CN101293907B - Technique for preparing 5'-inosine acid disodium - Google Patents
Technique for preparing 5'-inosine acid disodium Download PDFInfo
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- CN101293907B CN101293907B CN 200810028996 CN200810028996A CN101293907B CN 101293907 B CN101293907 B CN 101293907B CN 200810028996 CN200810028996 CN 200810028996 CN 200810028996 A CN200810028996 A CN 200810028996A CN 101293907 B CN101293907 B CN 101293907B
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Abstract
The invention relates to a production process of 5'-disodium inosinate, particularly to a production process of 5'-disodium inosinate by barium (Ba) precipitation. The production process comprises the steps of: collecting 5'-disodium inosinate water phase, adding certain 5'-disodium inosinate equivalent times of BaCl2 solution (saturated or nearly saturated), adding membrane caustic soda or alkali under stirring to neutralize to pH 7.3-7.6, adding certain 5'-disodium inosinate equivalent times of BaCl2 solution (saturated or nearly saturated), stirring, allowing precipitation, cooling down to below 10 DEG C, performing vacuum filtration with a Buchner funnel filter paper to obtain a mother liquid and a barium inosinate (IMPBa) salt, calculating mother liquid loss rate, adding the IMPBa salt into NaSP4 solution (saturated or nearly saturated) with certain equivalent times of 5'-disodium inosinate in the 5'-disodium inosinate water phase, stirring at 60-70 DEG C to precipitate inosinate (IMP), performing vacuum filtration with a Buchner funnel filter paper at 60-70 DEG C to obtain a BaSO4 precipitate and a filtrate, and calculating 5'-disodium inosinate yield and purity of 5'-disodium inosinate in the filtrate. Compared with the prior art, the inventive production process has the advantages of improved yield and purity of 5'-disodium inosinate, and reduced production cost.
Description
Technical field
The present invention relates to a kind of 5 '-inosine acid disodium production technique, particularly obtain the production technique of 5 '-inosine acid disodium with the Ba depositing technology.
Background technology
5 '-t-inosinic acid (5 '-IMP) be an intermediate material of biological nucleic acid anabolism system, it is used to multiple field, like food and medicine, and multiple medical field.5 '-t-inosinic acid (5 '-IMP) non-hygroscopic, water-soluble, stabilized aqueous solution.In acidic solution, be prone to during high temperature decompose, can be decomposed by Phosphoric acid esterase and destroy, be dissolved in ethanol slightly, be dissolved in ether hardly.When JECFA estimated once more in 1993,5 '-inosine acid disodium do not have carcinogenic, teratogenecity, and breeding is not had harm.And it belongs to one of nucleic acid class seasonings; Its sodium salt except that itself has delicate flavour and Sodium Glutamate produce synergy when mix using, simultaneously sweet taste, meat flavour are had synergism; One-tenth, acid, bitter taste and raw meat, the smell of burning there is restraining effect; Along with improving constantly of living standards of the people, the demand of 5 '-t-inosinic acid sodium salt is increased rapidly, therefore quality is also had higher requirement.As 5 ' of midbody-t-inosinic acid (5 '-IMP) quality played conclusive effect to the finished product.Through direct fermentation produce 5 '-production technique of inosine acid disodium is known in this field, the important key of economic aspect be high density with high yield production 5 '-inosine acid disodium.Prior art cooling water slowly adds 45%NaOH (w/v) solution, and record PH=10.8 this moment, and temperature is 20.3 ℃.When cooling to-0.5 ℃ again, centrifugation adds 45%NaOH (w/v) solution once more and neutralizes, and neutralization finishes, and this moment, pH value was 7.4, and temperature is 26 ℃, is cooled to 0 ℃ of cooling, and with the crystallization suction filtration, 5 '-the inosine acid disodium bullion.Whole process is consuming time longer, and the solution crystallization is slow, and in addition solution heats up higherly in the exogenously added alkali process, will constantly cool off midway, is unfavorable for the generation of xln, consumes cold greatly simultaneously, and power cost is high, and the bullion yield is low, and solution purity is also not high enough.
Summary of the invention
The object of the invention provides a kind of production technique of 5 '-inosine acid disodium, and it can overcome the deficiency of prior art.
The present invention is achieved in that
Get 5 '-the inosine acid disodium water, add 5 '-certain equivalent multiple BaCl of inosine acid disodium equivalents
2Solution (saturated or near saturated), stir on one side, adding film alkali is neutralized to PH7.3-7.6 on one side, or adds alkali and be neutralized to PH7.3-7.6, add 5 then '-certain equivalent multiple BaCl of inosine acid disodium equivalents
2Solution (saturated or approaching saturated) stirs deposition, is cooled to below 10 ℃; With B filter paper vacuum filtration; Mother liquor and IMPBa salt, calculating mother liquor rate of loss, IMPBa salt added to be equivalent to 5 '-inosine acid disodium aqueous phase 5 '-Na of certain equivalent multiple of inosine acid disodium equivalents
2SO
4Solution (saturated or approaching saturated), IMP is separated out in 60-70 ℃ of stirring, and 60-70 ℃ begins with B filter paper vacuum filtration, gets BaSO
4Deposition and filtrating, calculate in the filtrating 5 '-the inosine acid disodium yield with survey purity.
The present invention compared with prior art, have improve 5 '-yield and the purity of inosine acid disodium crystallization, advantage such as reduce production costs.
Embodiment
Embodiment 1
Get 5 '-inosine acid disodium water 200ml, add BaCl
2Solution (saturated or near saturated) 300ml, stir on one side, adding film alkali is neutralized to PH7.3-7.6 on one side, or adds alkali and be neutralized to PH7.3-7.6, adds BaCl
2Solution (saturated or approaching saturated) 300ml stirs deposition, normal temperature, and 5 minutes time, with B filter paper vacuum filtration, get mother liquor and IMPBa salt, calculate the mother liquor rate of loss, IMPBa salt is added to Na
2SO
4Solution (saturated or near saturated) is to 200ml, 60 ℃ of stirrings, and 3 hours time, separate out 5 '-inosine acid disodium, 60 ℃ begin to consider fast 5L/m with B filter paper vacuum filtration
2H gets BaSO
4Deposition and filtrating, calculate in the filtrating 5 '-the inosine acid disodium yield with survey purity.
Embodiment 2
Get 5 '-inosine acid disodium water 200ml, add BaCl
2Solution (saturated or near saturated) 300ml, stir on one side, adding film alkali is neutralized to PH7.3-7.6 on one side, or adds alkali and be neutralized to PH7.3-7.6, adds BaCl
2Solution (saturated or approaching saturated) 300ml stirs deposition, and 0 ℃, 5 minutes time, with B filter paper vacuum filtration, get mother liquor and IMPBa salt, calculate the mother liquor rate of loss, IMPBa salt is added to Na
2SO
4Solution (saturated or near saturated) is to 200ml, 60 ℃ of stirrings, and 20 minutes time, separate out 5 '-inosine acid disodium, 60 ℃ begin with B filter paper vacuum filtration, filtering velocity 5L/m
2H gets BaSO
4Deposition and filtrating, calculate in the filtrating 5 '-the inosine acid disodium yield with survey purity.
Embodiment 3
Get 5 '-inosine acid disodium water 200ml, add BaCl
2Solution (saturated or near saturated) 300ml, stir on one side, adding film alkali is neutralized to PH7.3-7.6 on one side, or adds alkali and be neutralized to PH7.3-7.6, adds BaCl
2Solution (saturated or approaching saturated) 300ml stirs deposition, is cooled to below 10 ℃, and 40 minutes time, with B filter paper vacuum filtration, get mother liquor and IMPBa salt, calculate the mother liquor rate of loss, IMPBa salt is added to Na
2SO
4Solution (saturated or near saturated) is to 200ml, stirring at normal temperature, and 20 minutes time, separate out 5 '-inosine acid disodium, with B filter paper vacuum filtration, filtering velocity 5L/m
2H gets BaSO
4Deposition and filtrating, calculate in the filtrating 5 '-the inosine acid disodium yield with survey purity.
Embodiment 4
Get 5 '-inosine acid disodium water 200ml, add BaCl
2Solution (saturated or near saturated) 300ml, stir on one side, adding film alkali is neutralized to PH7.3-7.6 on one side, or adds alkali and be neutralized to PH7.3-7.6, adds BaCl
2Solution (saturated or approaching saturated) 300ml stirs deposition, is cooled to below 10 ℃, and 40 minutes time, with B filter paper vacuum filtration, get mother liquor and IMPBa salt, calculate the mother liquor rate of loss, IMPBa salt is added to Na
2SO
4Solution (saturated or near saturated) is to 200ml, 60 ℃ of stirrings, and 3 hours time, separate out 5 '-inosine acid disodium, with B filter paper vacuum filtration, filtering velocity 5L/m
2H gets BaSO
4Deposition and filtrating, calculate in the filtrating 5 '-the inosine acid disodium yield with survey purity.
Embodiment 5
Get 5 '-inosine acid disodium water 200ml, add BaCl
2Solution (saturated or near saturated) 100ml, stir on one side, adding film alkali is neutralized to PH7.3-7.6 on one side, or adds alkali and be neutralized to PH7.3-7.6, adds BaCl
2Solution (saturated or approaching saturated) 100ml stirs deposition, is cooled to below 4 ℃, and 30 minutes time, with B filter paper vacuum filtration, get mother liquor and IMPBa salt, calculate the mother liquor rate of loss, IMPBa salt is added to Na
2SO
4Solution (saturated or near saturated) is to 200ml, 70 ℃ of stirrings, and 3 hours time, separate out 5 '-inosine acid disodium, with B filter paper vacuum filtration, filtering velocity 5L/m
2H gets BaSO
4Deposition and filtrating, calculate in the filtrating 5 '-the inosine acid disodium yield with survey purity.
Embodiment 6
Get 5 '-inosine acid disodium water 200ml, add BaCl
2Solution (saturated or near saturated) 100ml, stir on one side, adding film alkali is neutralized to PH7.3-7.6 on one side, or adds alkali and be neutralized to PH7.3-7.6, adds BaCl
2Solution (saturated or approaching saturated) 100ml stirs deposition, is cooled to below 4 ℃, and 120 minutes time, with B filter paper vacuum filtration, get mother liquor and IMPBa salt, calculate the mother liquor rate of loss, IMPBa salt is added to Na
2SO
4Solution (saturated or near saturated) is to 200ml, 70 ℃ of stirrings, and 3 hours time, separate out 5 '-inosine acid disodium, with B filter paper vacuum filtration, filtering velocity 5L/m
2H gets BaSO
4Deposition and filtrating, calculate in the filtrating 5 '-the inosine acid disodium yield with survey purity.
Embodiment 7
Get 5 '-inosine acid disodium water 200ml, add BaCl
2Solution (saturated or near saturated) 200ml, stir on one side, adding film alkali is neutralized to PH7.3-7.6 on one side, or adds alkali and be neutralized to PH7.3-7.6, adds BaCl
2Solution (saturated or approaching saturated) 100ml stirs deposition, is cooled to below 10 ℃, and 120 minutes time, with B filter paper vacuum filtration, get mother liquor and IMPBa salt, calculate the mother liquor rate of loss, IMPBa salt is added to Na
2SO
4Solution (saturated or near saturated) is to 200ml, 70 ℃ of stirrings, and 3 hours time, separate out 5 '-inosine acid disodium, with B filter paper vacuum filtration, filtering velocity 5L/m
2H gets BaSO
4Deposition and filtrating, calculate in the filtrating 5 '-the inosine acid disodium yield with survey purity.
Obtain in the foregoing description 1~7 5 '-yield of inosine acid disodium and purity with and the rate of loss of water mother liquor, the result is shown in table 1:
Table 1
The purity of 5 ' Sodium Inosinate disodium is to measure with HPLC, and the present invention uses BaCl
2The precipitator method have obtained desirable result.Compared with prior art, its rate of loss obviously reduces, and yield significantly improves, and its purity also increases under certain condition.In general, the present invention can obtain 5 ' Sodium Inosinate disodium more economically than prior art.
Claims (5)
1. the preparation method of 5 '-inosine acid disodium is characterized in that having following steps: get 5 '-inosine acid disodium water 200ml, add saturated BaCl
2Solution 300ml, stir on one side, adding alkali is neutralized to pH7.3-7.6 on one side, adds saturated BaCl
2Solution 300ml stirs deposition, and 0 ℃, 5 minutes time, with B filter paper vacuum filtration, get mother liquor and 5 '-t-inosinic acid barium salt, calculate the mother liquor rate of loss, 5 '-t-inosinic acid barium salt is added to saturated Na
2SO
4Solution is to 200ml, 60 ℃ of stirrings, and 20 minutes time, separate out 5 '-inosine acid disodium, 60 ℃ begin with B filter paper vacuum filtration, filtering velocity 5L/m
2H gets BaSO
4Precipitate and filtrating, calculate 5 '-inosine acid disodium yield and survey purity in the filtrating.
2. the preparation method of 5 '-inosine acid disodium is characterized in that having following steps: get 5 '-inosine acid disodium water 200ml, add saturated BaCl
2Solution 300ml, stir on one side, adding alkali is neutralized to pH7.3-7.6 on one side, adds saturated BaCl
2Solution 300ml stirs deposition, is cooled to below 10 ℃, and 40 minutes time, with B filter paper vacuum filtration, get mother liquor and 5 '-t-inosinic acid barium salt, calculate the mother liquor rate of loss, 5 '-t-inosinic acid barium salt is added to saturated Na
2SO
4Solution is to 200ml, and 60 ℃ of stirrings, are separated out 5 '-inosine acid disodium, with B filter paper vacuum filtration, filtering velocity 5L/m at 3 hours time
2H gets BaSO
4Precipitate and filtrating, calculate 5 '-inosine acid disodium yield and survey purity in the filtrating.
3. the preparation method of 5 '-inosine acid disodium is characterized in that having following steps: get 5 '-inosine acid disodium water 200ml, add saturated BaCl
2Solution 100ml, stir on one side, adding alkali is neutralized to pH7.3-7.6 on one side, adds saturated BaCl
2Solution 100ml stirs deposition, is cooled to below 4 ℃, and 30 minutes time, with B filter paper vacuum filtration, get mother liquor and 5 '-t-inosinic acid barium salt, calculate the mother liquor rate of loss, 5 '-t-inosinic acid barium salt is added to saturated Na
2SO
4Solution is to 200ml, and 70 ℃ of stirrings, are separated out 5 '-inosine acid disodium, with B filter paper vacuum filtration, filtering velocity 5L/m at 3 hours time
2H gets BaSO
4Precipitate and filtrating, calculate 5 '-inosine acid disodium yield and survey purity in the filtrating.
4. the preparation method of 5 '-inosine acid disodium is characterized in that having following steps: get 5 '-inosine acid disodium water 200ml, add saturated BaCl
2Solution 100ml, stir on one side, adding alkali is neutralized to pH7.3-7.6 on one side, adds saturated BaCl
2Solution 100ml stirs deposition, is cooled to below 4 ℃, and 120 minutes time, with B filter paper vacuum filtration, get mother liquor and 5 '-t-inosinic acid barium salt, calculate the mother liquor rate of loss, 5 '-t-inosinic acid barium salt is added to saturated Na
2SO
4Solution is to 200ml, and 70 ℃ of stirrings, are separated out 5 '-inosine acid disodium, with B filter paper vacuum filtration, filtering velocity 5L/m at 3 hours time
2H gets BaSO
4Precipitate and filtrating, calculate 5 '-inosine acid disodium yield and survey purity in the filtrating.
5. the preparation method of 5 '-inosine acid disodium is characterized in that having following steps: get 5 '-inosine acid disodium water 200ml, add saturated BaCl
2Solution 200ml, stir on one side, adding alkali is neutralized to pH7.3-7.6 on one side, adds saturated BaCl
2Solution 100ml stirs deposition, is cooled to below 10 ℃, and 120 minutes time, with B filter paper vacuum filtration, get mother liquor and 5 '-t-inosinic acid barium salt, calculate the mother liquor rate of loss, 5 '-t-inosinic acid barium salt is added to saturated Na
2SO
4Solution is to 200ml, and 70 ℃ of stirrings, are separated out 5 '-inosine acid disodium, with B filter paper vacuum filtration, filtering velocity 5L/m at 3 hours time
2H gets BaSO
4Precipitate and filtrating, calculate 5 '-inosine acid disodium yield and survey purity in the filtrating.
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CN102199182A (en) * | 2011-04-10 | 2011-09-28 | 浙江钱江生物化学股份有限公司 | One-step extraction method for disodium 5'-inosinate |
CN102718823B (en) * | 2012-06-26 | 2014-11-12 | 华南理工大学 | Process method for elution, crystallization and refining of 5'-flavor nucleotide disodium |
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CN1508140A (en) * | 2002-11-22 | 2004-06-30 | 味之素株式会社 | Method for preparing purine derivative disodium nucleotate crystal and dealcoholing method |
CN1539846A (en) * | 2003-10-29 | 2004-10-27 | 徐昌洪 | Technique for preparing 5'nucleotide bi-sodium |
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CN1508140A (en) * | 2002-11-22 | 2004-06-30 | 味之素株式会社 | Method for preparing purine derivative disodium nucleotate crystal and dealcoholing method |
CN1539846A (en) * | 2003-10-29 | 2004-10-27 | 徐昌洪 | Technique for preparing 5'nucleotide bi-sodium |
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黄亚光等.采用纳滤技术回收粗母液中的肌苷酸钠.《食品与发酵工业》.2004,(第8期),全文. * |
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