CN102219705B - Crystallization process of columnar crystal of L-serine and application of columnar crystal - Google Patents
Crystallization process of columnar crystal of L-serine and application of columnar crystal Download PDFInfo
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Abstract
The invention belongs to the technical field of medical biology and in particular relates to a crystallization process of columnar crystal of L-serine and application of the columnar crystal. According to the invention, a cooling crystallization process and a dissolving-out crystallization process of amino acid are combined so as to form a novel crystallization process, and the novel crystallization process is used for the production of the columnar crystal of L-serine. The process comprises the following steps: based on crude L-serine utilized as a raw material, dissolving and decoloring crude L-serine, and then cultivating the dissolved and decolored crude L-serine in a water phase system at the temperature of 30-50 DEG C so as to form the crystal nucleus and minicrystal of the columnar crystal of L-serine; and controlling the concentration of methanol or ethanol at 10-50%, and stirring in a water-organic solvent phase system for growth so as to obtain the columnar crystal of L-serine. Detected by quality standard (2002 version) of Ajinomoto joint-stock company, the product content and transmissivity of the columnar crystal of L-serine are not less than 99.0%. In the process, only temperature, alcohol concentration and stirring speed need to be controlled, thereby being beneficial to the stabilities of the production process and product quality; and simultaneously, the process has the advantages that the operation is convenient, no special equipment is not required, and the like; and the process is easy for industrial popularization and application.
Description
Technical field
The invention belongs to the medical biotechnology field, be specifically related to the crystallization processes and the purposes of L-Serine column crystallization body.
Background technology
Germanization scholar Cramer isolated a kind of sweetish crystal first from the sericin hydrolyzed solution in 1865, so originate this crystallization called after Serine (Serine) according to it.It is pantonine-hydroxy-propionic acid (α-amino-β-hydroxy propionic acid) that another Germanization scholar Erlenmeyer in 1880 infers the chemical structure of this compound.People such as German Pa Lin famous chemist Fischer of university in 1902 and Leuchs have verified this structural formula, and determine its molecular structure.Fischer in 1907 finds that the Serine in the natural protein is a kind of optically active material that has, and its optical activity is the L-type, so the Serine in the protein is commonly referred to as the L-Serine.
The L-Serine in vivo can be synthetic through three-step reaction by glycometabolic intermediate product 3-phoshoglyceric acid, so be called non-essential amino acid.Simultaneously, the L-Serine generates pyruvic acid through dehydration, dehydrogenation, so be a kind of glycogenic amino acid by the effect of body endoenzyme in vivo.The L-Serine has many important physical functions, is the precursor of purine biosynthesis, thymus pyrimidine, choline etc. in vivo, has been widely used in medicine, makeup, chemical industry and scientific research.At field of medicaments, the L-Serine is the important component of amino acid nutrient transfusion, being synthetic L-DOPA, microbiotic---the intermediate of products such as Ramipril, is the raw material that sets out of synthetic anticancer, anti-AIDS new drug and multiple medicine such as azaserine, seromycin, phosphatidylserine, alpha-substitution Serine and (s)-isoserine etc.At cosmetic field, the L-Serine is important natural Moisture factor, is applied to makeup and can plays increase epidermic cell vigor, delaying decrepitude of skin, also having effect antibiotic, that improve skin elasticity and nutrient-reinforced simultaneously, is the essential additive of superior cosmetics therefore.
The production method of L-Serine has four kinds of proteins extraction method, chemical synthesis, microbe fermentation method and enzyme transforming process.The proteins extraction method is to be raw material with protein such as silk gum, fibroin, useless silks, extracts preparation L-Serine through acid hydrolysis, resin isolation, crystallization.Last century, China mainly adopted this method to produce; Chemical synthesis is to be the raw material that sets out with vinyl cyanide or methyl acrylate or glycine etc., makes DL-serine through the multistep chemical reaction, splits preparation L-Serine again.Japan adopts vinyl cyanide to be the raw material production of setting out; Microbe fermentation method is to serve as to produce bacterial strain with the bacterial strain with high vigor serine transhydroxymethylase, and glycine is a precursor, through fermentation glycine is converted into the L-Serine; Enzyme transforming process is to be raw material with glycine and formaldehyde, in the presence of cofactor 5-pyridoxal phosphate (PLP) and tetrahydrofolic acid (THFA) (THFA), prepares the L-Serine through Serine hydroxymethyl transferases (SHMT) enzymatic reaction.Microbe fermentation method and enzyme transforming process are at home and abroad used at present.
Though the L-Serine has four kinds of production methods, all need adopt the crystallization processes refined product at last, could obtain L-Serine product, realize economic worth.The crystallization processes that is used for amino acid production at present mainly contains four kinds of crystallisation by cooling, dilution crystallization, evaporative crystallization and iso-electric point reactive crystallizations.
1, crystallisation by cooling is a character of utilizing amino acid different solubility under differing temps, adopts cooling method to change solution system Jie stable region, and amino acid is separated out from solution.Usually take solution concentration to be crystallized to change crystallization then over to finite concentration
With temperature reduction way progressively, amino acid is separated out from solution in jar.The solution system of this technology is a water, so products obtained therefrom is a crystal of hydrate, xln is an oblique crystal.A lot of amino acid such as L-Valerian propylhomoserin, L lysine HCL, L-Isoleucine etc. adopt this crystallization processes.
2, dilution crystallization is to utilize organic solvent can change Jie stable region of system rapidly, influences the solubleness of amino acid in system, and amino acid is separated out from solution.The solution system of this technology be water-organic solvent mutually or organic solvent-water, so products obtained therefrom based on the anhydride crystallization, xln is generally iris or prismatic crystal.Some are difficult for crystallization or the big amino acid of water solubility adopts this crystallization processes more at aqueous phase system, as L-Histidine, L-proline(Pro) etc.But the organic solvent amount that adds system is big more, and the organic solvent residual probability is high more.
3, evaporative crystallization is to adopt reduction vaporization moisture mode, under comparatively high temps with solution concentration to be crystallized to the supersolubility state, progressively cooling is separated out amino acid from solution again.The solution system of this technology is a water, and after the amino acid solution that is in the supersolubility state was put into crystallizer, temperature descended and causes mass crystallization to be separated out rapidly, so the gained crystallization is the mixture of hydrate and anhydride.The amino acid salts that some water solubilities are very big such as L-arginine acid hydrochloride, L-cysteine hydrochloride etc. adopt this crystallization processes.This crystallization processes is bigger than other technological equipment investment, energy consumption is high.
4, the iso-electric point reactive crystallization is to adopt to add the pH value that alkali is regulated amino acid solution, makes the amino acid crystallization processes that crystallization is separated out under its specific iso-electric point.The solution system of this technology is a water, the crystalline crystal formation with add alkali lye speed, stirring velocity has substantial connection.Be mainly used in the crystallization of water-soluble very low amino acid such as L-Gelucystine, L-tyrosine.
Amino acid whose crystal formation not only is directly connected to the quality of amino acid product itself, and influences the quality of derived product, also increases the production cost of derived product.2002, (chemical industry progress such as Han Jinyu, 2002,21(12): 945-948) in introducing " newtype drug crystallization technique " literary composition, quoted from Shekunov and York about the crystallization crystal formation to the research of drug influence and point out: degree of crystallinity (existence of indefinite form or hypocrystalline form) influences the physical and chemical stability of medicine, polymorphic, lattice imperfections etc. influence the solubility curve and the dissolution rate of medicine, the big medicine processing performance that influences of particle size distribution, grain surface texture influences the stability and the homogeneity of medicament, and is organic, inorganic impurity and residual solvent etc. are brought toxicity into to medicine.Domestic certain pharmaceutical factory is with homemade mealy crystal and granule shape prismatic crystal L-Serine products production L-serine derivative, with column crystallization body L-Serine contrast with Japanese import, the raw material consumption amount increases by 4.8% and 3.8% respectively, and the L-serine derivative of producing with column crystallization body L-Serine balling not, with the then balling of mealy crystal.
In order to obtain amino acid whose good crystal formation, many investigators have launched correlative study.1999, (Nanjing University of Chemical Technology's journal such as Wu Yue, 1999,21(3): 27-31) adopt adding 2% crystal seed, at the uniform velocity drip sulfuric acid, intermittently the cooling operation mode, with isoelectric precipitation crystallization processes and crystallisation by cooling prepared L-aspartic acid, the crystal crystalline form that obtains the L-aspartic acid is complete, and particle size dispersion is even, good dispersity.Calendar year 2001, (Qiqihar University's journal such as Yu Shujuan, 2001,17(3): 5-8) adopt the collaborative graining legal system of magnetic field-solvent to get α type glutamic acid crystal crystal seed, extract the technology of L-L-glutamic acid to add the crystal seed iso-electric point then, the crystal outward appearance that obtains, color and brilliant the habit all have bigger improvement, and the L-L-glutamic acid product that crystalline purity also improves a lot has improved about 5% than industrial crystallization processes crystallization yield commonly used.2008, (China Mining University's journal such as Meng Xianliang, 2008,37(3): 412-415) adopt orthogonal test that water and L-phenylalanine mass ratio, crystallizing system, three of Tcs are influenced L-phenylalanine crystalline factor and carry out process optimization, the mass ratio of having determined water and L-phenylalanine is 1:3, with hydrochloric acid-triethylamine/DMF is crystallizing system, 25 ℃ of crystallization initial temperatures, mid-term, temperature was 55 ℃, the optimization technology that finishing temperature is 15 ℃, make L-phenylalanine grain size number and be evenly distributed, crystal face is complete, and yield reaches more than 85 %.2008, (chemical industry and engineering such as Li Xia, 2008,25(2): 129-133) adopt laser method to measure the solubleness of L-Serine in water and show that the crystal conversion temperature of anhydrous synthetic body of L-Serine and hydrate crystal is 309.14 K, in the concurrent present aqueous phase system crystallisation by cooling process, the L-Serine mainly forms anhydrous synthetic body by intermolecular hydrogen bond action under the hot conditions, but be cooled to the crystal conversion temperature when following, then mainly by the hydrogen bond action formation hydrate crystal (hydrate crystal of hexagonal plate) of L-Serine with water molecules.
The L-Serine is water-soluble very big amino acid, and the solubleness in 100g water is 25.4g (10 ℃), 72.0g (50 ℃), and therefore above-mentioned first three planted crystallization processes and all can be adopted.Domestic manufacturer produces the L-Serine and mainly adopts crystallisation by cooling or these two kinds of crystallization processes of dilution crystallization.The molecular structure of L-Serine has determined that the binding ability of it and water molecules is extremely strong, if adopt crystallisation by cooling technology, grow up at crystal that the L-Serine easily forms hydration nucleus and hydration crystallite in the process, and the crystallite growth process is slower, therefore be easy to make the impurity in the solution to be embedded in the xln, at crystallizing and drying operation moisture evaporation subsequently, crystalline hydrate is broken into the powdery crystalline substance, impurity then remains in the product, so adopting the L-Serine crystallization of crystallisation by cooling technology is indefinite form or hypocrystalline form, purity is lower.Adopt dilution crystallization technology, organic solvent has changed the polarity of solution system, and the probability that makes L-Serine crystal grow up to bound water molecule in the process reduces, thereby can obtain the particulate state prismatic crystal.But, the nucleus of this technology is to form after adding organic solvent, crystal grows up to process and is difficult to avoid organic solvent to be embedded in the xln, though the crystal formation of gained L-Serine is good than crystallisation by cooling technology, purity is also than crystallisation by cooling technology height, but the organic solvent of embedding brings disadvantageous effect for the application of L-Serine.If the control of organic solvent add-on is improper, crystallization is grown up rapidly, and organic solvent embedding amount is higher.
Above-mentioned two kinds of crystallization processes of existing employing, the very difficult L-Serine that obtains good crystal formation.Therefore, solving the crystal formation problem of L-Serine, is the gordian technique that current L-Serine is produced.But up to now, relate to L-Serine column crystallization body crystallization processes of the present invention and do not see document or patent report as yet.
Summary of the invention
The objective of the invention is to set up a kind of column crystallization body crystallization processes of L-Serine and provide high-quality L-Serine raw material for field of medicaments, cosmetic field.
The present invention can reach by the following technical programs:
1. L-Serine crude product is made the L-Serine crystal solution of purifying through processing such as dissolving, decolourings;
2. the L-Serine crystal solution of purifying is at 30～50 ℃, and cultivation does not contain the L-Serine nucleus of crystal water under stirring, and grows up to the column crystallite gradually;
3. under agitation add methyl alcohol or ethanol, control determining alcohol 10～50% constantly grows up the column crystallite of L-Serine under stirring, the control stirring velocity makes the slow sedimentation of column crystallization body of growing up to certainweight, treats that the column crystallization body separates out when finishing, stop to stir blowing;
4. column crystallization body centrifuge dripping, after the alcohol washing, 60 ℃ of dryings obtain the column crystallization body product of L-Serine;
5. the solution that throws away of whizzer is failed back crystallizer, continues crystallization under determining alcohol 30%-50%, 5 ℃ of-10 ℃ of conditions of temperature, reclaims uncrystallized L-Serine in the filtrate.
That L-Serine column crystallization body of the present invention can be used as is anticancer, anti-AIDS new drug, medicine intermediate raw material, is used for the superior cosmetics additive.
L-Serine crude product in above-mentioned 1 is the undried product of centrifuge dripping after the alcohol washing, and dissolving water is anti-saturated with water, and active carbon for decolorization is a monosodium glutamate level carbon, and addition is 3～5% of a L-Serine crude product, and destainer filters through carbon block filter.
Temperature control in above-mentioned 2,30～50 ℃ of temperature ranges adopt the hot water control of full automatic control electric heat water tank.
The methyl alcohol that adopts in above-mentioned 3 is 96～97%, and the ethanol of employing is 95%, 98%.
Washing alcohol in above-mentioned 4 is 95% ethanol, and drying mode is oven dry under the normal pressure.
The 5 ℃ of temperature that are not less than in above-mentioned 5 adopt the control of ethylene glycol refrigerant.
The present invention compares with existing domestic crystallization processes has following advantage:
1. the crystallization processes of the present invention's employing is in aqueous phase system, changes between crystallization control process sphere of instability and Jie stable region, makes the L-Serine at first form the nucleus of not being with crystal water, and suitably grows up to the column crystallite;
2. the crystallization processes of the present invention's employing is promptly to add organic solvent after the column crystallite of aqueous phase system is bred, and constantly changes the polarity of solution system, and the column crystallization body is grown up under water-organic solvent phase system;
3. the crystallization processes that adopts of the present invention, neither crystallisation by cooling technology under the simple aqueous phase system, neither single dilution crystallization technology, but two new crystallization processes that technology produces through optimum combination;
4. by crystallization processes operation of the present invention, gained L-Serine is not powder crystal or hexagonal rhomboidal crystal, but the column crystallization body;
5. the crystallization processes that adopts of the present invention, gained L-Serine product detects by Japanese Ajincomoto Co., Inc quality standard (2002 version), and product content and product transmitance all are not less than 99.0 %;
6. the crystallization processes of the present invention's employing can be finished the crystallization of L-Serine in general crystallizer, does not need to increase special crystallizer, factory can use original production equipment and implement crystallization processes of the present invention, so less investment is arranged, instant effect, the advantage of high efficiency;
7. the crystallization processes of the present invention's employing only needs controlled temperature, determining alcohol, three reference mark of stirring velocity, helps the stable, practical of production technique and quality product;
8. the crystallization processes of the present invention's employing is simple to operate, easily is operated the workman and grasps, and is fit to industrialization promotion and uses.
Description of drawings
1, Fig. 1 crystallisation by cooling technology, the L-Serine xln of aqueous phase system gained easily is broken into indefinite form or hypocrystalline form, * 10
2, Fig. 2 dilution crystallization technology, the methanol-water phase system is through the L-Serine xln of cooling gained, for containing the prismatic crystal form of embedding thing, * 10
3, Fig. 3 dilution crystallization technology, the L-Serine xln of methanol-water phase system gained is for containing the particulate state prismatic crystal form of embedding thing, * 10
4, the L-Serine column crystallization crystallite bred of Fig. 4 crystallization processes aqueous phase system of the present invention, * 40
5, the L-Serine column crystal habit of Fig. 5 crystallization processes water of the present invention-pure phase system gained, * 10.
Embodiment
Example one
1. take by weighing L-Serine crude product 5000g, knock down and be equipped with in the anti-waterlogged retort of 8.0L, be warming up to about 70 ℃ of dissolving crude products under stirring, after dissolving crude product is complete, add 150～250g gac, decolouring 30min imports solution carbon block filter then and filters the removal gac, and crossing the about 10.0L of cleaner liquid is solution to be crystallized;
2. with in the solution input crystallizer to be crystallized,, be stirred to and see that L-Serine crystallite occurs with 30～50 ℃ of temperature in the electric heat water tank hot water crystallization control jar;
3. after treating that L-Serine crystallite occurs, 30～50 ℃ of additional proportion amount methyl alcohol, controlled temperature, the column crystallization body of L-Serine is slowly grown up, look crystallization situation additional proportion amount methyl alcohol again, the control methanol concentration constantly increases the column crystallization body of generation 10～50%, the control stirring velocity, allow the column crystallization body sedimentation that has grown up to, ensure the xln homogeneous that generates;
4. the column crystallization body crystallization situation of L-Serine in the observation crystallizer when finding that the column crystallization body is no longer grown up, stops to stir, and makes the column crystallization body sedimentation that has grown up to;
5. the column crystallization body that will fall to the crystallizer bottom moves into whizzer, dries, and filtrate is failed back crystallizer, and the xln of drying adds an amount of washing with alcohol secondary, dries the back and shifts out from whizzer;
6. the xln that dries is placed in the loft drier 60 ℃ of controlled temperature, the down dry about 6h of normal pressure, the column crystallization body 2950g of acquisition L-Serine;
7. fail back the filtrate of crystallizer, about 50% at determining alcohol, temperature is not less than under 5 ℃ of conditions and continues crystallization, reclaims uncrystallized L-Serine in the filtrate;
8. dried column crystallization body send to be picked up, and detects product content 99.2 %, product transmitance 99.0% by Japanese Ajincomoto Co., Inc quality standard (2002 version).
Example two
1. take by weighing L-Serine crude product 5000g, knock down and be equipped with in the anti-waterlogged retort of 8.0L, be warming up to about 70 ℃ of dissolving crude products under stirring, after dissolving crude product is complete, add 150～250g gac, 30 min that decolour import solution carbon block filter then and filter and remove gac, and crossing the about 10.0L of cleaner liquid is solution to be crystallized;
2. with in the solution input crystallizer to be crystallized,, be stirred to and see that L-Serine crystallite occurs with 30～50 ℃ of temperature in the electric heat water tank hot water crystallization control jar;
3. after treating that L-Serine crystallite occurs, additional proportion amount methyl alcohol, 30～50 ℃ of controlled temperature, the column crystallization body of L-Serine is slowly grown up, look crystallization situation additional proportion amount methyl alcohol again, the control methanol concentration is 10～50%, the column crystallization body of generation is constantly increased, the control stirring velocity allows the column crystallization body sedimentation that has grown up to, ensures the xln homogeneous that generates;
4. the column crystallization body crystallization situation of L-Serine in the observation crystallizer when finding that the column crystallization body is no longer grown up, stops to stir, and makes the column crystallization body sedimentation that has grown up to;
5. the column crystallization body that will fall to the crystallizer bottom moves into whizzer, dries, and filtrate is failed back crystallizer, and the xln of drying adds an amount of washing with alcohol secondary, dries the back and shifts out from whizzer;
6. the xln that dries is placed in the loft drier 60 ℃ of controlled temperature, dry 6h under the normal pressure, the column crystallization body 3030g of acquisition L-Serine;
7. fail back the filtrate of crystallizer,, temperature about 50% at determining alcohol is not less than under 5 ℃ of conditions and continues crystallization, reclaims uncrystallized L-Serine in the filtrate;
8. dried column crystallization body send to be picked up, and detects product content 99.0 %, product transmitance 99.0% by Japanese Ajincomoto Co., Inc quality standard (2002 version).
Example three
1. take by weighing L-Serine crude product 5000g, knock down and be equipped with in the anti-waterlogged retort of 8.0L, be warming up to about 70 ℃ of dissolving crude products under stirring, after dissolving crude product is complete, add 150～250g gac, 30 min that decolour import solution carbon block filter then and filter and remove gac, and crossing the about 10.0L of cleaner liquid is solution to be crystallized;
2. with in the solution input crystallizer to be crystallized,, be stirred to and see that L-Serine crystallite occurs with 30～50 ℃ of temperature in the electric heat water tank hot water crystallization control jar;
3. after treating that L-Serine crystallite occurs, additional proportion amount ethanol, 30～50 ℃ of controlled temperature, the column crystallization body of L-Serine is slowly grown up, look crystallization situation additional proportion amount ethanol again, the control alcohol concn is 10～50%, the column crystallization body of generation is constantly increased, the control stirring velocity allows the column crystallization body sedimentation that has grown up to, ensures the xln homogeneous that generates;
4. the column crystallization body crystallization situation of L-Serine in the observation crystallizer when finding that the column crystallization body is no longer grown up, stops to stir, and makes the column crystallization body sedimentation that has grown up to;
5. the column crystallization body that will fall to the crystallizer bottom moves into whizzer, dries, and filtrate is failed back crystallizer, and the xln of drying adds an amount of washing with alcohol secondary, dries the back and shifts out from whizzer;
6. the xln that dries is placed in the loft drier 60 ℃ of controlled temperature, down dry about 6 h of normal pressure, the column crystallization body 2900g of acquisition L-Serine;
7. fail back the filtrate of crystallizer, about 50% at determining alcohol, temperature is not less than under 5 ℃ of conditions and continues crystallization, reclaims uncrystallized L-Serine in the filtrate;
8. dried column crystallization body send to be picked up, and detects product content 99.2 %, product transmitance 99.3% by Japanese Ajincomoto Co., Inc quality standard (2002 version).
Example four
1. take by weighing L-Serine crude product 5000g, knock down and be equipped with in the anti-waterlogged retort of 8.0L, be warming up to about 70 ℃ of dissolving crude products under stirring, after dissolving crude product is complete, add 150～250g gac, 30 min that decolour import solution carbon block filter then and filter and remove gac, and crossing the about 10.0L of cleaner liquid is solution to be crystallized;
2. with in the solution input crystallizer to be crystallized,, be stirred to and see that L-Serine crystallite occurs with 30～50 ℃ of temperature in the electric heat water tank hot water crystallization control jar;
3. after treating that L-Serine crystallite occurs, additional proportion amount ethanol, 30～50 ℃ of controlled temperature, the column crystallization body of L-Serine is slowly grown up, look crystallization situation additional proportion amount ethanol again, the control alcohol concn is 10～50%, the column crystallization body of generation is constantly increased, the control stirring velocity allows the column crystallization body sedimentation that has grown up to, ensures the xln homogeneous that generates;
4. the column crystallization body crystallization situation of L-Serine in the observation crystallizer when finding that the column crystallization body is no longer grown up, stops to stir, and makes the column crystallization body sedimentation that has grown up to;
5. the column crystallization body that will fall to the crystallizer bottom moves into whizzer, dries, and filtrate is failed back crystallizer, and the xln of drying adds an amount of washing with alcohol secondary, dries the back and shifts out from whizzer;
6. the xln that dries is placed in the loft drier 60 ℃ of controlled temperature, the down dry about 6h of normal pressure, the column crystallization body 2860g of acquisition L-Serine;
7. fail back the filtrate of crystallizer,, temperature about 50% at determining alcohol is not less than under 5 ℃ of conditions and continues crystallization, reclaims uncrystallized L-Serine in the filtrate;
Dried column crystallization body send to be picked up, and detects product content 99.4 %, product transmitance 99.3% by Japanese Ajincomoto Co., Inc quality standard (2002 version).
Claims (1)
1. the column crystallization body crystallization processes of a L-Serine is characterized in that being made up of following steps:
(1) .L-Serine crude product is handled through dissolving, decolouring, makes the L-Serine crystal solution of purifying;
(2). the L-Serine crystal solution of purifying is at 30～50 ℃, and cultivation does not contain the L-Serine nucleus of crystal water under stirring, and grows up to the column crystallite gradually;
(3). under agitation add methyl alcohol or ethanol, control determining alcohol 10～50% is constantly grown up the column crystallite of L-Serine, the control stirring velocity makes the slow sedimentation of column crystallization body of growing up to certainweight, treats that the column crystallization body separates out when finishing, stop to stir blowing;
(4). column crystallization body centrifuge dripping, after the alcohol washing, 60 ℃ of dryings, the column crystallization body product of acquisition L-Serine;
(5). the solution that whizzer throws away is failed back crystallizer, at determining alcohol 30～50%, continues crystallization under 5～10 ℃ of conditions of temperature, reclaims uncrystallized L-Serine in the filtrate.
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| L-丝氨酸结晶过程研究;李侠;《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》;20090415(第4期);B016-53 * |
| 李侠.L-丝氨酸结晶过程研究.《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》.2009,(第4期),B016-53. |
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