CN102146052B - Method for preparing tryptophan - Google Patents

Method for preparing tryptophan Download PDF

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CN102146052B
CN102146052B CN 201010603780 CN201010603780A CN102146052B CN 102146052 B CN102146052 B CN 102146052B CN 201010603780 CN201010603780 CN 201010603780 CN 201010603780 A CN201010603780 A CN 201010603780A CN 102146052 B CN102146052 B CN 102146052B
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tryptophan
lower aliphatic
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water
solution
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CN102146052A (en
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马冉
左良成
于传军
张利强
朱维忠
王文笙
常晓菲
齐志强
王静
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山东鲁抗医药股份有限公司
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Abstract

本发明涉及一种氨基酸的制备方法,尤其涉及提供一种简便高效的制备高透光率色氨酸的方法。 The present invention relates to a method for preparing amino acid, in particular, to provide a simple and efficient method of producing a high transmittance tryptophan. 该方法包括:将粗品色氨酸加入混合溶解液中,加热使其全部溶解,加入活性炭吸附半小时后,过滤除去活性炭,再用滤膜进行膜过滤,其中混合溶解液为纯化水、低级脂肪醇或低级脂肪酮和低级脂肪酸的混合液;将滤液在搅拌下缓慢结晶,并使用物理方法进一步降温使其充分结晶;结晶液过滤得到的白色晶体经充分洗涤,调节PH值后再次过滤,干燥得纯品;所有母液均可循环利用。 The method comprising: mixing the crude tryptophan dissolved solution was added, heated to dissolve all, a half hour after adding activated carbon adsorption, the activated carbon was removed by filtration, and then membrane filtration membrane, wherein the fluid is mixed and dissolved in purified water, lower aliphatic lower aliphatic ketones or a mixture of alcohols and lower fatty acids; and the filtrate was slowly crystallized under stirring, and cooling it using a physical method further sufficiently crystallized; crystallized was filtered to give white crystals were washed well, after adjusting the PH value filtered again, and dried pure commodities; all liquor can be recycled. 此法获得的色氨酸产品符合2010版药典中药用级标准规定的透光率95%等各项指标;且该法所使用溶媒单一,不需单独回收,母液简单处理后可重复使用,不造成任何污染。 Light transmittance of the obtained product complies with this method tryptophan Chinese Pharmacopoeia 2010 edition with a predetermined standard level of 95% of the targets; law and the single solvent used, alone without recycling, the mother liquor can be reused after simple treatment, not cause any pollution.

Description

一种制备色氨酸的方法 A process for preparing tryptophan

技术领域 FIELD

[0001] 本发明涉及一种氨基酸的制备方法,具体是制备高透光率色氨酸的方法。 [0001] The present invention relates to a method for preparing amino acid, in particular a method for preparing a high light transmittance tryptophan.

[0002] 背景技术 [0002] BACKGROUND OF THE INVENTION

[0003] L-色氨酸的分子式C11H12N2O2,分子量204.23,别名氨基Π引哚丙酸,结构式如下: [0003] L- tryptophan formula C11H12N2O2, molecular weight 204.23, Π alias amino acid indole, the following structural formula:

Figure CN102146052BD00041

[0004] L-色氨酸为白色或微黄色结晶或结晶性粉末;无臭或微臭,稍有苦味,289°C分解,在水中微溶,不溶于乙醇;在稀酸或稀碱中溶解,长时间光照则着色,与水共热产生少量吲哚,如在氢氧化钠、硫酸铜存在下加热,则产生大量吲哚,与酸在暗处加热叫稳定,与其他氨基酸、糖类、醛类共存时极易分解。 [0004] L- tryptophan white or slightly yellow crystal or crystalline powder; odorless or slight odor, slightly bitter, 289 ° C decomposition, slightly soluble in water, insoluble in ethanol; dilute acid or dilute alkali dissolved, the long light colored, with small amounts of aqueous co-indol-heat generating, such as heating in the presence of sodium hydroxide, copper sulfate, a large amount of the indole with an acid called heat stable in the dark, with other amino acids, sugars , aldehyde coexist easily break.

[0005] 色氨酸是人和动物维持生长的必需氨基酸之一,天然来源色氨酸通常是谷物类饲料的第二或第三限制性氨基酸,尤其在以高梁和玉米为基础的饲料中显得更为明显。 [0005] Tryptophan is one of the essential amino acids to maintain the growth of human and animal, natural sources of tryptophan are usually the second or third limiting amino acid feed grains, is especially the sorghum and corn-based diet more obvious. 色氨酸作为具有多种生理功能的氨基酸,受到了广泛的关注。 Tryptophan as amino acids with a variety of physiological functions, has received extensive attention. 研究作为医药的高品质色氨酸产品有重要意义。 As a study of high-quality pharmaceutical products tryptophan is important.

[0006]目前色氨酸纯化技术主要采用树脂法,进行离子交换提纯。 [0006] Tryptophan purification techniques currently used mainly resin method, ion exchange purification. 使用树脂会产生大量含酸碱废液,造成环保压力,也增加了生产成本。 A resin containing a large amount of acid waste would cause environmental pressures, but also increases the production cost. 有少数溶解提取的也需经活性炭活化、浓缩结晶等繁琐步骤生产。 A few also subject to dissolution extracted activated charcoal, and concentrated crystallization cumbersome production step.

[0007]日本专利说明书JP895/1983采用色氨酸溶液先通过非极性多孔树脂,再经过超滤的方法提纯色氨酸,但杂质去除不理想,达不到高透光率要求。 [0007] Japanese Patent Specification JP895 / 1983 by using tryptophan solution to a nonpolar porous resin, and then through an ultrafiltration process purifying tryptophan, but not over the impurity removal, reach high transmittance requirements. 专利说明书JP39857/1984提出色氨酸用碱液溶解,在低级脂肪醇或酮存在下中和结晶,提高纯度,但杂质去除仍不充分,透光率很难达到95%,而且,使用大量溶剂,需回收和后处理。 Patent Specification No. JP39857 / 1984 proposes the tryptophan dissolved with lye, and the crystallization in a lower aliphatic alcohol or ketone present, increasing the purity, but still insufficient removal of impurities, is difficult to achieve a light transmittance of 95%, and using large amounts of solvent , and post-processing to be recovered. JP126070/1986将色氨酸溶解在95-100°C的酸性水溶液中,用活性炭吸附,滤炭后经非极性多孔树脂吸附,洗脱色氨酸,在低级脂肪醇存在下中和结晶。 JP126070 / 1986 was dissolved in an acidic aqueous solution of tryptophan 95-100 ° C, the activated carbon adsorption, carbon adsorption was filtered off through a nonpolar porous resin, eluting tryptophan, and the lower aliphatic alcohol in the presence of crystallization. 因其使用温度较高,吲哚环不稳定产生有色物质,致使透光率不理想。 Because the use of higher temperatures, indole ring to produce a colored substance unstable, resulting in light transmittance is not ideal.

[0008] 美国专利说明书US5057615重点研究了仅用醋酸对色氨酸的溶解情况。 [0008] U.S. Patent specification US5057615 focused on the dissolution of the only acetic acid tryptophan. 提出其重结晶过程可在醋酸溶液中降温,收率89%,含量98.9%,未提及透光率。 Proposed process may be recrystallized in acetic acid solution to cool, yield 89%, content 98.9%, the light transmittance is not mentioned. 美国专利说明书US4820825将粗品色氨酸溶解后,用经酸活化的活性炭3% -25%吸附,再经过非极性多孔树脂,最后得到成品透光率90 %,达不到透光率95 %的要求。 U.S. Patent specification US4820825 crude tryptophan dissolved, acid-activated charcoal with 3% -25% adsorbed, and then through a nonpolar porous resin, and finally be finished light transmittance of 90%, the light transmittance of less than 95% requirements. US5776740介绍了化学法合成L-色氨酸的方法;US5756345是大肠杆菌发酵法,US 5624828和US 5605818也都是细菌发酵法,简单阐述了粗提取方法。 US5776740 describes a method of chemical synthesis of L- tryptophan; US5756345 E. coli fermentation, US 5624828 and US 5605818 are also bacterial fermentation process, briefly discusses the crude extraction methods.

[0009] 国内专利说明书在精制高品质色氨酸方面少有提及,ZL200710068130.9公布了从发酵到浓缩的提取过程,ZL97113051.5是从发酵液直接喷干制粒作添加剂的方法,ZL96197716是日本味之素关于发酵菌种制备的专利。 [0009] Domestic Patent Specification mentioned in the refined high-quality rare tryptophan aspect, ZL200710068130.9 released to the concentrated extract from the fermentation process, ZL97113051.5 granulation is spray dried directly from a fermentation broth as an additive to, ZL96197716 Ajinomoto is the patent for the preparation of the seed fermentation. 专利说明书ZL200810065762.4是将色氨酸溶液用活化后的活性炭吸附,过滤后分步浓缩结晶,可得到透光率高于95%的产品。 Patent specification ZL200810065762.4 activated carbon adsorption is the tryptophan solution with activated, fractional crystallization was filtered and concentrated, to obtain a high transmittance of 95% product. 但该法步骤繁琐,不仅活性炭需多步处理,还要分几次进行浓缩结晶,极不便于工业化生产。 However, the process step complicated, multi-step treatment for an activated carbon only, but also crystallization was concentrated several times, not very convenient for industrial production. 而且其对粗品含量要求在95%以上,降低了提取纯化技术的适用范围。 The crude product and its contents more than 95% required, reducing the scope of extraction and purification techniques.

发明内容 SUMMARY

[0010] 本发明的目的是提供一种简便高效制备高透光率色氨酸的方法,此法获得的色氨酸产品符合2010版药典中药用级标准规定的透光率95%等各项指标。 [0010] The object of the present invention is to provide a simple method for high transmittance efficient preparation of tryptophan, tryptophan product obtained by this method meet the predetermined transmittance Chinese Pharmacopoeia 2010 edition standard level of 95% with the other index.

[0011] 为达到目的,本发明采用了如下技术方案: [0011] To achieve the object, the present invention employs the following technical solutions:

[0012] 一种高透光率色氨酸的制备方法,包括以下步骤: [0012] A method for producing a high transmittance tryptophan, comprising the steps of:

[0013] 步骤一、将粗品色氨酸加入混合溶解液中,加热使其全部溶解,加入活性炭吸附半小时后,过滤除去活性炭,再用滤膜进行膜过滤,其中混合溶解液为纯化水、低级脂肪醇或低级脂肪酮和低级脂肪酸的混合液; [0013] Step a, the crude tryptophan mixed and dissolved solution was added, followed by heating completely dissolved, adding activated carbon adsorption and a half hours, the activated carbon was removed by filtration, membrane filtration and then filter, wherein the fluid is mixed and dissolved in purified water, a lower aliphatic alcohol or lower aliphatic ketone, and a mixture of lower fatty acids;

[0014] 步骤二、将滤液在搅拌下缓慢结晶,并使用物理方法进一步降温使其充分结晶; [0014] Step two, and the filtrate was slowly crystallized under stirring, and the physical means further sufficiently cooling crystallization;

[0015] 步骤三、将结晶液过滤得到的白色晶体经充分洗涤,调节PH值后再次过滤,干燥得纯品; [0015] Step three, the crystal was filtered to give white crystals were washed well, after adjusting the PH value again filtered, and dried to give pure product;

[0016] 其中,母液能循环利用。 [0016] wherein the mother liquor can be recycled.

[0017] 作为优选,步骤一中所述的粗品色氨酸为固体或液体状态,经由发酵或合成过程得到,其中不含发酵菌丝体,含量在30重量% -100重量%。 [0017] Advantageously, step a crude tryptophan in the solid or liquid state, obtained via fermentation or synthesis, wherein the mycelium-free fermentation, the content of 30 wt% to 100 wt%.

[0018] 更进一步,步骤一中所述的粗品色氨酸的用量为可形成重量浓度为30-75克/升的澄清溶液。 [0018] Still further, the amount of the crude product of tryptophan in a step to be formed according to a concentration of 30 to 75 wt. G / l clear solution.

[0019] 更进一步,步骤一中混合溶解液用量的比例为,低级脂肪醇或低级脂肪酮:低级脂肪酸=2-7: I ;低级脂肪醇或低级脂肪酮:水=0.5-5: I。 [0019] Still further, the step of mixing a proportion of an amount of the dissolving liquid, lower aliphatic ketone or a lower aliphatic alcohol: lower fatty acid = 2-7: I; lower aliphatic alcohol or lower aliphatic ketone: water = 0.5-5: I.

[0020] 更进一步,步骤一中所述低级脂肪醇或低级脂肪酮为乙醇、异丙醇或丙酮;低级脂肪酸为甲酸、乙酸或丙酸。 [0020] Still further, in the step of a lower aliphatic ketone or a lower aliphatic alcohol is ethanol, isopropanol or acetone; lower fatty acid is formic acid, acetic acid or propionic acid.

[0021] 更进一步,步骤一中混合溶解液所加入试剂可先行混合,也可分别加入,且无先后顺序要求,可根据实际设备情况安排。 [0021] Still further, the step of mixing a lysate reagent may be added to the first mixture, can be added, respectively, and no required order, the device can be arranged according to the actual situation.

[0022] 更进一步,步骤一中所述加热溶解温度为30_70°C,使粗品溶解且不破坏色氨酸组分。 [0022] Still further, in the step of heating a solution temperature of 30_70 ° C, the crude product was dissolved component does not destroy tryptophan.

[0023] 更进一步,步骤一中所加活性炭为普通工业生产用活性炭,且不用做任何前期处理,根据粗品色氨酸含量不同,用量为所加粗品重量的I重量% -10重量%。 [0023] Still further, a step of added activated charcoal for general industrial use, and do not have any pre-processing, the crude tryptophan content depending on an amount of the thickening article I wt% to 10 wt% by weight.

[0024] 更进一步,步骤二中所述结晶过程时间在2-5小时,进一步降温的最终温度降至-10°C -10°c。 [0024] Still further, in the two step crystallization process time is 2-5 hours, further cooling down to a final temperature of -10 ° C -10 ° c.

[0025] 更进一步,步骤三中所述充分洗涤包含水洗和混合溶液洗步骤。 [0025] Still further, the three step comprising washing with water and sufficiently washed with a mixed solution wash step.

[0026] 更进一步,步骤三中所述混合溶液为低级脂肪醇或低级脂肪酮和水的混合溶液,混合比例为0.1-3.5: I。 [0026] Still further, in step three of the mixed solution is a mixed solution of a lower aliphatic alcohol or lower aliphatic ketone and water, mixing ratio of 0.1-3.5: I.

[0027] 更进一步,步骤三中所述调节PH值是指以呈碱性物质将PH值调至5-8。 [0027] Still further, the step of adjusting the PH value of the three refers to the alkaline substance PH value was adjusted to 5-8.

[0028] 更进一步,所述呈碱性物质为氢氧化钠或氨水。 [0028] Still further, the alkaline substance is sodium hydroxide or aqueous ammonia.

[0029] 更进一步,步骤三中所述干燥过程是指将湿品放入鼓风干燥箱或真空干燥箱,或混浆用喷干塔进行干燥。 [0029] Furthermore, the drying process of step 3 refers to the wet product into the drying oven or a vacuum drying oven, or mixing the slurry with a spray drying tower and dried.

[0030] 更进一步,所述循环利用是指将母液蒸馏得到的水与醇或酮的混合溶液,测出其中醇或酮浓度,在下一批次纯化时重复利用。 [0030] Still further, the recycling means a mixed solution of water and an alcohol or ketone mother liquor obtained by distillation, wherein the measured concentration of alcohol or ketone, at the next re-use batch purification. [0031] 一种高透光率色氨酸的制备方法,其特征在于,包括以下步骤: [0031] The method for producing a high transmittance of tryptophan, characterized by comprising the steps of:

[0032] 步骤一:粗品色氨酸加入水和低级脂肪醇或低级脂肪酮的混合溶解液中,加入醋酸,加热至30°C以上使其全部溶解,形成浓度为30-75克/升的溶液,按色氨酸重量的I重量% -10重量%加入活性炭,在保温状态下搅拌吸附半小时后,过滤除去活性炭,再用微孔滤膜进行膜过滤; [0032] Step a: dissolving crude tryptophan mixed solution was added water and lower aliphatic alcohol or lower aliphatic ketone, acetic acid was added, heated to above 30 ° C it has completely dissolved, a concentration of 30 to 75 g / l solution, tryptophan by weight I% to 10% by weight of activated carbon was added, stirred for half an hour adsorption, the activated carbon was removed by filtration in the insulating state, and then membrane filtration microporous membrane;

[0033] 步骤二:滤液在搅拌下缓慢降温结晶,并使用水浴、冰浴进一步降温至_5°C -1O0C左右,使其充分结晶,降温过程在2小时以上; [0033] Step two: the crystallization filtrate slowly cooled with stirring, and using a water bath, an ice bath was further cooled to about _5 ° C -1O0C, sufficiently crystallized in the cooling process more than 2 hours;

[0034] 步骤三:结晶液过滤得到的白色晶体,分别以纯化水、混合溶液充分洗涤,氨水调节PH值至4-9后再次过滤抽干,放入真空干燥箱,30°C -90°C干燥3小时得纯品,其中混合溶液为低级脂肪醇或低级脂肪酮和水的混合溶液,混合比例为0.1-3.5: I ; [0034] Step Three: crystal was filtered to give white crystals, respectively, purified water, sufficiently washed with a mixed solution of ammonia to adjust PH value to 4-9 after drained again filtered, placed in a vacuum oven, 30 ° C -90 ° C for 3 hours to obtain pure product, wherein the mixed solution is a mixed solution of a lower aliphatic alcohol or lower aliphatic ketone and water, mixing ratio of 0.1-3.5: I;

[0035] 步骤四:母液经蒸馏得到低级脂肪醇或低级脂肪酮与水的混合溶液,测出其中低级脂肪醇或低级脂肪酮浓度,循环利用。 [0035] Step Four: the mother liquor was distilled to give a mixed solution of a lower aliphatic ketone or a lower aliphatic alcohol and water, wherein the measured lower aliphatic ketone or a lower aliphatic alcohol concentration and recycling.

[0036] 本发明所使用溶媒单一,不需单独回收,可将母液简单处理后重复使用,不造成任何三废污染;所用活性炭无需活化,市面即可买到,节省成本及时间;没有浓缩步骤,降低了对动力系统的要求,很容易实现工业化生产。 [0036] The present invention is the use of a single vehicle, without separately recovered, the mother liquor may simply be reused after treatment, does not cause any waste pollution; used without activated charcoal, can be commercially available, cost and time; step is not concentrated, reducing the requirements for the power system, it is easy to realize industrial production.

具体实施方式 Detailed ways

[0037] 实施例一: [0037] Example a:

[0038] 含量95%、透光率38%的色氨酸粗品50g,加入异丙醇280ml,甲酸50ml,水503.33ml,加热至50°C使其全部溶解,形成浓度为60g/L的溶液,加入2.5g活性炭,在保温状态下搅拌吸附半小时后,过滤除去活性炭,再用0.5 μ m微孔滤膜进行膜过滤; [0038] content of 95%, a light transmittance of 38% crude tryptophan 50g, was added 280 ml of isopropanol, formic 50ml, water 503.33ml, heated to 50 ° C it has completely dissolved, a concentration of 60g / L solution of after addition of 2.5g of activated carbon, stirred for a half hour incubated adsorbed state, activated carbon was removed by filtration, and then 0.5 μ m millipore membrane filtration;

[0039] 滤液在搅拌下缓慢降温结晶,并进一步降温至0°C左右,使其充分结晶,降温过程总计三小时; [0039] The filtrate was stirred under slow cooling crystallization and further cooled to about 0 ° C, crystallization sufficiently, the cooling process a total of three hours;

[0040] 结晶液过滤得到的白色晶体,经充分洗涤、调节PH值后再次过滤抽干,放入真空干燥箱,干燥3小时得纯品。 [0040] The crystallization solution was filtered to give white crystals, sufficiently washed, after adjusting the PH value drained again filtered, placed in a vacuum oven, dried for 3 hours to obtain pure product. 收率78 %,色氨酸含量99 %、透光率97 %,其他指标合格。 Yield 78%, tryptophan content of 99%, a light transmittance of 97%, other indicators qualified.

[0041] 实施例二: [0041] Example II:

[0042] 含量89 %、透光率32 %的色氨酸粗品50g,加入丙醇350ml,醋酸200ml,水219.23ml,加热至70°C使其全部溶解,形成浓度为65g/L的溶液,加入3g活性炭,在保温状态下搅拌吸附半小时后,过滤除去活性炭,再用0.5 μ m微孔滤膜进行膜过滤; [0042] content of 89%, light transmittance of 32% crude tryptophan 50g, propanol added 350ml, 200ml of acetic acid, water 219.23ml, heated to 70 ° C it has completely dissolved, a concentration of 65g / L of solution, after addition of 3g of activated carbon and stirred under a state incubated for half an hour adsorption, the activated carbon was removed by filtration, and then 0.5 μ m millipore membrane filtration;

[0043] 滤液在搅拌下缓慢降温结晶,并使用水域、冰域进一步降温至5°C左右,使其充分结晶,降温过程总计三小时; [0043] The filtrate was stirred under slow cooling crystallization, and use of water, further cooled to about ice-domain 5 ° C, crystallization sufficiently, the cooling process a total of three hours;

[0044] 结晶液过滤得到的白色晶体,经充分洗涤、氨水调节PH值后再次过滤抽干,放入真空干燥箱,干燥3小时得纯品。 [0044] The crystallization solution was filtered to give white crystals, sufficiently washed, after adjusting the PH value of aqueous ammonia and filtered again drained, placed in a vacuum oven, dried for 3 hours to obtain pure product. 收率71 %,色氨酸含量98 %、透光率95 %,其他指标合格。 71% yield, tryptophan content of 98%, a light transmittance of 95%, other indicators qualified.

[0045] 实施例三: [0045] Example III:

[0046] 含量98 %、透光率39 %的色氨酸粗品50g,加入丙酮100ml,丙酸50ml,水961.11ml,加热至50°C使其全部溶解,形成浓度为45g/L的溶液,加入2g活性炭,在保温状态下搅拌吸附半小时后,过滤除去活性炭,再用0.5 μ m微孔滤膜进行膜过滤; [0046] content of 98%, light transmittance of 39% crude tryptophan 50g, acetone was added 100ml, propionic acid 50ml, water 961.11ml, heated to 50 ° C it has completely dissolved, a concentration of 45g / L of solution, after addition of charcoal 2g, stirred at state incubated for half an hour adsorption, the activated carbon was removed by filtration, and then 0.5 μ m millipore membrane filtration;

[0047] 滤液在搅拌下缓慢降温结晶,并使用水域、冰域进一步降温至0°C左右,使其充分结晶,降温过程总计三小时;[0048] 结晶液过滤得到的白色晶体,经充分洗涤、氨水调节PH值后再次过滤抽干,放入真空干燥箱,干燥3小时得纯品。 [0047] The filtrate was stirred under slow cooling crystallization, and use of water, further cooled to about ice field 0 ° C, crystallization sufficiently, a total of three hours the cooling process; [0048] The crystallization solution was filtered to give white crystals, was thoroughly washed after adjusting the PH value of ammonia and filtered again drained, placed in a vacuum oven, dried for 3 hours to obtain pure product. 收率82 %,色氨酸含量99 %、透光率95 %,其他指标合格。 82% yield, tryptophan content of 99%, 95% light transmission rate, other indicators qualified.

[0049] 实施例四: [0049] Example IV:

[0050] 本实施例用于说明循环利用的母液。 [0050] The present examples serve to illustrate the mother liquor recycling. 母液800ml在50°C,真空_0.1MPa旋转蒸发浓缩,蒸出650ml丙酮和水的混合溶液,检查丙酮浓度28%。 The mother liquor 800ml at 50 ° C, concentrated by rotary evaporation in vacuo _0.1MPa, a mixed solution of distilled water and 650ml of acetone, 28% acetone concentration check. 浓后母液出现结晶,过滤干燥后作为粗品使用。 The mother liquor after the crystallization concentration, the crude product was filtered and dried as.

Claims (8)

1.一种高透光率色氨酸的制备方法,其特征在于,包括以下步骤: 步骤一、将粗品色氨酸加入混合溶解液中,加热使其全部溶解,加入活性炭吸附半小时后,过滤除去活性炭,再用滤膜进行膜过滤,其中混合溶解液为纯化水、低级脂肪醇或低级脂肪酮和低级脂肪酸的混合液; 步骤二、将滤液在搅拌下缓慢结晶,并使用物理方法进一步降温使其充分结晶; 步骤三、将结晶液过滤得到的白色晶体经充分洗涤,调节PH值后再次过滤,干燥得纯品; 其中,母液能循环利用; 步骤一中所述的粗品色氨酸为固体或液体状态,经由发酵或合成过程得到,其中不含发酵菌丝体,含量在30重量% -100重量% ;其用量为能形成重量浓度为30-75克/升的澄清溶液;混合溶解液用量的比例为,低级脂肪醇或低级脂肪酮:低级脂肪酸=2-7: I ;低级脂肪醇或低级脂肪酮:水=0.5-5: I ;所述 1. A process for producing high transmittance of tryptophan, characterized in that it comprises the following steps: Step one, the crude mixture was added the tryptophan dissolved solution, heated to dissolve all, half an hour after adding activated carbon adsorption, activated carbon was removed by filtration, and then membrane filtration membrane, wherein the fluid is mixed and dissolved in purified water, a mixture of lower aliphatic alcohols and lower aliphatic ketones or a lower fatty acid; step two, and the filtrate was slowly crystallized under stirring, and further the use of physical methods sufficiently cooling crystallization; step three, the crystal was filtered to give white crystals were washed sufficiently, adjusting the PH value again filtered, and dried to give the pure product; wherein the mother liquor can be recycled; a step in the crude tryptophan a solid or liquid state, obtained via fermentation or synthesis, wherein the mycelium-free fermentation, the content of 30 wt% to 100 wt%; an amount capable of forming a concentration of 30 to 75 wt. g / l clear solution; mixing the proportion of an amount of the dissolving liquid, lower aliphatic ketone or a lower aliphatic alcohol: lower fatty acid = 2-7: I; lower aliphatic alcohol or lower aliphatic ketone: water = 0.5-5: I; the 低级脂肪醇或低级脂肪酮为乙醇、异丙醇或丙酮;低级脂肪酸为甲酸、乙酸或丙酸;混合溶解液所加入试剂可先行混合,也可分别加入,且无先后顺序要求,可根据实际设备情况安排;所述加热溶解温度为30-70°C,使粗品溶解且不破坏色氨酸组分; 步骤二中所述结晶过程时间在2-5小时,进一步降温的最终温度降至-10°C -10°C。 Lower aliphatic ketone or a lower aliphatic alcohol is ethanol, isopropanol or acetone; lower fatty acid is formic acid, acetic acid or propionic acid; mixed and dissolved was added to the first mixing agent may also be added separately, and no required order, according to the actual equipment cases arrangements; heating said solution temperature of 30-70 ° C, the crude product was dissolved without impairing tryptophan component; the two step crystallization process time is 2-5 hours, further cooling down to a final temperature - 10 ° C -10 ° C.
2.根据权利要求1所述的色氨酸的制备方法,其特征在于:步骤一中所加活性炭为普通工业生产用活性炭,且不用做任何前期处理,根据粗品色氨酸含量不同,用量为所加粗品重量的I重量% -10重量%。 2. Preparation method of claim tryptophan, wherein: the step of adding the activated carbon as a general industrial production of activated carbon, do not have any pre-processing and, depending on the content of the crude product of tryptophan, the amount of the thickened product I wt% to 10 wt% by weight.
3.根据权利要求1所述的色氨酸的制备方法,其特征在于:步骤三中所述充分洗涤包含水洗和混合溶液洗步骤,其中所述混合溶液为低级脂肪醇或低级脂肪酮和水的混合溶液,混合比例为0.1-3.5: I。 The production method according to claim 1 tryptophan, wherein: the three step comprising washing with water and sufficiently washed with a mixed solution wash step, wherein the mixed solution is a lower aliphatic alcohol or lower aliphatic ketone and water the solution was mixed, the mixing ratio of 0.1-3.5: I.
4.根据权利要求1所述的色氨酸的制备方法,其特征在于:步骤三中所述调节PH值是指以呈碱性物质将PH值调至5-8。 The production method according to claim 1 of tryptophan, characterized in that: in the step of adjusting the PH value of the three refers to the alkaline substance PH value was adjusted to 5-8.
5.根据权利要求4所述的色氨酸的制备方法,其特征在于:所述呈碱性物质为氢氧化钠或氨水。 The preparation method according to claim tryptophan, wherein: said alkaline substance is sodium hydroxide or aqueous ammonia.
6.根据权利要求1所述的色氨酸的制备方法,其特征在于:步骤三中所述干燥过程是指将湿品放入鼓风干燥箱或真空干燥箱,或混浆用喷干塔进行干燥。 6. The production method according to claim 1 tryptophan, wherein: step 3 refers to the drying process of wet product into the drying oven or a vacuum drying oven, or by spray drying tower Mixing drying.
7.根据权利要求1所述的色氨酸的制备方法,其特征在于:所述循环利用是指将母液蒸馏得到的水与醇或酮的混合溶液,测出其中醇或酮浓度,在下一批次纯化时重复利用。 7. The production method according to claim 1 of tryptophan, characterized in that: said means to recycle the mother liquor distilled water and a mixed solution of an alcohol or a ketone, alcohol or ketone wherein the measured concentration, in the next when a batch purification reuse.
8.一种高透光率色氨酸的制备方法,其特征在于,包括以下步骤: 步骤一:粗品色氨酸加入水和低级脂肪醇或低级脂肪酮的混合溶解液中,加入醋酸,加热至30°C以上使其全部溶解,形成浓度为30-75克/升的溶液,按色氨酸重量的I重量% -10重量%加入活性炭,在保温状态下搅拌吸附半小时后,过滤除去活性炭,再用微孔滤膜进行膜过滤; 步骤二:滤液在搅拌下缓慢降温结晶,并使用水浴、冰浴进一步降温至_5°C -10°C左右,使其充分结晶,降温过程在2小时以上; 步骤三:结晶液过滤得到的白色晶体,分别以纯化水、混合溶液充分洗涤,氨水调节pH值至4-9后再次过滤抽干,放入真空干燥箱,300C _90°C干燥3小时得纯品,其中混合溶液为低级脂肪醇或低级脂肪酮和水的混合溶液,混合比例为01-3.5: I ; 步骤四:母液经蒸馏得到低级脂肪醇或低级脂肪酮与水的混合溶 8. A method for preparing a high transmittance of tryptophan, characterized in that it comprises the following steps: Step 1: The crude product mixture was added water and lower aliphatic alcohol tryptophan or a lower aliphatic ketone dissolved solution, acetic acid was added, heating above 30 ° C to make it completely dissolved, a concentration of 30 to 75 g / l solution, by weight tryptophan I wt% to 10 wt% activated carbon was added, stirred for half an hour after adsorption at the insulating state, removed by filtration activated carbon, and then millipore membrane filtration; step two: the crystallization filtrate slowly cooled with stirring, and using a water bath, an ice bath was further cooled to about _5 ° C -10 ° C, sufficiently crystallized in the cooling process more than 2 hours; step three: the crystal was filtered to give white crystals, respectively, purified water, sufficiently washed with a mixed solution of ammonia to adjust the pH to 4-9 drained again filtered, placed in a vacuum drying oven, 300C _90 ° C and dried 3 hours to give a mixed solution of pure product, wherein a mixed solution of a lower aliphatic alcohol or lower aliphatic ketone and water, mixing ratio of 01-3.5: I; step four: the mother liquor was distilled to give the mixed lower aliphatic ketone or a lower aliphatic alcohol and water dissolve 液,测出其中低级脂肪醇或低级脂肪酮浓度,循环利用`。 Liquid, wherein a lower aliphatic alcohol or measured lower aliphatic ketone concentration, `recycling.
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