CN101450960B - Abomacetin extraction by salting-out method - Google Patents
Abomacetin extraction by salting-out method Download PDFInfo
- Publication number
- CN101450960B CN101450960B CN200710195544A CN200710195544A CN101450960B CN 101450960 B CN101450960 B CN 101450960B CN 200710195544 A CN200710195544 A CN 200710195544A CN 200710195544 A CN200710195544 A CN 200710195544A CN 101450960 B CN101450960 B CN 101450960B
- Authority
- CN
- China
- Prior art keywords
- oxacyclotetradecane
- erythromycin deriv
- sodium
- filtrating
- erythrocin
- Prior art date
- 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.)
- Active
Links
- ULGZDMOVFRHVEP-RWJQBGPGSA-N Erythromycin Chemical compound O([C@@H]1[C@@H](C)C(=O)O[C@@H]([C@@]([C@H](O)[C@@H](C)C(=O)[C@H](C)C[C@@](C)(O)[C@H](O[C@H]2[C@@H]([C@H](C[C@@H](C)O2)N(C)C)O)[C@H]1C)(C)O)CC)[C@H]1C[C@@](C)(OC)[C@@H](O)[C@H](C)O1 ULGZDMOVFRHVEP-RWJQBGPGSA-N 0.000 title claims abstract description 94
- 238000000034 method Methods 0.000 title claims abstract description 17
- 238000000605 extraction Methods 0.000 title abstract description 11
- 238000005185 salting out Methods 0.000 title abstract description 8
- 239000007788 liquid Substances 0.000 claims abstract description 11
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims abstract description 10
- 229910052938 sodium sulfate Inorganic materials 0.000 claims abstract description 10
- 235000011152 sodium sulphate Nutrition 0.000 claims abstract description 10
- 238000000855 fermentation Methods 0.000 claims abstract description 8
- 230000004151 fermentation Effects 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 230000002209 hydrophobic effect Effects 0.000 claims abstract description 7
- 239000003960 organic solvent Substances 0.000 claims abstract description 6
- 229960003276 erythromycin Drugs 0.000 claims description 40
- SKDGGFHGLZBNBC-YZPBMOCRSA-N (3r,4s,5s,6r,7r,9r,11r,12r,13s,14r)-6-[(2s,3r,4s,6r)-4-(dimethylamino)-3-hydroxy-6-methyloxan-2-yl]oxy-14-ethyl-7,12,13-trihydroxy-4-[(2r,4r,5s,6s)-5-hydroxy-4-methoxy-4,6-dimethyloxan-2-yl]oxy-3,5,7,9,11,13-hexamethyl-oxacyclotetradecane-2,10-dione;dodec Chemical compound CCCCCCCCCCCCOS(O)(=O)=O.O([C@@H]1[C@@H](C)C(=O)O[C@@H]([C@@]([C@H](O)[C@@H](C)C(=O)[C@H](C)C[C@@](C)(O)[C@H](O[C@H]2[C@@H]([C@H](C[C@@H](C)O2)N(C)C)O)[C@H]1C)(C)O)CC)[C@H]1C[C@@](C)(OC)[C@@H](O)[C@H](C)O1 SKDGGFHGLZBNBC-YZPBMOCRSA-N 0.000 claims description 39
- DPDMMXDBJGCCQC-UHFFFAOYSA-N [Na].[Cl] Chemical compound [Na].[Cl] DPDMMXDBJGCCQC-UHFFFAOYSA-N 0.000 claims description 10
- 238000013019 agitation Methods 0.000 claims description 9
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims description 7
- 229940043232 butyl acetate Drugs 0.000 claims description 7
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims description 7
- MLFHJEHSLIIPHL-UHFFFAOYSA-N isoamyl acetate Chemical compound CC(C)CCOC(C)=O MLFHJEHSLIIPHL-UHFFFAOYSA-N 0.000 claims description 6
- PGMYKACGEOXYJE-UHFFFAOYSA-N pentyl acetate Chemical compound CCCCCOC(C)=O PGMYKACGEOXYJE-UHFFFAOYSA-N 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- 239000012074 organic phase Substances 0.000 claims description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 3
- YEJCDKJIEMIWRQ-UHFFFAOYSA-N Linopirdine Chemical compound O=C1N(C=2C=CC=CC=2)C2=CC=CC=C2C1(CC=1C=CN=CC=1)CC1=CC=NC=C1 YEJCDKJIEMIWRQ-UHFFFAOYSA-N 0.000 claims description 3
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 claims description 3
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 claims description 3
- 229940022663 acetate Drugs 0.000 claims description 3
- 150000001298 alcohols Chemical class 0.000 claims description 3
- 229940117955 isoamyl acetate Drugs 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- 239000000706 filtrate Substances 0.000 abstract description 19
- 150000003839 salts Chemical class 0.000 abstract description 7
- 238000005192 partition Methods 0.000 abstract description 5
- 239000000284 extract Substances 0.000 abstract description 4
- 239000002904 solvent Substances 0.000 abstract description 4
- 239000007864 aqueous solution Substances 0.000 abstract description 2
- NNRXCKZMQLFUPL-WBMZRJHASA-N (3r,4s,5s,6r,7r,9r,11r,12r,13s,14r)-6-[(2s,3r,4s,6r)-4-(dimethylamino)-3-hydroxy-6-methyloxan-2-yl]oxy-14-ethyl-7,12,13-trihydroxy-4-[(2r,4r,5s,6s)-5-hydroxy-4-methoxy-4,6-dimethyloxan-2-yl]oxy-3,5,7,9,11,13-hexamethyl-oxacyclotetradecane-2,10-dione;(2r,3 Chemical group OC(=O)[C@H](O)[C@@H](O)[C@@H]([C@H](O)CO)O[C@@H]1O[C@H](CO)[C@H](O)[C@H](O)[C@H]1O.O([C@@H]1[C@@H](C)C(=O)O[C@@H]([C@@]([C@H](O)[C@@H](C)C(=O)[C@H](C)C[C@@](C)(O)[C@H](O[C@H]2[C@@H]([C@H](C[C@@H](C)O2)N(C)C)O)[C@H]1C)(C)O)CC)[C@H]1C[C@@](C)(OC)[C@@H](O)[C@H](C)O1 NNRXCKZMQLFUPL-WBMZRJHASA-N 0.000 abstract 8
- 229940098008 erythrocin Drugs 0.000 abstract 7
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 abstract 4
- 239000011780 sodium chloride Substances 0.000 abstract 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 10
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 9
- -1 inorganic acid salt Chemical class 0.000 description 9
- 239000007787 solid Substances 0.000 description 6
- AFWGHSXNGWVDRI-STEFZQRDSA-N (e)-but-2-enedioic acid;(3r,4s,5s,6r,7r,9r,11r,12r,13s,14r)-6-[(2s,3r,4s,6r)-4-(dimethylamino)-3-hydroxy-6-methyloxan-2-yl]oxy-14-ethyl-7,12,13-trihydroxy-4-[(2r,4r,5s,6s)-5-hydroxy-4-methoxy-4,6-dimethyloxan-2-yl]oxy-3,5,7,9,11,13-hexamethyl-oxacyclotetr Chemical compound OC(=O)\C=C\C(O)=O.O([C@@H]1[C@@H](C)C(=O)O[C@@H]([C@@]([C@H](O)[C@@H](C)C(=O)[C@H](C)C[C@@](C)(O)[C@H](O[C@H]2[C@@H]([C@H](C[C@@H](C)O2)N(C)C)O)[C@H]1C)(C)O)CC)[C@H]1C[C@@](C)(OC)[C@@H](O)[C@H](C)O1 AFWGHSXNGWVDRI-STEFZQRDSA-N 0.000 description 5
- 229950007610 erythromycin acistrate Drugs 0.000 description 5
- 229920006395 saturated elastomer Polymers 0.000 description 5
- 229910000029 sodium carbonate Inorganic materials 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 4
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical class CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 4
- 239000006184 cosolvent Substances 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 3
- 238000004128 high performance liquid chromatography Methods 0.000 description 3
- 238000000967 suction filtration Methods 0.000 description 3
- 239000001103 potassium chloride Substances 0.000 description 2
- 235000011164 potassium chloride Nutrition 0.000 description 2
- 159000000000 sodium salts Chemical class 0.000 description 2
- RYDFXSRVZBYYJV-TYYBGVCCSA-N (e)-but-2-enedioic acid;sodium Chemical compound [Na].OC(=O)\C=C\C(O)=O RYDFXSRVZBYYJV-TYYBGVCCSA-N 0.000 description 1
- 208000006558 Dental Calculus Diseases 0.000 description 1
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 1
- 241000187747 Streptomyces Species 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 239000003120 macrolide antibiotic agent Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- LJCNRYVRMXRIQR-OLXYHTOASA-L potassium sodium L-tartrate Chemical compound [Na+].[K+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O LJCNRYVRMXRIQR-OLXYHTOASA-L 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- HELHAJAZNSDZJO-OLXYHTOASA-L sodium L-tartrate Chemical compound [Na+].[Na+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O HELHAJAZNSDZJO-OLXYHTOASA-L 0.000 description 1
- 239000001632 sodium acetate Substances 0.000 description 1
- 235000017281 sodium acetate Nutrition 0.000 description 1
- MFBOGIVSZKQAPD-UHFFFAOYSA-M sodium butyrate Chemical compound [Na+].CCCC([O-])=O MFBOGIVSZKQAPD-UHFFFAOYSA-M 0.000 description 1
- 239000001509 sodium citrate Substances 0.000 description 1
- ZNCPFRVNHGOPAG-UHFFFAOYSA-L sodium oxalate Chemical compound [Na+].[Na+].[O-]C(=O)C([O-])=O ZNCPFRVNHGOPAG-UHFFFAOYSA-L 0.000 description 1
- 229940039790 sodium oxalate Drugs 0.000 description 1
- 235000011006 sodium potassium tartrate Nutrition 0.000 description 1
- JXKPEJDQGNYQSM-UHFFFAOYSA-M sodium propionate Chemical compound [Na+].CCC([O-])=O JXKPEJDQGNYQSM-UHFFFAOYSA-M 0.000 description 1
- 239000004324 sodium propionate Substances 0.000 description 1
- 229960003212 sodium propionate Drugs 0.000 description 1
- 235000010334 sodium propionate Nutrition 0.000 description 1
- 239000001433 sodium tartrate Substances 0.000 description 1
- 229960002167 sodium tartrate Drugs 0.000 description 1
- 235000011004 sodium tartrates Nutrition 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229940095064 tartrate Drugs 0.000 description 1
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 description 1
- 229940038773 trisodium citrate Drugs 0.000 description 1
- ZNRSXPDDVNZGEN-UHFFFAOYSA-K trisodium;chloride;sulfate Chemical compound [Na+].[Na+].[Na+].[Cl-].[O-]S([O-])(=O)=O ZNRSXPDDVNZGEN-UHFFFAOYSA-K 0.000 description 1
Abstract
The invention discloses a method for extracting erythrocin form a fermentation filtrate or from an aqueous solution containing erythrocin by a salting-out. The method is that an adequate amount of sodium chloride or sodium sulfate or other salts are added in to the fermentation filtrate to reduce the solubility of the erythrocin to precipitate the erythrocin from the water liquid, or during extraction of the erythrocin with a hydrophobic organic solvent, an adequate amount of sodium chloride or sodium sulfate or other salts are added at the same time to improve the partition ratio of the erythrocin in the organic phrase. The method extracts the erythrocin from the fermentation filtrate, saves solvent media and improves the yield of the erythrocin.
Description
Technical field
A kind of microbiotic process for extracting is about from ferment filtrate, extracting Oxacyclotetradecane,erythromycin deriv with salting-out process or from the aqueous solution that contains Oxacyclotetradecane,erythromycin deriv, extracting Oxacyclotetradecane,erythromycin deriv concretely.
Background technology
Oxacyclotetradecane,erythromycin deriv is a kind of macrolide antibiotics, has been widely used in clinical.The production of Oxacyclotetradecane,erythromycin deriv is divided into two and goes on foot greatly, and the one, by streptomyces erythreus fermentation synthesis of erythromycin; The 2nd, from fermented liquid, Oxacyclotetradecane,erythromycin deriv is extract.
The process for extracting of Oxacyclotetradecane,erythromycin deriv has solvent extraction, three kinds of ion exchange method and macroreticular resin absorbing methods (Gu Juefen chief editor, microbiotic, Shanghai science tech publishing house, September calendar year 2001 the 1st edition, the 217th～218 page).
The present invention extracts Oxacyclotetradecane,erythromycin deriv with salting-out process from ferment filtrate; The invention main points are following: the sodium-chlor or sodium sulfate or other salts that in ferment filtrate, add capacity; Readjust the distribution ferment filtrating PH to 7.5～11.5 then and (also can transfer PH earlier; The back adds salt), Oxacyclotetradecane,erythromycin deriv is just separated out from ferment filtrate, and its eduction rate can reach more than 95%; Adopt filtration or centrifugation method to collect the Oxacyclotetradecane,erythromycin deriv of separating out then.Also can in the system of above-mentioned " 1 ", add an amount of (be equivalent to ferment filtrate volume 5～50%) hydrophobic solvent (as: alcohols of ETHYLE ACETATE, butylacetate, Isoamyl Acetate FCC, pentyl acetate, 4-methyl-2 pentanone, 4～8 carbon); Because the existence of salt; Thereby reduced the solubleness of Oxacyclotetradecane,erythromycin deriv in water, improved the partition ratio (partition rate) of Oxacyclotetradecane,erythromycin deriv in organic phase.For example: with the butylacetate/butanols or the octanol cosolvent that are equivalent to ferment filtrate volume 8%, under the situation that the salt that capacity is arranged exists, through single extraction, the percentage extraction of Oxacyclotetradecane,erythromycin deriv can reach more than 97%; If under no salt added situation, the solvent with 15% (butylacetate/butanols or octanol) extraction, the percentage extraction that extracts Oxacyclotetradecane,erythromycin deriv through twice just can reach about 95%.
This shows that the outstanding advantage of abomacetin extraction by salting-out is: can reduce the solvent usage quantity and reach 1/2～2/3.
Summary of the invention
The invention relates to the process for extracting of Oxacyclotetradecane,erythromycin deriv, definite saying is to adopt salting-out process to extract Oxacyclotetradecane,erythromycin deriv.This method feature is: the adding weight ratio is 3～85% inorganic acid salt or organic acid salt in abomacetin fermentation filtrating; Oxacyclotetradecane,erythromycin deriv is separated out from ferment filtrate; Perhaps when adopting hydrophobic organic solvent from ferment filtrate, to extract Oxacyclotetradecane,erythromycin deriv; The adding weight ratio is 3～85% inorganic acid salt or organic acid salt in system, is partition ratio thereby can significantly improve the partition rate of Oxacyclotetradecane,erythromycin deriv in the hydrophobicity organic phase.The sufficient quantity that in abomacetin fermentation filtrating, adds inorganic acid salt or organic acid salt is 8～36% (W/V).
Inorganic acid salt and organic acid salt used among the present invention are: the organic acid salt of sylvite, sodium salt, ammonium salt, hydrochloride, vitriol, 2～8 carbon.Described sylvite comprises: Repone K, vitriolate of tartar, soluble tartrate; Described sodium salt comprises: sodium-chlor, sodium sulfate, sodium acetate, Sodium Propionate, Sodium propanecarboxylate, sodium tartrate, Seignette salt, sodium oxalate, fumaric acid sodium, Trisodium Citrate.
The Oxacyclotetradecane,erythromycin deriv process for extracting that the present invention selects is following: the adding weight percent is 10～35% sodium-chlor or sodium sulfate in ferment filtrate; Under agitation condition; Readjust the distribution ferment filtrating PH7.2～11; Treat that the Oxacyclotetradecane,erythromycin deriv eduction rate reaches 93% when above, get final product solid-liquid separation, obtain to contain the bullion of Oxacyclotetradecane,erythromycin deriv; Also can readjust the distribution ferment filtrating pH value earlier is 7.2～11, and then, the adding weight percent is 10～35% sodium-chlor or sodium sulfate.
Also can in ferment filtrate, add hydrophobic organic solvent, and to add weight percent simultaneously be 5～35% sodium-chlor or sodium sulfate, under agitation condition; Readjust the distribution ferment filtrating PH7.2～11, behind the thorough mixing, leave standstill or centrifugal; Abandon water, must contain the organic phase of Oxacyclotetradecane,erythromycin deriv.
In the present invention; When salting-out process combines with extraction process to use; Used hydrophobic organic solvent is: the alcohols of ETHYLE ACETATE, butylacetate, Isoamyl Acetate FCC, pentyl acetate, 4-methyl-2 pentanone, 4～8 carbon, and they can use separately, also can more than one form the cosolvent use; Usage quantity is 2～50% of a ferment filtrate amount, volume per-cent.
Embodiment
The following example is provided so that people can make much of the present invention, but this can not be interpreted as the restriction to claim scope of the present invention and core content.
Instance 1, get the ferment filtrate 1L that tires to 3321ug Oxacyclotetradecane,erythromycin deriv/ml, under agitation condition, add 300g sodium-chlor, transfer liquid PH8.2 with saturated aqueous sodium carbonate, stir after 5 minutes, suction filtration must contain the wet solids of Oxacyclotetradecane,erythromycin deriv.
The wet solids that will contain Oxacyclotetradecane,erythromycin deriv is all used dissolve with methanol, filtration, carries out HPLC and analyzes, and wherein containing Oxacyclotetradecane,erythromycin deriv is 3198mg, and yield is 96.3% (weight ratio).
Instance 2, get the ferment filtrate 1L that tires to 3321ug Oxacyclotetradecane,erythromycin deriv/ml, under agitation condition, add 200g sodium-chlor, transfer liquid PH8.2 with saturated aqueous sodium carbonate, stir after 5 minutes, suction filtration must contain the wet solids of Oxacyclotetradecane,erythromycin deriv.
The wet solids that will contain Oxacyclotetradecane,erythromycin deriv is all used dissolve with methanol, filtration, carries out HPLC and analyzes, and wherein containing Oxacyclotetradecane,erythromycin deriv is 3039mg, and yield is 91.5% (weight ratio).
Instance 3, get the ferment filtrate 1L that tires to 3321ug Oxacyclotetradecane,erythromycin deriv/ml, be heated to 35 ℃, under agitation condition, add 200g sodium sulfate, transfer liquid PH8.2 with saturated aqueous sodium carbonate, stir after 5 minutes, suction filtration must contain the wet solids of Oxacyclotetradecane,erythromycin deriv.
The wet solids that will contain Oxacyclotetradecane,erythromycin deriv is all used dissolve with methanol, filtration, carries out HPLC and analyzes, and wherein containing Oxacyclotetradecane,erythromycin deriv is 3231mg, and yield is 97.3% (weight ratio).
Instance 4,
Experimental group: get the ferment filtrate 1L that tires to 3321ug Oxacyclotetradecane,erythromycin deriv/ml, be heated to 35 ℃, under agitation condition; Add 80ml butylacetate/butanols cosolvent, add 300g sodium-chlor then, transfer liquid PH8.2 with saturated aqueous sodium carbonate; Stir after 5 minutes; Leave standstill, treat complete layering after, Oxacyclotetradecane,erythromycin deriv content is measured in water intaking mutually.
Control group: other gets the ferment filtrate 1L that tires to 3321ug Oxacyclotetradecane,erythromycin deriv/ml, is heated to 35 ℃, under agitation condition; Add 80ml butylacetate/butanols cosolvent; Transfer liquid PH8.2 with saturated aqueous sodium carbonate then, stir after 5 minutes, leave standstill; After treating complete layering, Oxacyclotetradecane,erythromycin deriv content is measured in water intaking mutually.
Experimental result:
Residual tiring is that 142ug/ml, percentage extraction are 96% in the experimental group water liquid;
Residual tiring is that 587ug/ml, percentage extraction are 82.3% in the control group water liquid.
Claims (2)
1. Oxacyclotetradecane,erythromycin deriv process for extracting; It is characterized in that in abomacetin fermentation filtrating, adding weight percent and be 10～35% sodium-chlor or sodium sulfate; Under agitation condition, readjust the distribution ferment filtrating PH 7.2～11, treat that the Oxacyclotetradecane,erythromycin deriv eduction rate reaches 93% when above; Carry out solid-liquid separation, can obtain to contain the bullion of Oxacyclotetradecane,erythromycin deriv; Also can readjust the distribution ferment filtrating pH value earlier is 7.2～11, adds weight percent then and be 10～35% sodium-chlor or sodium sulfate.
2. Oxacyclotetradecane,erythromycin deriv process for extracting is characterized in that in abomacetin fermentation filtrating, adding volume per-cent and is 2～50% hydrophobic organic solvent, and to add weight percent be 5～35% sodium-chlor or sodium sulfate; Under agitation condition; Readjust the distribution ferment filtrating PH 7.2～11, behind the thorough mixing, leave standstill phase-splitting or centrifugal phase-splitting; Abandon water, must contain the organic phase of Oxacyclotetradecane,erythromycin deriv; Above-described hydrophobic organic solvent is: the alcohols of ETHYLE ACETATE, butylacetate, Isoamyl Acetate FCC, pentyl acetate, 4-methyl-2 pentanone, 4～8 carbon.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200710195544A CN101450960B (en) | 2007-12-07 | 2007-12-07 | Abomacetin extraction by salting-out method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200710195544A CN101450960B (en) | 2007-12-07 | 2007-12-07 | Abomacetin extraction by salting-out method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101450960A CN101450960A (en) | 2009-06-10 |
| CN101450960B true CN101450960B (en) | 2012-08-29 |
Family
ID=40733461
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200710195544A Active CN101450960B (en) | 2007-12-07 | 2007-12-07 | Abomacetin extraction by salting-out method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101450960B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103159812B (en) * | 2011-12-08 | 2016-03-23 | 湖南中创化工股份有限公司 | A kind of method extracting erythromycin from the erythromycin aqueous solution |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2881162A (en) * | 1953-11-16 | 1959-04-07 | Abbott Lab | Recovery process |
-
2007
- 2007-12-07 CN CN200710195544A patent/CN101450960B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2881162A (en) * | 1953-11-16 | 1959-04-07 | Abbott Lab | Recovery process |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101450960A (en) | 2009-06-10 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US4886889A (en) | Process for recovery of an amino acid from aqueous mixtures thereof | |
| CN101381756B (en) | Purification method of super tylosin | |
| JP2009519245A (en) | Purification method of echinocandin type compound | |
| CN113648834B (en) | Ceramic membrane and preparation method and application thereof | |
| CN101619069A (en) | Preparation method of cefotiam hexetil hydrochloride | |
| CN101921302B (en) | Purification technology of rokitamycin | |
| CN102040638A (en) | Method for preparing nonsolvent of high-purity natamycin | |
| CN106188188B (en) | A kind of preparation method of avermectin | |
| CN101450960B (en) | Abomacetin extraction by salting-out method | |
| CN103275150A (en) | Method for refining and preparing erythromycin thiocyanate | |
| CN100513578C (en) | Method for extracting natural beta-caroetne | |
| CN101531694A (en) | Method for extracting erythromycins by salting-out method | |
| CN100402516C (en) | Prepn process of mofe-til mycophenolate | |
| CN1289609C (en) | Method for preparing crystal of lycopene and concentrate | |
| CN101580515B (en) | Method for extracting and purifying staurosporin | |
| CN101156664B (en) | Method for distilling fucoidin from sea tangle caustic refining liquid | |
| CN103012344B (en) | Method of recovering lovastatin from lovastatin crystal mother liquor | |
| CN101709072B (en) | Method for efficiently extracting and purifying natamycin | |
| CN103709219A (en) | Tylosin extraction method | |
| CN104341377B (en) | The method reclaiming lovastatin from lovastatin crystalline mother solution | |
| CN110540570A (en) | method for separating and purifying fusidic acid through ion exchange resin | |
| CN1470515A (en) | Method for extracting tetrodotoxin from globefish livers | |
| CN109651438A (en) | A kind of preparation of modified oxidized magnesium and its application in L-Ascorbic Acid L-O-Phosphate | |
| CN107937472A (en) | A kind of method of straight-through synthesis Amoxicillin | |
| CN107446965A (en) | A kind of preparation method of ornithine hydrochloride |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| ASS | Succession or assignment of patent right |
Owner name: BEIJING AGRICHINA PHARMACEUTICAL CO., LTD. Free format text: FORMER OWNER: PAN ZHENDE Effective date: 20131127 |
|
| C41 | Transfer of patent application or patent right or utility model | ||
| COR | Change of bibliographic data |
Free format text: CORRECT: ADDRESS; FROM: 100089 HAIDIAN, BEIJING TO: 100000 CHANGPING, BEIJING |
|
| TR01 | Transfer of patent right |
Effective date of registration: 20131127 Address after: 100000 Wang Zhuang Industrial Zone, Shahe Airport Road, Changping District, Beijing Patentee after: BEIJING AGRICHINA PHARMACEUTICAL CO., LTD. Address before: 100089 Beijing box 8956 Haidian District Wanliu spring Sinorama District Building 5 room 103 Patentee before: Pan Zhende |
|
| CP03 | Change of name, title or address | ||
| CP03 | Change of name, title or address |
Address after: 102209, Changping District science and Technology Park, Beijing, No. 37, building 16, No. 2, building C2034 Patentee after: Beijing Zhongnonghuawei pharmaceutical Limited by Share Ltd Address before: 100000 Wang Zhuang Industrial Zone, Shahe Airport Road, Changping District, Beijing Patentee before: BEIJING AGRICHINA PHARMACEUTICAL CO., LTD. |
|
| PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: Abomacetin extraction by salting-out method Effective date of registration: 20180910 Granted publication date: 20120829 Pledgee: Huaxia Bank Beijing branch Wanliu Limited by Share Ltd Pledgor: Beijing Zhongnonghuawei pharmaceutical Limited by Share Ltd Registration number: 2018990000795 |
|
| PC01 | Cancellation of the registration of the contract for pledge of patent right | ||
| PC01 | Cancellation of the registration of the contract for pledge of patent right |
Date of cancellation: 20191122 Granted publication date: 20120829 Pledgee: Huaxia Bank Beijing branch Wanliu Limited by Share Ltd Pledgor: Beijing Zhongnonghuawei pharmaceutical Limited by Share Ltd Registration number: 2018990000795 |
|
| PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: Abomacetin extraction by salting-out method Effective date of registration: 20191128 Granted publication date: 20120829 Pledgee: Huaxia Bank Beijing branch Wanliu Limited by Share Ltd Pledgor: Beijing Zhongnonghuawei pharmaceutical Limited by Share Ltd Registration number: Y2019990000606 |
|
| CP01 | Change in the name or title of a patent holder | ||
| CP01 | Change in the name or title of a patent holder |
Address after: 102209 C2034 2, 16 building, No. 37 Chao Yuan Road, Changping District science and Technology Park, Beijing. Patentee after: Zhongnonghuawei Pharmaceutical Co., Ltd Address before: 102209 C2034 2, 16 building, No. 37 Chao Yuan Road, Changping District science and Technology Park, Beijing. Patentee before: Beijing Zhongnong Huawei Pharmaceutical Co.,Ltd. |
|
| PC01 | Cancellation of the registration of the contract for pledge of patent right |
Date of cancellation: 20210531 Granted publication date: 20120829 Pledgee: Huaxia Bank Beijing branch Wanliu Limited by Share Ltd. Pledgor: Beijing Zhongnong Huawei Pharmaceutical Co.,Ltd. Registration number: Y2019990000606 |
|
| PC01 | Cancellation of the registration of the contract for pledge of patent right |