CN108157908A - It is a kind of to utilize the method for vacuumizing and preparing high heap density I+G mixed crystal - Google Patents

It is a kind of to utilize the method for vacuumizing and preparing high heap density I+G mixed crystal Download PDF

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CN108157908A
CN108157908A CN201810132321.5A CN201810132321A CN108157908A CN 108157908 A CN108157908 A CN 108157908A CN 201810132321 A CN201810132321 A CN 201810132321A CN 108157908 A CN108157908 A CN 108157908A
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mixed crystal
dissolved
crystal
heap density
agent
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武晓丹
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    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L27/00Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
    • A23L27/20Synthetic spices, flavouring agents or condiments
    • A23L27/23Synthetic spices, flavouring agents or condiments containing nucleotides

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  • Life Sciences & Earth Sciences (AREA)
  • Proteomics, Peptides & Aminoacids (AREA)
  • Health & Medical Sciences (AREA)
  • Nutrition Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Polymers & Plastics (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Saccharide Compounds (AREA)

Abstract

The application is a kind of theoretical using the method combination cocrystallization for preparing high heap density I+G mixed crystal is vacuumized, introducing vacuumizes means, the parameters such as dissolved agent drop rate, stir speed (S.S.), vacuum degree are studied, it is high that a kind of heap density is prepared, granularity is big, product is uniform, the I+G mixed crystal of good fluidity.Technical process is simple, is easy to control, and solves in I+G mixed crystal preparation process, influence factor is excessive, the mixed crystal product of high-quality can be prepared in the technical issues of many factors are difficult to coordinate in constant parameter area, significantly reduce the difficulty of technical process control.The I+G mixed crystal Lens capsule d (50) of preparation are 481~569 μm, and heap density is 0.90~0.96g/ml.When vacuumizing crystallization, dissolved agent is recycled, and the dissolved agent of recycling is added in solution and continues to participate in dissolved, has saved cost.

Description

It is a kind of to utilize the method for vacuumizing and preparing high heap density I+G mixed crystal
Technical field
A kind of preparation method of the sapidity nucleotide disodium is claimed in the present invention, belongs to food dressing field, specifically relates to A kind of and method that the sapidity nucleotide disodium is prepared using crystallization mode.
Background technology
The sapidity nucleotide disodium (Disodium 5 '-ribonucleotide, abbreviation I+G) is 5 '-inosine acid disodium
(Disodium 5 '-inosinate, abbreviation IMP) and 5 '-Sodium guanylate (5 '-guanylate of Disodium , abbreviation GMP) crystal or mixture,.IMP, GMP are nucleotide derivative, are widely present in the various meat of the Nature In class and mushroom class, in natural meat delicate flavour and mushroom delicate flavour.The process of production flavour nucleotide mainly has microorganism hair Ferment method, enzymatic isolation method, enzyme catalysis method and chemical synthesis etc..By IMP and GMP stostes made from above-mentioned several method, through overrich The operations separation such as contract, crystallize, being filtered, washed and dried can obtain respective crude product.The crystallization process of IMP easily carries out, molten Crystal can directly be precipitated in liquid crystallization;And that GMP is precipitated in the solution is usually amorphous, to obtain GMP and have to pass through one The process of crystalline form conversion, process control is more complicated, and crystal product poor morphology, the heap density generally yielded is low, easy coalescence. Due to the difference of the various crystal shapes of IMP and GMP and powder characteristics, if the solid for simply crystallizing the two zymotic fluid Powder-product mechanical mixture in proportion, not only mixed process have various operational difficulties, but also obtained mix product It is difficult to obtain ideal mixed effect.
The process of production flavour nucleotide mainly has microbe fermentation method, enzymatic isolation method, enzyme catalysis method and chemical synthesis Method etc..By IMP and GMP stostes made from above-mentioned several method, by concentrating, crystallizing, the operations such as being filtered, washed and dried and detach It can obtain respective crude product.The crystallization process of IMP easily carries out, and crystal can directly be precipitated in solution crystallization;And GMP is in solution Middle precipitation it is usually amorphous, to obtain the process that GMP has to pass through the conversion of crystalline form, process control is more complicated, The crystal product poor morphology, the heap density that generally yield is low, easy coalescence.Due to the various crystal shapes of IMP and GMP and powder characteristics Difference, if the solid powder product for simply crystallizing the two zymotic fluid mechanical mixture in proportion, not only mixed process There are various operational difficulties, and obtained mix product also is difficult to obtain ideal mixed effect.
Dilution crystallization is the difference using separated object matter and solvent molecule Interaction Force, by solute be dissolved in water or In other solvents, then other solvent is so that solubility of the solute in former solvent reduces, so as to make solute that crystallization be precipitated.It crosses Saturation degree is the important factor in order of lolute crystallization, and degree of supersaturation is small, and growth rate is slow, advantageously forms that grain size is big, crystal form is complete Whole, good dispersion crystal, degree of supersaturation is too big, and crystal growth rate and nucleation rate increase, easily formed it is explosive into Core easily forms irregular crystal.
The Chinese patent of CN101619086A discloses a kind of flavour nucleotide crystal and preparation method.In preparation process In, using IMP, GMP crude product as raw material, component ratio 1:1.By dissolving, eluting, dissolved, natural cooling, again dissolved, cold again But, filtering, vacuum drying step, obtain reported crystal form.The technique is changed by adjusting the parameters such as stirring, solution temperature, pH It has been apt to product crystal form and quality.But the preparation method cools down fine grain by standing, makes its outburst nucleation, the granularity and shape of crystal Shape can not regulate and control, and final product heap density is 0 .58-0 .63g/ml, and crystal angle of repose is 38-46 °.The heap of crystal Density is still relatively low, mobility is poor.
CN105495528A discloses a kind of method for preparing high heap density the sapidity nucleotide disodium mixed crystal, with IMP, GMP crude products are raw material, and dissolving, the agent of addition dissolved carry out growing the grain, by adding nucleus, and adjust the adding rate of solvent to control Crystallization process processed, the Lens capsule d (50) being prepared are 200~450 μm, and heap density is 0.76~0.86g/ml, not Angle till is 20~30 °.However, its heap density is still relatively low, and the crystal structure time is long, low production efficiency.Control of keeping under strict control is needed simultaneously The adding rate of dissolved agent processed, technique are relatively complicated.
The comprehensive analysis prior art, the method for finding to prepare I+G mixed crystal in the prior art, technical process is complex, mistake Journey is difficult to control, and the I+G mixed crystal heap density prepared is relatively low, and particle is smaller, and mobility is poor.
Invention content
In view of the deficiencies of the prior art, the application provides a kind of method that can quickly prepare I+G, and technical process is easily controlled System, process is simple, and the I+G heaps density being prepared is high, and granularity is big, good fluidity.
The present invention is achieved through the following technical solutions.
A kind of method for preparing high heap density the sapidity nucleotide disodium mixed crystal;It is it is characterized in that as follows including step:
1) IMP, GMP crude product are pressed 0.95 ~ 1.05:1 is added to the water, and compound concentration is the aqueous solution of 150 ~ 180g/L, and stirring is molten Solution adjusts pH to 7.5~8.0;2) solubilization analysis agent to solution is in saturation state, and the I+G for then adding in crude product quality 2 ~ 3% is brilliant Kind;It at the uniform velocity stirs, while constant-speed material-adding solubilization analysis agent, and vacuumizes crystallization;3) suction filtration, washing and normal temperature and pressure drying are in Flavor nucleotide disodium mixed crystal product.
When vacuumizing crystallization, dissolved agent is recycled, and the dissolved agent of recycling is then added in solution and carries out dissolved.
Step 2)In, stir speed (S.S.) is 100rpm ~ 125rpm.
Step 2)In, dissolved agent is ethyl alcohol, and dissolved agent at the uniform velocity drop rate is 0.5 ~ 2ml/min.
Step 2)In, vacuum degree control is in 0.07 ~ 0.09MP.
The size distribution d (50) of crystal product is 481~569 μm, and heap density is 0.90~0.96g/ml.
The drop rate of dissolved agent and the crystallization of flavour nucleotide and growing the grain have very big relationship, usually faster to be added dropwise Rate causes high degree of supersaturation, leads to the generation of a large amount of nucleus, conversely, slower drop rate then have using formed it is larger Crystal.The size of stir speed (S.S.) has a great impact to the speed of crystallization, the size of crystal, form more, is not stirred after gentle agitation The supersaturated solution mixed can form wider metastable region, and crystallization induction time is elongated, and the crystal of preparation is larger, and particle It is more uniform, and during stir speed (S.S.) increase, metastable region narrows, degree of supersaturation increase, easily explosive to be nucleated, and obtains smaller crystalline substance Body product.Temperature is one of important parameter for influencing Crystallization and growth, and when solution degree of supersaturation is certain, crystallization temperature is low When, obtained crystal is comparatively fine, and the extraction then obtained when temperature is high is larger, and higher temperature can change crystallization medium and solution The interfacial tension of phase, diffusion coefficient increase, nucleus generates rate and reduces, but the growth rate of nucleus increases, and can obtain larger Crystal grain.The addition of crystal seed all has very important influence to the rate and crystal growth of crystallization, adds suitable crystalline substance Kind can make crystal seed suspend in the solution, and most of solute will be attached to seed crystals, promote nucleus growth, can obtain Even crystal product.With reference to cocrystallization theory, applicant has carried out above-mentioned technological parameter analysis experiment, it is intended to find a kind of behaviour Make simple, superior product quality I+G products, however, since the factor influenced on solution degree of supersaturation is too many, any one amount Variation can all cause larger change, and research, which once entered, stagnates, however, when applicant introduces and vacuumizes means, surprisingly It was found that dissolved agent adding rate, stir speed (S.S.) can maintained constant, and do not have on the basis of additionally temperature is adjusted, A kind of I+G products of high-quality are prepared.It vacuumizing in crystallization process, solvent and dissolved agent are evaporated concentration simultaneously, but by In the instillation for keeping dissolved agent, solution is remained in hypersaturated state, the study found that control vacuum degree control 0.07 ~ In the range of 0.09MP, it is 0.5 ~ 2ml/min to keep solvent drop rate.Solution degree of supersaturation can be maintained to maintain Jie steady Area, solute are uniformly attached on crystal seed, and product form is uniform.On the other hand, it due to the presence of vacuum state, is formd in nucleus Certain negative pressure due to the propulsion of pressure, promotes solute closer when being attached on crystal seed, close so as to improve the heap of product Degree.Crystal product size distribution d (50) prepared by the application is 481~569 μm, and heap density is 0.90~0.96g/ml.
The application has the advantages that relative to the prior art:
1. technical process is simple, it is easy to control, solves in I+G mixed crystal preparation process, influence factor is excessive, and many factors are difficult to The mixed crystal product of high-quality can be prepared in constant parameter area, significantly reduce work the technical issues of coordination The difficulty of skill process control.
3. vacuumize crystallization, dissolved agent is recycled, and the dissolved agent of recycling is added in solution and is continued to participate in Dissolved has saved cost.
3. in I+G mixed crystal preparation process, vacuum crystallization means are introduced, with reference to dissolved agent drop rate, stir speed (S.S.) The control of technological parameters is waited, the I+G mixed crystal of high-quality has been prepared, Lens capsule d (50) is 481~569 μm, heap Density is 0.90~0.96g/ml.
Specific embodiment
With reference to embodiment, the invention will be further described.
Embodiment 1:
1) 95gIMP crude products, 100gGMP crude products is taken to be added to the water, compound concentration is the aqueous solution of 180g/L, and stirring and dissolving is adjusted PH to 7.5;2) solubilization analysis agent to solution is in saturation state, then adds in the I+G crystal seeds of crude product quality 3%;100rpm is at the uniform velocity stirred It mixes, ethyl alcohol is at the uniform velocity added, and vacuumize by the rate of 2ml/min, maintenance vacuum degree is 0.09MP, is crystallized;3) filter, wash, It is dry, obtain I+G mixed crystal products;When vacuumizing crystallization, recycle dissolved agent, and by the dissolved agent of recycling be then added in solution into Row dissolved, after measured, product heap density are 0.93g/ml, and granularity is 532 μm.
Embodiment 2:
1) 105gIMP crude products, 100gGMP crude products is taken to be added to the water, compound concentration is the aqueous solution of 150g/L, and stirring and dissolving is adjusted Save pH to 7.7;2) solubilization analysis agent to solution is in saturation state, then adds in the I+G crystal seeds of crude product quality 2%;110rpm is at the uniform velocity Stirring, ethyl alcohol is at the uniform velocity added, and vacuumize by the rate of 2ml/min, and maintenance vacuum degree is 0.08MP, is crystallized;3) it filters, wash It washs, dry, obtain I+G mixed crystal products.When vacuumizing crystallization, dissolved agent is recycled, and the dissolved agent of recycling is then added to solution Middle carry out dissolved.After measured, product heap density is 0.95g/ml.Granularity is 569 μm.
Embodiment 3:
1) 100gIMP crude products, 100gGMP crude products is taken to be added to the water, compound concentration is the aqueous solution of 160g/L, and stirring and dissolving is adjusted Save pH to 7.6;2) solubilization analysis agent to solution is in saturation state, then adds in the I+G crystal seeds of crude product quality 2.5%;115rpm is even Speed stirring, ethyl alcohol is at the uniform velocity added, and vacuumize by the rate of 1.0ml/min, and maintenance vacuum degree is 0.08MP, is crystallized;3) filter, Washing, drying, obtain I+G mixed crystal products.When vacuumizing crystallization, dissolved agent is recycled, and the dissolved agent of recycling is then added to molten Dissolved is carried out in liquid.After measured, product heap density is 0.93g/ml.Granularity is 501 μm.
Embodiment 4:
1) 103gIMP crude products, 100gGMP crude products is taken to be added to the water, compound concentration is the aqueous solution of 170g/L, and stirring and dissolving is adjusted Save pH to 8.0;2) solubilization analysis agent to solution is in saturation state, then adds in the I+G crystal seeds of crude product quality 2.3%;125rpm is even Speed stirring, ethyl alcohol is at the uniform velocity added, and vacuumize by the rate of 0.5ml/min, and maintenance vacuum degree is 0.07MP, is crystallized;3) filter, Washing, drying, obtain I+G mixed crystal products.When vacuumizing crystallization, dissolved agent is recycled, and the dissolved agent of recycling is then added to molten Dissolved is carried out in liquid.After measured, product heap density is 0.90g/ml.Granularity is 545 μm.
Comparative example 1:
1) 100gIMP crude products, 100gGMP crude products is taken to be added to the water, compound concentration is the aqueous solution of 160g/L, and stirring and dissolving is adjusted Save pH to 7.6;2) solubilization analysis agent to solution is in saturation state, then adds in the I+G crystal seeds of crude product quality 2.5%;115rpm is even Speed stirring, ethyl alcohol is at the uniform velocity added, and vacuumize by the rate of 1.0ml/min, and maintenance vacuum degree is 0.12MP, is crystallized;3) filter, Washing, drying, obtain I+G mixed crystal products.After measured, product heap density is 0.78g/ml.Granularity is 394 μm.
Comparative example 2:
1) 99gIMP crude products, 100gGMP crude products is taken to be added to the water, compound concentration is the aqueous solution of 170g/L, and stirring and dissolving is adjusted PH to 8.0;2) solubilization analysis agent to solution is in saturation state, then adds in the I+G crystal seeds of crude product quality 2.3%;125rpm is at the uniform velocity Stirring, ethyl alcohol is at the uniform velocity added by the rate of 1ml/min, is crystallized;3) it filters, wash, is dry, obtaining I+G mixed crystal products.Through surveying Fixed, product heap density is 0.50g/ml.Granularity is 315 μm.
Above-described embodiment is the preferable embodiment of the application, and contrast test reflects the application technical process and technique Influence of the adjustment of parameter to the crystal quality of preparation, but presently filed embodiment and be not restricted to the described embodiments, Parameter is adjusted all within the protection domain of the application in the range that the application gives.

Claims (5)

1. it is a kind of using the method for preparing high heap density I+G mixed crystal is vacuumized, it is characterized in that as follows including step:
1) IMP, GMP crude product are pressed 0.95 ~ 1.05:1 is added to the water, and compound concentration is the aqueous solution of 150 ~ 180g/L, and stirring is molten Solution adjusts pH to 7.5~8.0;2) solubilization analysis agent to solution is in saturation state, and the I+G for then adding in crude product quality 2 ~ 3% is brilliant Kind;It at the uniform velocity stirs, while constant-speed material-adding solubilization analysis agent, and vacuumizes crystallization;3) suction filtration, washing and normal temperature and pressure drying are in Flavor nucleotide disodium mixed crystal product;When vacuumizing crystallization, recycle dissolved agent, and by the dissolved agent of recycling be then added in solution into Row dissolved.
2. the method as described in claim 1, step 2)In, stir speed (S.S.) is maintained in the range of 100rpm ~ 125rpm.
3. the method as described in claim 1, step 2)In, dissolved agent is ethyl alcohol, and dissolved agent at the uniform velocity drop rate control is 0.5 In the range of ~ 2ml/min.
4. the method as described in claim 1, step 2)In, vacuum degree control is in the range of 0.07 ~ 0.09MP.
5. I+G mixed crystal prepared by any one of claim 1 ~ 4 the method, the size distribution d (50) of crystal is 481~569 μ M, heap density are 0.90~0.96g/ml.
CN201810132321.5A 2018-02-09 2018-02-09 It is a kind of to utilize the method for vacuumizing and preparing high heap density I+G mixed crystal Pending CN108157908A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102718823A (en) * 2012-06-26 2012-10-10 华南理工大学 Process method for elution, crystallization and refining of 5'-flavor nucleotide disodium
CN103755723A (en) * 2014-02-07 2014-04-30 天津大学 Method for preparing rifampicin I crystal form
CN105495528A (en) * 2015-11-27 2016-04-20 天津大学 Method for preparing high-bulk-density flavor nucleotides disodium mixed crystal
CN106008297A (en) * 2016-06-03 2016-10-12 宁夏紫光天化蛋氨酸有限责任公司 Novel methionine crystal form II and preparation method thereof
CN106928297A (en) * 2017-03-10 2017-07-07 南京工业大学 A kind of method of oil analysis conversion regulation and control Sodium guanylate crystallization process

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102718823A (en) * 2012-06-26 2012-10-10 华南理工大学 Process method for elution, crystallization and refining of 5'-flavor nucleotide disodium
CN103755723A (en) * 2014-02-07 2014-04-30 天津大学 Method for preparing rifampicin I crystal form
CN105495528A (en) * 2015-11-27 2016-04-20 天津大学 Method for preparing high-bulk-density flavor nucleotides disodium mixed crystal
CN106008297A (en) * 2016-06-03 2016-10-12 宁夏紫光天化蛋氨酸有限责任公司 Novel methionine crystal form II and preparation method thereof
CN106928297A (en) * 2017-03-10 2017-07-07 南京工业大学 A kind of method of oil analysis conversion regulation and control Sodium guanylate crystallization process

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