraction method.
Background art:
heparin sodium is an acidic mucopolysaccharide, has strong anticoagulation effect, is mainly present in intestinal mucosa of mammals, is a first choice medicament for clinical antithrombotic diseases, and is a valuable biochemical medicament exported in China in large quantity.
The traditional method for preparing heparin sodium mainly comprises two methods, one is salt hydrolysis and the other is enzymolysis. The main defects of the salt hydrolysis method are that the yield of heparin sodium is low, and the main defects of the enzymolysis method are that intestinal residues are decomposed and the pollution is serious.
The invention content is as follows:
the invention aims to provide a heparin sodium crude product extraction method which can reduce pollution and improve the yield of heparin sodium.
The purpose of the invention is implemented by the following technical scheme: a method for extracting a crude heparin sodium product comprises the following steps: (1) salt decomposition; (2) adsorption; (3) cleaning the resin; (4) resin desorption; (5) precipitating; (6) decomposing alcohol; (7) drying; wherein,
(1) salt decomposition: mincing fresh small intestine mucosa, mixing the minced fresh small intestine mucosa and water according to the mass ratio of 1:3, pumping into a reaction tank, adding salt or saline water to adjust the salinity to 5.9-6.1 ℃, adding edible alkali to adjust the pH value to 9-9.3, directly heating to 95-97 ℃, preserving the temperature for 9-10 minutes to carry out salt decomposition, fishing out intestinal residues after the salt decomposition, collecting the intestinal residues as feed, and mixing the residual intestinal mucosa and water;
(2) adsorption: filtering the mixed solution of the intestinal mucosa and water by using a 80-100-mesh filter screen, pumping the filtered filtrate into an adsorption tank, then injecting clear water into the adsorption tank, wherein the volume ratio of the filtrate to the clear water is 1:1, adjusting the water temperature to 58-60 ℃, adjusting the salinity to 2.5-3 ℃, adding standby resin for adsorption, and the volume ratio of the resin to the fresh intestinal mucosa is 0.75: 100, respectively;
(3) resin cleaning: after adsorption, collecting the resin after adsorption, washing the resin after adsorption for 2-3 times by using clean water at 40-50 ℃, and washing away grease and impurities on the surface of the resin after adsorption;
(4) resin desorption: draining the washed resin, putting the washed resin into a desorption tank, adding 20-DEG saline into the desorption tank, wherein the volume ratio of the washed resin to the saline is 2: 1, stirring for 10 minutes, adjusting salinity to 17-18 ℃, adjusting the pH value to 8.3-8.5, then heating to 55-60 ℃, stirring for 2-2.5 hours for first desorption, and collecting first desorption resin and first desorption filtrate after the first desorption is finished; then carrying out secondary desorption on the first desorption resin, wherein the salinity is required to be not lower than 20 ℃, heating to 55-60 ℃, and stirring for 2-2.5 hours; then collecting the second desorption resin and the second desorption filtrate; the collected second desorption resin is filled in a filter screen and is repeatedly used in the step (2) after being soaked in saline water with the temperature of 20-25 ℃; the resin mainly plays a role in adsorption, and is fully expanded by soaking in clear water, and is also soaked in saline water with different concentrations twice, so that the heparin sodium adsorbed by the resin is fully eluted, the extraction amount of the heparin sodium is increased, and the repeated adsorption capacity of the resin is improved.
(5) And (3) precipitation: collecting the second desorption filtrate for next first desorption circulation; collecting the first desorption filtrate into a precipitation barrel, adjusting the pH value to 9-12, precipitating for more than 12 hours, separating out alkali protein and other impurities, and precipitating at the bottom of the precipitation barrel;
(6) alcohol decomposition: extracting the clear liquid on the precipitation barrel for filtering after precipitation, adding hydrochloric acid into the filtered clear liquid while stirring, adjusting the pH of the filtered clear liquid to be neutral, then adding alcohol with the alcohol content of more than 70 degrees into the filtered clear liquid while stirring, adjusting the alcohol content of the filtered clear liquid to 30-35 degrees, adjusting the pH value to be 8-9, precipitating for 24-48 hours, and forming alcohol supernatant and heparin sodium paste;
(7) and (3) drying: and extracting the alcohol supernatant, collecting the heparin sodium paste, hanging and filtering the collected heparin sodium paste by using cotton cloth for 24 hours, taking out the paste, and drying the paste to obtain the finished product heparin sodium.
Specifically, the resin is a strongly basic ion exchange resin.
The invention has the advantages that the separated intestinal residue is used as feed, and the second desorption filtrate is used for the next first desorption cycle, thereby solving the pollution problem; the method improves the salinity, the salinity used by the traditional method is four degrees, the salinity used by the method is six degrees, and the yield of the heparin sodium is improved. Taking ten thousand sheep intestines as an example, 0.59 hundred million units of heparin sodium is produced by the traditional salt hydrolysis method, and one thousand kilograms of intestinal residues are produced; the traditional enzymolysis method produces 0.83 hundred million units of heparin sodium, and does not produce intestinal dregs. The patent produces 0.83 hundred million units of heparin sodium and produces one thousand kilograms of intestinal residues; the invention can reach the medicine yield of enzymolysis and can not waste intestinal dregs generated in production, thereby reaching the highest benefit of production.
The specific implementation mode is as follows:
example 1: a method for extracting a crude heparin sodium product comprises the following steps: (1) salt decomposition; (2) adsorption; (3) cleaning the resin; (4) resin desorption; (5) precipitating; (6) decomposing alcohol; (7) drying; wherein,
(1) salt decomposition: mincing fresh small intestine mucosa, mixing the minced fresh small intestine mucosa and water according to the mass ratio of 1:3, pumping into a reaction tank, adding salt or brine to adjust the salinity to 5.9 ℃, adding edible alkali to adjust the pH value to 9, directly heating to 95 ℃, preserving the temperature for 10 minutes to carry out salting out, fishing out intestinal residues after the salting out, collecting the intestinal residues as feed, and mixing the residual intestinal mucosa and water;
(2) adsorption: filtering the mixed solution of the intestinal mucosa and water by using a 80-mesh filter screen, pumping the filtered filtrate into an adsorption tank, then injecting clean water into the adsorption tank, adjusting the volume ratio of the filtrate to the clean water to 58 ℃, adjusting the salinity to 2.5 ℃, adding standby resin for adsorption, wherein the volume ratio of the resin to the fresh small intestinal mucosa is 0.75: 100, respectively;
(3) resin cleaning: after adsorption, collecting the resin after adsorption, washing the resin after adsorption for 2 times by using clear water at 50 ℃, and washing away grease and impurities on the surface of the resin after adsorption;
(4) resin desorption: draining the washed resin, putting the washed resin into a desorption tank, adding 20-DEG saline into the desorption tank, wherein the volume ratio of the washed resin to the saline is 2: 1, stirring for 10 minutes, adjusting salinity to 17 ℃, adjusting the pH value to 8.3, heating to 55 ℃, stirring for 2 hours for first desorption, and collecting first desorption resin and first desorption filtrate after the first desorption is finished; then carrying out secondary desorption on the first desorption resin, wherein the salinity is required to be not lower than 20 ℃, heating to 55 ℃, and stirring for 2 hours; then collecting the second desorption resin and the second desorption filtrate; the collected second desorption resin is filled in a filter screen and is repeatedly used in the step (2) after being soaked in saline water at the temperature of 20 ℃; the resin mainly plays a role in adsorption, and is fully expanded by soaking in clear water, and is also soaked in saline water with different concentrations twice, so that the heparin sodium adsorbed by the resin is fully eluted, the extraction amount of the heparin sodium is increased, and the repeated adsorption capacity of the resin is improved.
(5) And (3) precipitation: collecting the second desorption filtrate for next first desorption circulation; collecting the first desorption filtrate into a precipitation barrel, adjusting the pH value to 9, precipitating for more than 12 hours, separating out alkali protein and other impurities, and precipitating at the bottom of the precipitation barrel;
(6) alcohol decomposition: after precipitation, extracting the clear liquid on the precipitation barrel for filtration, adding hydrochloric acid into the filtered clear liquid while stirring, adjusting the pH of the filtered clear liquid to be neutral, then adding alcohol with the alcohol content of more than 70 degrees into the filtered clear liquid while stirring, adjusting the alcohol content of the filtered clear liquid to 30 degrees, adjusting the pH value to be 8, and precipitating for 24 hours to form alcohol supernatant and heparin sodium paste;
(7) and (3) drying: and extracting the alcohol supernatant, collecting the heparin sodium paste, hanging and filtering the collected heparin sodium paste by using cotton cloth for 24 hours, taking out the paste, and drying the paste to obtain the finished product heparin sodium.
Specifically, the resin is a strongly basic ion exchange resin.
Example 2: a method for extracting a crude heparin sodium product comprises the following steps: (1) salt decomposition; (2) adsorption; (3) cleaning the resin; (4) resin desorption; (5) precipitating; (6) decomposing alcohol; (7) drying; wherein,
(1) salt decomposition: mincing fresh small intestine mucosa, mixing the minced fresh small intestine mucosa and water according to the mass ratio of 1:3, pumping into a reaction tank, adding salt or brine to adjust the salinity to 6.1 ℃, adding edible alkali to adjust the pH value to 9.3, directly heating to 97 ℃, preserving the temperature for 9 minutes to carry out salting out, fishing out intestinal residues after the salting out, collecting the intestinal residues as feed, and mixing the residual intestinal mucosa and water;
(2) adsorption: filtering the mixed solution of the intestinal mucosa and water by using a 100-mesh filter screen, pumping the filtered filtrate into an adsorption tank, then injecting clean water into the adsorption tank, adjusting the volume ratio of the filtrate to the clean water to 60 ℃, adjusting the salinity to 3 ℃, adding standby resin for adsorption, wherein the volume ratio of the resin to the fresh intestinal mucosa is 0.75: 100, respectively;
(3) resin cleaning: after adsorption, collecting the resin after adsorption, washing the resin after adsorption for 3 times by using clear water at 40 ℃, and washing away grease and impurities on the surface of the resin after adsorption;
(4) resin desorption: draining the washed resin, putting the washed resin into a desorption tank, adding 20-DEG saline into the desorption tank, wherein the volume ratio of the washed resin to the saline is 2: 1, stirring for 10 minutes, adjusting salinity to 18 ℃, adjusting the pH value to 8.5, then heating to 60 ℃, stirring for 2.5 hours, carrying out first desorption, and collecting first desorption resin and first desorption filtrate after the first desorption is finished; then carrying out secondary desorption on the first desorption resin, wherein the salinity is required to be not lower than 20 ℃, heating to 60 ℃, and stirring for 2.5 hours; then collecting the second desorption resin and the second desorption filtrate; the collected second desorption resin is filled in a filter screen and is repeatedly used in the step (2) after being soaked in saline water at the temperature of 25 ℃; the resin mainly plays a role in adsorption, and is fully expanded by soaking in clear water, and is also soaked in saline water with different concentrations twice, so that the heparin sodium adsorbed by the resin is fully eluted, the extraction amount of the heparin sodium is increased, and the repeated adsorption capacity of the resin is improved.
(5) And (3) precipitation: collecting the second desorption filtrate for next first desorption circulation; collecting the first desorption filtrate into a precipitation barrel, adjusting the pH value to 12, precipitating for more than 12 hours, separating out alkali protein and other impurities, and precipitating at the bottom of the precipitation barrel;
(6) alcohol decomposition: after precipitation, extracting the clear liquid on the precipitation barrel for filtration, adding hydrochloric acid into the filtered clear liquid while stirring, adjusting the pH of the filtered clear liquid to be neutral, then adding alcohol with the alcohol content of more than 70 degrees into the filtered clear liquid while stirring, adjusting the alcohol content of the filtered clear liquid to 35 degrees, adjusting the pH value to be 9, and precipitating for 48 hours to form alcohol supernatant and heparin sodium paste;
(7) and (3) drying: and extracting the alcohol supernatant, collecting the heparin sodium paste, hanging and filtering the collected heparin sodium paste by using cotton cloth for 24 hours, taking out the paste, and drying the paste to obtain the finished product heparin sodium.
Specifically, the resin is a strongly basic ion exchange resin.
Example 3: a method for extracting a crude heparin sodium product comprises the following steps: (1) salt decomposition; (2) adsorption; (3) cleaning the resin; (4) resin desorption; (5) precipitating; (6) decomposing alcohol; (7) drying; wherein,
(1) salt decomposition: mincing fresh small intestine mucosa, mixing the minced fresh small intestine mucosa and water according to the mass ratio of 1:3, pumping into a reaction tank, adding salt or brine to adjust the salinity to 6 ℃, adding edible alkali to adjust the pH value to 9, directly heating to 96 ℃, preserving the temperature for 10 minutes to carry out salting out, fishing out intestinal residues after the salting out, collecting the intestinal residues as feed, and mixing the residual intestinal mucosa and water;
(2) adsorption: filtering the mixed solution of the intestinal mucosa and water by using a 90-mesh filter screen, pumping the filtered filtrate into an adsorption tank, then injecting clean water into the adsorption tank, adjusting the volume ratio of the filtrate to the clean water to 59 ℃, adjusting the salinity to 3 ℃, adding standby resin for adsorption, wherein the volume ratio of the resin to the fresh intestinal mucosa is 0.75: 100, respectively;
(3) resin cleaning: after adsorption, collecting the resin after adsorption, washing the resin after adsorption for 3 times by using clean water at 45 ℃, and washing away grease and impurities on the surface of the resin after adsorption;
(4) resin desorption: draining the washed resin, putting the washed resin into a desorption tank, adding 20-DEG saline into the desorption tank, wherein the volume ratio of the washed resin to the saline is 2: 1, stirring for 10 minutes, adjusting salinity to 17 ℃, adjusting the pH value to 8.4, then heating to 60 ℃, stirring for 2 hours for first desorption, and collecting first desorption resin and first desorption filtrate after the first desorption is finished; then carrying out secondary desorption on the first desorption resin, wherein the salinity is required to be not lower than 20 ℃, heating to 60 ℃, and stirring for 2 hours; then collecting the second desorption resin and the second desorption filtrate; the collected second desorption resin is filled in a filter screen and is repeatedly used in the step (2) after being soaked in saline water at the temperature of 23 ℃; the resin mainly plays a role in adsorption, and is fully expanded by soaking in clear water, and is also soaked in saline water with different concentrations twice, so that the heparin sodium adsorbed by the resin is fully eluted, the extraction amount of the heparin sodium is increased, and the repeated adsorption capacity of the resin is improved.
(5) And (3) precipitation: collecting the second desorption filtrate for next first desorption circulation; collecting the first desorption filtrate into a precipitation barrel, adjusting the pH value to 10, precipitating for more than 12 hours, separating out alkali protein and other impurities, and precipitating at the bottom of the precipitation barrel;
(6) alcohol decomposition: after precipitation, extracting the clear liquid on the precipitation barrel for filtration, adding hydrochloric acid into the filtered clear liquid while stirring, adjusting the pH of the filtered clear liquid to be neutral, then adding alcohol with the alcohol content of more than 70 degrees into the filtered clear liquid while stirring, adjusting the alcohol content of the filtered clear liquid to 33 degrees, adjusting the pH value to be 9, and precipitating for 36 hours to form alcohol supernatant and heparin sodium paste;
(7) and (3) drying: and extracting the alcohol supernatant, collecting the heparin sodium paste, hanging and filtering the collected heparin sodium paste by using cotton cloth for 24 hours, taking out the paste, and drying the paste to obtain the finished product heparin sodium.
The resin is strong-base ion exchange resin.
Claims (2)
1. The extraction method of the heparin sodium crude product is characterized by comprising the following steps: (1) salt decomposition; (2) adsorption; (3) cleaning the resin; (4) resin desorption; (5) precipitating; (6) decomposing alcohol; (7) drying; wherein,
(1) salt decomposition: mincing fresh small intestine mucosa, mixing the minced fresh small intestine mucosa and water according to the mass ratio of 1:3, pumping into a reaction tank, adding salt or saline water to adjust the salinity to 5.9-6.1 ℃, adding edible alkali to adjust the pH value to 9-9.3, directly heating to 95-97 ℃, preserving the temperature for 9-10 minutes to carry out salt decomposition, fishing out intestinal residues after the salt decomposition, collecting the intestinal residues as feed, and mixing the residual intestinal mucosa and water;
(2) adsorption: filtering the mixed solution of the intestinal mucosa and water by using a 80-100-mesh filter screen, pumping the filtered filtrate into an adsorption tank, then injecting clear water into the adsorption tank, wherein the volume ratio of the filtrate to the clear water is 1:1, adjusting the water temperature to 58-60 ℃, adjusting the salinity to 2.5-3 ℃, adding standby resin for adsorption, and the volume ratio of the resin to the fresh intestinal mucosa is 0.75: 100, respectively;
(3) resin cleaning: after adsorption, collecting the resin after adsorption, washing the resin after adsorption for 2-3 times by using clean water at 40-50 ℃, and washing away grease and impurities on the surface of the resin after adsorption;
(4) resin desorption: draining the washed resin, putting the washed resin into a desorption tank, adding 20-DEG saline into the desorption tank, wherein the volume ratio of the washed resin to the saline is 2: 1, stirring for 10 minutes, adjusting salinity to 17-18 ℃, adjusting the pH value to 8.3-8.5, then heating to 55-60 ℃, stirring for 2-2.5 hours for first desorption, and collecting first desorption resin and first desorption filtrate after the first desorption is finished; then carrying out secondary desorption on the first desorption resin, wherein the salinity is required to be not lower than 20 ℃, heating to 55-60 ℃, and stirring for 2-2.5 hours; then collecting the second desorption resin and the second desorption filtrate; the collected second desorption resin is filled in a filter screen and is repeatedly used in the step (2) after being soaked in saline water with the temperature of 20-25 ℃;
(5) and (3) precipitation: collecting the second desorption filtrate for next first desorption circulation; collecting the first desorption filtrate into a precipitation barrel, adjusting the pH value to 9-12, precipitating for more than 12 hours, separating out alkali protein and other impurities, and precipitating at the bottom of the precipitation barrel;
(6) alcohol decomposition: extracting the clear liquid on the precipitation barrel for filtering after precipitation, adding hydrochloric acid into the filtered clear liquid while stirring, adjusting the pH of the filtered clear liquid to be neutral, then adding alcohol with the alcohol content of more than 70 degrees into the filtered clear liquid while stirring, adjusting the alcohol content of the filtered clear liquid to 30-35 degrees, adjusting the pH value to be 8-9, precipitating for 24-48 hours, and forming alcohol supernatant and heparin sodium paste;
(7) and (3) drying: and extracting the alcohol supernatant, collecting the heparin sodium paste, hanging and filtering the collected heparin sodium paste by using cotton cloth for 24 hours, taking out the paste, and drying the paste to obtain the finished product heparin sodium.
2. The method for extracting crude heparin sodium product according to claim 1, wherein the resin is a strongly basic ion exchange resin.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108314749A (en) * | 2018-03-08 | 2018-07-24 | 广元市海鹏生物科技有限公司 | A kind of method of driven Object Extraction heparin sodium |
| CN110229252A (en) * | 2019-06-25 | 2019-09-13 | 广元市海天实业有限责任公司 | A kind of processing technology improving refined heparin sodium yield |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1876687A (en) * | 2006-06-27 | 2006-12-13 | 胡世辉 | Heparin sodium production process |
| CN103044575A (en) * | 2011-10-11 | 2013-04-17 | 如皋市坝新肠衣有限公司 | Extracting method of heparin sodium |
| KR101447123B1 (en) * | 2014-02-27 | 2014-10-06 | 박상협 | Extraction Method of Heparin |
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2015
- 2015-05-07 CN CN201510228781.4A patent/CN104844731B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1876687A (en) * | 2006-06-27 | 2006-12-13 | 胡世辉 | Heparin sodium production process |
| CN103044575A (en) * | 2011-10-11 | 2013-04-17 | 如皋市坝新肠衣有限公司 | Extracting method of heparin sodium |
| KR101447123B1 (en) * | 2014-02-27 | 2014-10-06 | 박상협 | Extraction Method of Heparin |
Non-Patent Citations (2)
| Title |
|---|
| 孔保华: "《畜产品加工储藏新技术（第1版）》", 31 May 2007 * |
| 张豁中等: "《动物活性成分化学（第1版）》", 31 May 1995 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108314749A (en) * | 2018-03-08 | 2018-07-24 | 广元市海鹏生物科技有限公司 | A kind of method of driven Object Extraction heparin sodium |
| CN110229252A (en) * | 2019-06-25 | 2019-09-13 | 广元市海天实业有限责任公司 | A kind of processing technology improving refined heparin sodium yield |
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