CN101560234A - Production method of ribonucleotide sodium salt - Google Patents
Production method of ribonucleotide sodium salt Download PDFInfo
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- CN101560234A CN101560234A CNA2009101318082A CN200910131808A CN101560234A CN 101560234 A CN101560234 A CN 101560234A CN A2009101318082 A CNA2009101318082 A CN A2009101318082A CN 200910131808 A CN200910131808 A CN 200910131808A CN 101560234 A CN101560234 A CN 101560234A
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- sodium salt
- ampna
- ribonucleotide
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- umpna
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Abstract
As a food additive and a pharmaceutical intermediate, the ribonucleotide sodium salt is very important. The ribonucleotide comprises an adenylic acid, a cytidylic acid, a uridylic acid, a guanylic acid and an inosinic acid. The sodium salt is usually 5'-ribonucleotide disodium. The invention relates to and adopts a special preparation technology for resolving the problem of bad crystal form and can obtain a plurality of types of sodium salt even tetrasodium salt, and the invention has the characteristics of good crystal form, high quality and high yield.
Description
One, technical field
Nucleotide and sodium salt thereof are very important as foodstuff additive and medicine intermediate, the present invention relates to adopt special preparation technology to solve the characteristic of poor crystal form, raising sodium salt quality and yield.
Two, technical background
In the prior art, adopt the nucleolysis method, chemosynthesis and enzymic synthesis method three major types make Nucleotide, on molecular structure, generally form Nucleotide by nucleosides and phosphoric acid, by pentose and based composition nucleosides, wherein phosphoric acid be connected on the 5th carbon of sugar be called 5 '-Nucleotide, 5 ' position phosphoric acid has two hydroxyls, can with alkali reaction generate sodium salt promptly 5 '-disodium 5 '-ribonucleotide, when we find with alkali reaction in practice, under different pH values, can generate multiple sodium salt or even four sodium, also be found report at present at home, 5 '-Nucleotide in sugar second, two hydroxyls are also arranged on three carbon, add that phosphoric acid has two hydroxyls, have four hydroxyls, can form sodium salt in theory, divide into one but in product, be difficult to strictness, two, three, tetra-na salt is in the disodium salt commonly used, neither pure disodium, often contain one, two, trisodium salt, so normal product content and pH value of influencing, the present invention adopts special methods to make product content and pH value reach requirement and improve yield in preparation.
Moreover because sodium salt contains a plurality of crystal water, general requirement is moisture less than 25%, inosine acid disodium (IMPNa
2) less than 29%, adopt traditional oven drying method to survey content that moisture content calculates and compare on the low sidely with actual, need change the karl Fischer method into and survey moisture content and calculate content, practice shows that this method is relatively near actual value.
It should be appreciated that in addition because the sodium salt water content is big, the sodium salt that has can not obtain good crystallization routinely, for example adenylic acid (AMP) disodium (AMPNa
2) becoming viscous fluid easily, the sodium salt that has contains a large amount of phosphoric acid salt and sodium-chlor, needs to make with extra care repeatedly to cause low, the complex operation of product yield, and the present invention is intended to solve the technical barrier that different sodium salt runs into.
Three, summary of the invention
The general conventional preparation technology of ribonucleotide sodium salt is after Nucleotide or its sodium salt add water adjust pH dissolving, add alcohol (first, ethanol) separate out sodium salt after filtration, washing, exsiccant sodium salt finished product.AMPNa for example
2Preparation technology can only obtain thickly routinely, and the present invention adopts low pH value to obtain a crystal formation sodium preferably earlier, slowly adds the good AMPNa of alkali reaction generation crystal formation again
2, also can make the good AMPNa of crystal formation
4The uridylic acid trisodium that customer requirement provides generally can not get the good UMPNa of crystal formation
3Among the conventional preparation technology, disodium 5 '-ribonucleotide salt is defined as 5% aqueous solution in the standard at home and abroad, wherein urine, bird, inosine acid disodium (U, G, IMPNa2) pH value are 7～8.5, cytidylic acid disodium (CMPNa2) pH value is 8～9.5, as seen pH value a wider range, sometimes product pH value and content are defective, and there is the low problem of yield in process for purification routinely.The present invention adopts the method that adjust pH reacts in certain dilute alcohol solution, can obtain qualified sodium salt.
The domestic process for purification of once reporting a kind of like this UMPNa2: adopt the UMPNa2 aqueous ethanolic solution, low temperature is separated out inorganic salt, remove by filter to add alcohol again and separate out UMPNa2, but the difficult grasp of this technology, operation is complicated.Given this, the present invention adopts the UMPNa2 aqueous solution to be cooled to and removes inorganic salt about zero degree, add the method that alcohol obtains UMPNa2 again, has the yield advantages of higher.
Four, embodiment
Example 1: adenylic acid (AMP) four sodium AMPNa
4Preparation: 15 gram AMP add water 45ml, add 17ml 30% liquid caustic soda, splash into 95% ethanol 210ml, separate out the about 4h of white crystals filtration, with the 100ml washing with alcohol dry AMPNa
422.91g, moisture 20%, weight yield 152.71%.5% aqueous solution, pH value 12.32, chromatogram content 98.10%, ultraviolet content is pressed AMPNa85.12%, AMPNa
290.19%, AMPNa
395.26%, AMPNa
4100.34%, from content and strong pH value, not 5 '-the adenylic acid (AMP) disodium, but 5 ', 2 ', 3 '-adenylic acid (AMP) four sodium.
Example 2:AMPNa preparation: 15 gram AMP add the dissolving of water 60ml adjust pH, add 240ml 95% ethanol and separate out AMPNa, filtration washing oven dry, content 98.5%, 5% pH value of water solution 5.82.
Example 3:AMPNa
2Preparation: 15 gram AMP add water 45ml adjust pH dissolving, after adding 210ml 95% ethanol and separating out AMPNa, slowly add again alkali reaction obtain crystal formation good, do not have block, not sticking AMPNa
2, content 99.63%.
Example 4: uridine monophosphate disodium UMPNa
2Preparation: according to UMPNa
2In contain the inorganic salt amount, be made into the finite concentration aqueous solution, about zero degree of lowering the temperature is separated out inorganic salt and is removed by filter UMPNa
2Aqueous solution furnishing finite concentration, adjust pH add 95% ethanol and separate out UMPNa
2Filtration washing, the heavily refining routinely high purity UMPNa that obtains
2
Example 5: the disodium 5 '-ribonucleotide salt of low levels prepares the high yield sodium salt of high quality: low levels disodium 5 '-ribonucleotide salt adds a certain amount of Diluted Alcohol, and adjust pH stirs several hours after-filtration washing and drying and obtains the high yield sodium salt of high purity.
Claims (4)
1. ribonucleotide sodium salt preparation method, this method comprises: produce crystal formation earlier a good sodium generates disodium again under the highly basic condition, for example AMPNa
2, the sodium salt of low levels can be adjusted the reaction of pH value at aqueous ethanolic solution, and filtration washing obtains high-content sodium salt, UMPNa
2Furnishing finite concentration and pH value cooling desalination, redilution adds alcohol and produces high-content UMPNa
2
2. by the described AMPNa of claim 1
2Preparation method, AMP add 2～6 times of water, with adjusting PH with base 5～7, add 5～15 times of 95% ethanol, make to generate crystal formation sodium salt preferably, slowly add alkali again, and final pH 5.8～7.0 filtration washings get AMPNa
2
3. in 30～80% alcohol dilute solutions, transfer pH5.8～8.5 by the described low levels sodium salt of claim 1 (comprising five kinds of ribonucleotide sodium salts), react several hours filtration washings and obtain the high yield sodium salt of high quality.
4. by claim 1UMPNa
2Furnishing 25～60% concentration of aqueous solution are transferred pH7～9, lower the temperature-2～3 ℃, remove inorganic salt, transfer concentration 10～30% aqueous solution again, and pH5.8～7.5 add 1.2～4 times of 95% ethanol and separate out UMPNa
2Filtration washing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2009101318082A CN101560234A (en) | 2009-04-08 | 2009-04-08 | Production method of ribonucleotide sodium salt |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2009101318082A CN101560234A (en) | 2009-04-08 | 2009-04-08 | Production method of ribonucleotide sodium salt |
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|---|---|
| CN101560234A true CN101560234A (en) | 2009-10-21 |
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ID=41219233
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|---|---|---|---|
| CNA2009101318082A Pending CN101560234A (en) | 2009-04-08 | 2009-04-08 | Production method of ribonucleotide sodium salt |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103435669A (en) * | 2013-09-09 | 2013-12-11 | 南京工业大学 | Solvent-out crystallization method for uridine-5'-monophosphate disodium |
-
2009
- 2009-04-08 CN CNA2009101318082A patent/CN101560234A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103435669A (en) * | 2013-09-09 | 2013-12-11 | 南京工业大学 | Solvent-out crystallization method for uridine-5'-monophosphate disodium |
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Application publication date: 20091021 |