CN101245047B - Purification method for tryptophane - Google Patents
Purification method for tryptophane Download PDFInfo
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- CN101245047B CN101245047B CN2008100657624A CN200810065762A CN101245047B CN 101245047 B CN101245047 B CN 101245047B CN 2008100657624 A CN2008100657624 A CN 2008100657624A CN 200810065762 A CN200810065762 A CN 200810065762A CN 101245047 B CN101245047 B CN 101245047B
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- tryptophane
- filtrate
- purification method
- gac
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- QIVBCDIJIAJPQS-VIFPVBQESA-N L-tryptophane Chemical compound C1=CC=C2C(C[C@H](N)C(O)=O)=CNC2=C1 QIVBCDIJIAJPQS-VIFPVBQESA-N 0.000 title claims abstract description 45
- QIVBCDIJIAJPQS-UHFFFAOYSA-N Tryptophan Natural products C1=CC=C2C(CC(N)C(O)=O)=CNC2=C1 QIVBCDIJIAJPQS-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000000746 purification Methods 0.000 title claims abstract description 16
- 229960004799 tryptophan Drugs 0.000 title claims description 41
- 239000006035 Tryptophane Substances 0.000 title claims description 37
- 239000000706 filtrate Substances 0.000 claims abstract description 26
- 239000000047 product Substances 0.000 claims abstract description 14
- 238000002425 crystallisation Methods 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 230000008025 crystallization Effects 0.000 claims abstract description 9
- 238000010301 surface-oxidation reaction Methods 0.000 claims description 16
- 239000012141 concentrate Substances 0.000 claims description 11
- 238000005406 washing Methods 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 9
- -1 peracid salt Chemical class 0.000 claims description 9
- 238000010792 warming Methods 0.000 claims description 9
- 150000003839 salts Chemical class 0.000 claims description 8
- 239000013078 crystal Substances 0.000 claims description 5
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 4
- WQYVRQLZKVEZGA-UHFFFAOYSA-N hypochlorite Chemical compound Cl[O-] WQYVRQLZKVEZGA-UHFFFAOYSA-N 0.000 claims description 4
- 239000012528 membrane Substances 0.000 claims description 4
- 238000005374 membrane filtration Methods 0.000 claims description 4
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 230000004913 activation Effects 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 150000002500 ions Chemical class 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- XTEGARKTQYYJKE-UHFFFAOYSA-N chloric acid Chemical compound OCl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-N 0.000 claims description 2
- 229940005991 chloric acid Drugs 0.000 claims description 2
- 239000007800 oxidant agent Substances 0.000 claims description 2
- 230000006353 environmental stress Effects 0.000 claims 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 12
- 239000012535 impurity Substances 0.000 abstract description 5
- 238000001816 cooling Methods 0.000 abstract description 4
- 238000003756 stirring Methods 0.000 abstract description 4
- 239000012452 mother liquor Substances 0.000 abstract description 2
- 239000002699 waste material Substances 0.000 abstract description 2
- 230000001590 oxidative effect Effects 0.000 abstract 1
- 238000002207 thermal evaporation Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 12
- 238000010521 absorption reaction Methods 0.000 description 8
- 238000002834 transmittance Methods 0.000 description 8
- 239000012043 crude product Substances 0.000 description 6
- 239000002904 solvent Substances 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 229910052785 arsenic Inorganic materials 0.000 description 3
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- PVNIIMVLHYAWGP-UHFFFAOYSA-N Niacin Chemical compound OC(=O)C1=CC=CN=C1 PVNIIMVLHYAWGP-UHFFFAOYSA-N 0.000 description 2
- 150000003863 ammonium salts Chemical class 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 239000003610 charcoal Substances 0.000 description 2
- 238000004737 colorimetric analysis Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005342 ion exchange Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 238000001953 recrystallisation Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- QZAYGJVTTNCVMB-UHFFFAOYSA-N serotonin Chemical compound C1=C(O)C=C2C(CCN)=CNC2=C1 QZAYGJVTTNCVMB-UHFFFAOYSA-N 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 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 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229930013930 alkaloid Natural products 0.000 description 1
- 150000003797 alkaloid derivatives Chemical class 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000005515 coenzyme Substances 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 235000020776 essential amino acid Nutrition 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- SEOVTRFCIGRIMH-UHFFFAOYSA-N indole-3-acetic acid Chemical compound C1=CC=C2C(CC(=O)O)=CNC2=C1 SEOVTRFCIGRIMH-UHFFFAOYSA-N 0.000 description 1
- 125000001041 indolyl group Chemical group 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 229960003512 nicotinic acid Drugs 0.000 description 1
- 235000001968 nicotinic acid Nutrition 0.000 description 1
- 239000011664 nicotinic acid Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000008213 purified water Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 229940076279 serotonin Drugs 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000000108 ultra-filtration Methods 0.000 description 1
Abstract
The invention discloses a purification method of tryptophan; wherein, the tryptophan to be purified is dissolved in water; filtrate which is absorbed after being added with surface oxidative activated carbon is treated with vacuum condensation into a volumn which is 6 to 10 percent of the original volume at the temperature of 40 to 65 DEG C, and the temperature is reduced to 3 to 5 DEG C to carry out stirring and crystallization to obtain pure products; an intermittent concentration cooling crystallization mode is preferably chosen in the concentration process. The purification method basically has no three wastes; the mother liquor can be recycled and used for a plurality of times; the purification method is low in cost, simple in technical control, high in the purity of the obtained products and low in impurity content; and the purification method more conveniently obtains the tryptophan products which meet the requirements of the version 2005 of Chinese pharmacopoeia and the 29th version of American pharmacopoeia.
Description
Technical field
The present invention relates to a kind of amino acid whose method of purification, specifically is the method for purification of tryptophane.
Background technology
The molecular formula C of L-tryptophane
11H
12N
2O
2, molecular weight 204.23, CAS No.73-22-3, structural formula is as follows:
The L-tryptophane is one of eight kinds of indispensable amino acids of human body, in vivo, tryptophane can change into important physiologically active substances such as serotonin, indolylacetic acid, nicotinic acid, alkaloid and coenzyme, participate in regulating proteinic synthetic, the growing of humans and animals, metabolism are played an important role, therefore research and produce and meet edible and medicinal high purity tryptophane product has important society and economic implications.
The tryptophane purification technique mainly adopts absorption and ion exchange method purifying at present, and by neutralization or cooling recrystallization, complex process has adopted organic solvent, increases solvent recuperation and post-processing difficulty, and environmental protection is caused disadvantageous effect in the presence of lower aliphatic alcohols.
Japanese Patent prospectus JP895/1983 adopts tryptophane solution earlier by nonpolar porous resin, pass through the method purification tryptophane of ultrafiltration again, but Impurity removal is undesirable, does not reach the high transmission rate requirement.Japanese Patent prospectus JP39857/1984 proposes tryptophane and dissolves with alkali lye, in the presence of lower aliphatic alcohols or ketone in and crystallization, raising purity, but Impurity removal is still insufficient, and transmittance is difficult to reach 95%, and, use a large amount of solvents, solvent need reclaim and aftertreatment.Japanese Patent prospectus JP126070/1986 is dissolved in tryptophane in 95～100 ℃ the acidic aqueous solution, use activated carbon adsorption, behind the filtering carbon, again through nonpolar porous resin absorption, the wash-out tryptophane, in the presence of lower aliphatic alcohols in and crystallization, because of the indole ring instability of tryptophane, decompose and the generation coloring matter at more acid high-temperature, transmittance is undesirable.
US Patent specification US4820825 under pH value 1～4 condition, uses charcoal absorption with tryptophane solution for 50 ℃, again through nonpolar porous resin absorption, in in the presence of lower aliphatic alcohols and crystallization, transmittance reaches more than 95%, but uses a large amount of solvents equally, needs the solvent recuperation aftertreatment.Among the US Patent specification US5057615, tryptophane in 40～115 ℃ aqueous acetic acid, is used charcoal absorption earlier, behind the filtering carbon, decrease temperature crystalline, tryptophane can reach 99% content, but exists tryptophane to decompose discoloration problem equally.
Domestic tryptophane purification technique report is less, " research of ion-exchange absorption L-tryptophane " (biotechnology journal, 1996,12 (4): 499～502 pages) research is carried out separation and purification with absorption, the wash-out of Zeo-karb to the L-tryptophane in the aqueous solution; " separation of tryptophane during enzyme process is synthetic " (industrial microorganism, 1996,26 (1): 27～30 pages) cross 330 and 732 ion exchange resin columnss in series earlier with tryptophane solution, 5% acetone and 5% ammonia water mixture wash-out, concentrate crude product, activated carbon decolorizing again is with 60% ethanol recrystallization repeatedly, product purity 99%, though reach purity requirement, complex process is loaded down with trivial details, with an organic solvent, aftertreatment requires high, and industrialization is poor for applicability.
Summary of the invention
The purpose of this invention is to provide a kind of technology and simply obtain high purity and high transmission rate crystalline purification method for tryptophane.
The present invention includes following steps:
A. tryptophane to be purified is dissolved in the water, the formation weight concentration is 1～1.5% solution, add the surface oxidation gac by 0.5～2.5% of tryptophane weight to be purified, the whip attachment after-filtration is removed the surface oxidation gac, carries out membrane filtration with 0.15～0.4 μ m filtering membrane again;
B. filtrate to original volume 6～10%, is cooled to 3～5 ℃ of stirred crystallization at 40～65 ℃ of following vacuum concentration;
C. the white crystal that obtains of crystal solution centrifuging after the pure water washing, gets pure product 30～45 ℃ of following vacuum-dryings.
In steps A, the surface oxidation gac is in sour environment, after gac is immersed in aqueous oxidizing agent solution, washing to washings with pure water does not have acid ion, drying is again 80～250 ℃ of oven dry activation down, wherein, described oxygenant is: concentrated nitric acid, chromic salt, hydrogen peroxide, peracid salt, hypochlorite, permanganate, the mixture of one or more of perchloric acid or its salt, chloric acid or its salt.
Tryptophane to be purified can be synthetic or the crude product that obtains through preliminary crystallization of the tryptophane of fermentation.Preferably selecting tryptophane for use is crude product more than 95%, if tryptophane is lower than 95%, can repeats the present invention operation and finish purifying.The absorption of the dissolving of tryptophane crude product, surface oxidation gac is preferably under 40～45 ℃ to be carried out, to obtain working efficiency preferably.Preferred 15～60 minutes of surface oxidation gac whip attachment time.Removing adoptable 10～15 μ m strainers of surface oxidation gac filters.
Among the step B, concentrate system pressure is 10～40Kpa preferably.
Concentration process preferably adopts batch concentration crystallisation by cooling mode, get part filtrate earlier and when being concentrated into 10～35% volumes for 40～65 ℃, stop heating, being cooled to 15～25 ℃ stirred 40～80 minutes, be warming up to 40～65 ℃ then and concentrate and progressively add part filtrate, control adding speed makes the concentrated solution volume be 10～35% of filtrate volume before adding, being cooled to 15～25 ℃ again stirred 20～40 minutes, repeat to heat up-replenish filtrate-cooling-insulation operation until adding whole filtrates, 6～10% of the extremely whole filtrate volumes of reconcentration.
Concentration process is more preferably: get filtrate 20～40% and stop heating when being concentrated into 20～35% volumes for 40～65 ℃, being cooled to 15～25 ℃ stirred 40～80 minutes, be warming up to 40～65 ℃ then and concentrate and progressively replenish filtrate 20～40%, control adding speed makes the concentrated solution volume for concentrating 15～25% of front volume, being cooled to 15～25 ℃ again stirred 20～40 minutes, be warming up to 40～65 ℃ again and concentrate and constantly replenish residual filtrate, keep concentrating volume for concentrating 12～16% of front volume, after all filtrate added, reconcentration was to concentrating 6～10% of front volume.
The present invention carries out oxide treatment to gac, formed the oxidation carbon-coating of one deck band portion negative charge at activated carbon surface, adopt the surface oxidation gac as sorbing material, except decoloration performance with gac, the ability that also has adsorbing metal ions, good decolouring and Impurity removal effect are arranged, and the surface oxidation activated carbon is easy to prepare, and raw material is easy to get.By control condensing crystal process, adopt batch concentration crystallisation by cooling mode, make the solution degree of supersaturation in whole crystallisation process, maintain a lower level, avoid impurity to be embedded in the lattice, the pure product of crystallization have bigger granularity.The product that the present invention obtains is a white crystalline powder, purity＞99%, transmittance＞96%, molysite＜10ppm, heavy metal＜10ppm, arsenic salt＜1ppm, muriate＜0.02%, vitriol＜0.02%, substantially do not have the three wastes, mother liquor can repeatedly recycle, and cost is low, technology controlling and process is simple, and what more convenient acquisition met Chinese Pharmacopoeia 2005 editions and American Pharmacopeia 29 editions requires the tryptophane product.
Embodiment
Embodiment 1
Gac is immersed in the concentrated nitric acid, stirs 30 minutes after-filtration, washing to washings with pure water does not have acid ion, and drying 120 ℃ of oven dry activation down, obtains the surface oxidation gac again.
Content 97.3wt%, the tryptophane crude product of transmittance 53% is dissolved in 150 liters of 45 ℃ of pure water for 1.8 kilograms, adds the above-mentioned surface oxidation gac of 18g, stirs 30 minutes, solution is removed the surface oxidation gac by 12 μ m strainers, carry out membrane filtration with 0.22 μ m filtering membrane again, get 50 liters of filtrates, be concentrated into about 17.5 liters in the 10Kpa pressure environment at 45 ℃, be cooled to 15 ℃, stirred 1 hour, and be warming up to 45 ℃ again and concentrate and constantly replenish filtrate, about 23 liters of maintenance concentrated solution volume, continuous when adding filtrate and reaching 50 liters, be cooled to 25 ℃, stirred 30 minutes, be warming up to 45 ℃ again and concentrate and constantly replenish filtrate, keep concentrating about 23 liters of volume, after all filtrates add, be concentrated into 15 liters, be cooled to 5 ℃, stirred 2 hours, filter, a small amount of pure water washing, vacuum drying obtains pure product.After testing, tryptophane 99.7% in the pure product, molysite 4ppm, and ammonium salt does not detect, heavy metallic salt 3ppm, arsenic salt＜0.5ppm (colorimetry), muriate 0.007%, vitriol does not detect, transmittance 97.6%, specific rotatory power-31.3 °.
Embodiment 2
Content 97.3wt%, the tryptophane crude product of transmittance 53% is dissolved in 150 liters of 45 ℃ of purified water for 1.8 kilograms, adds 18 gram embodiment, 1 described surface oxidation gac, stirs 30 minutes, solution is removed the surface oxidation gac by 12 μ m strainers, carry out membrane filtration with 0.22 μ m filtering membrane again, get 50 liters of filtrates, be concentrated into about 12 liters in the 30KPa pressure environment at 60 ℃, be cooled to 25 ℃, stirred 2 hours, and continued to be warming up to 60 ℃ and concentrate and constantly additional filtrate, keep concentrating about 20 liters of volume, continuous add 50 liters of filtrates after, be cooled to 25 ℃, stirred 30 minutes, be warming up to 60 ℃ again and concentrate and constantly replenish filtrate, keep concentrating about 20 liters of volume, after all filtrates add, be concentrated into 10 liters, be cooled to 4 ℃, stirred 2 hours, filter, a small amount of pure water washing, vacuum drying obtains pure product.After testing, tryptophane 99.2% in the pure product, molysite 5ppm, and ammonium salt does not detect, heavy metallic salt 5ppm, arsenic salt＜0.5ppm (colorimetry), muriate 0.008%, vitriol does not detect, transmittance 96.4%, specific rotatory power-31.9 °.
Claims (3)
1. purification method for tryptophane may further comprise the steps:
A. tryptophane to be purified is dissolved in the water, the formation weight concentration is 1～1.5% solution, add the surface oxidation gac by 0.5～2.5% of tryptophane weight to be purified, the whip attachment after-filtration is removed the surface oxidation gac, carries out membrane filtration with 0.1 5～0.4 μ m filtering membrane again;
B. filtrate to original volume 6～10%, is cooled to 3～5 ℃ of stirred crystallization at 40～65 ℃ of following vacuum concentration;
C. the white crystal that obtains of crystal solution centrifuging after the pure water washing, gets pure product 30～45 ℃ of following vacuum-dryings;
Above-mentioned surface oxidation gac is in sour environment, after gac is immersed in aqueous oxidizing agent solution, washing to washings with pure water does not have acid ion, dry, again 80～250 ℃ of oven dry activation down, wherein, described oxygenant is: more than one of concentrated nitric acid, chromic salt, hydrogen peroxide, peracid salt, hypochlorite, permanganate, perchloric acid or its salt, chloric acid or its salt.
2. according to the described purification method for tryptophane of claim 1, it is characterized in that, among the described step B, concentration process is: get filtrate 20～40% and stop heating when being concentrated into 20～35% volumes for 40～65 ℃, being cooled to 15～25 ℃ stirred 40～80 minutes, be warming up to 40～65 ℃ then and concentrate and progressively replenish filtrate 20～40%, control adding speed makes the concentrated solution volume for concentrating 15～25% of front volume, being cooled to 15～25 ℃ again stirred 20～40 minutes, be warming up to 40～65 ℃ again and concentrate and constantly replenish residual filtrate, keep concentrating volume for concentrating 12～16% of front volume, after all filtrate added, reconcentration was to concentrating 6～10% of front volume.
3. according to claim 1 or 2 described purification method for tryptophane, it is characterized in that among the described step B, spissated environmental stress is 10～40KPa.
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| CN2008100657624A CN101245047B (en) | 2008-03-04 | 2008-03-04 | Purification method for tryptophane |
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Families Citing this family (12)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101550101B (en) * | 2009-01-20 | 2011-09-07 | 福建省建阳武夷味精有限公司 | Method for clean purifying L-tryptophan by utilizing fermented liquid |
| CN101717360B (en) * | 2009-12-24 | 2011-09-07 | 安徽丰原发酵技术工程研究有限公司 | Method for extracting L-tryptophan from fermentation liquid |
| CN102249980B (en) * | 2011-05-10 | 2013-09-25 | 中国人民解放军第四军医大学 | Process for controlling generation of 4,5-tryptophan-diketone in tryptophan |
| CN102304077A (en) * | 2011-06-24 | 2012-01-04 | 南通诚信氨基酸有限公司 | Method for purifying tryptophan |
| CN103044309A (en) * | 2012-09-07 | 2013-04-17 | 赵立地 | Method for purifying tryptophan |
| CN104447942A (en) * | 2013-09-12 | 2015-03-25 | 深圳翰宇药业股份有限公司 | Method for purifying polypeptide containing amino acid susceptible to oxidation |
| EP3092218B1 (en) | 2014-01-07 | 2022-03-09 | Novasep Process Solutions | Process for the purification of aromatic aminoacids |
| CN104829519A (en) * | 2015-05-15 | 2015-08-12 | 南通荣泰生物科技有限公司 | Purification process of L-tryptophan |
| CN105481750B (en) * | 2015-12-10 | 2018-02-27 | 河南巨龙生物工程股份有限公司 | A kind of process for extracting high-purity medicine rank tryptophan |
| CN105949111B (en) * | 2016-05-24 | 2018-10-19 | 南通紫琅生物医药科技有限公司 | A kind of preparation process of high-purity high light transmission L-Trp |
| CN106478462B (en) * | 2016-09-23 | 2018-04-24 | 精晶药业股份有限公司 | A kind of method of purification of raw material citrulling |
| CN113354569A (en) * | 2021-06-04 | 2021-09-07 | 无锡晶海氨基酸股份有限公司 | Method for purifying tryptophan |
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Owner name: SHANTOU JIAHE BIOTECHNOLOGY CO., LTD. Free format text: FORMER OWNER: ZIGUANG GUHAN AMINO-ACID CO., LTD., SHANTOU Effective date: 20121224 |
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Effective date of registration: 20121224 Address after: Jinping District West Port Road 515000 Guangdong city of Shantou Province Wang No. 4 Patentee after: SHANTOU JIAHE BIOLOGICAL TECHNOLOGY CO.,LTD. Address before: Jinping District West Port Road 515000 Guangdong city of Shantou Province Wang No. 4 Patentee before: Shantou Ziguang Guhan Amino Acid Co.,Ltd. |
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Denomination of invention: Purification method for tryptophane Effective date of registration: 20170822 Granted publication date: 20100714 Pledgee: Shantou SME financing Company limited by guarantee Pledgor: SHANTOU JIAHE BIOLOGICAL TECHNOLOGY CO.,LTD. Registration number: 2017990000770 |
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Date of cancellation: 20190108 Granted publication date: 20100714 Pledgee: Shantou SME financing Company limited by guarantee Pledgor: SHANTOU JIAHE BIOLOGICAL TECHNOLOGY CO.,LTD. Registration number: 2017990000770 |
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Denomination of invention: Purification method of tryptophan Effective date of registration: 20231214 Granted publication date: 20100714 Pledgee: Shantou Bay Rural Commercial Bank Co.,Ltd. Pledgor: SHANTOU JIAHE BIOLOGICAL TECHNOLOGY CO.,LTD. Registration number: Y2023980071776 |