CN101293907A - Technique for preparing 5'-inosine acid disodium - Google Patents
Technique for preparing 5'-inosine acid disodium Download PDFInfo
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- CN101293907A CN101293907A CN 200810028996 CN200810028996A CN101293907A CN 101293907 A CN101293907 A CN 101293907A CN 200810028996 CN200810028996 CN 200810028996 CN 200810028996 A CN200810028996 A CN 200810028996A CN 101293907 A CN101293907 A CN 101293907A
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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 10DEG 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 60-70DEG C to precipitate inosinate (IMP), performing vacuum filtration with a Buchner funnel filter paper at 60-70DEG 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, as food and medicine, and multiple medical field.5 '-t-inosinic acid (5 '-IMP) non-hygroscopic, water-soluble, stabilized aqueous solution.In acidic solution, easily decompose during high temperature, 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 is except that itself has delicate flavour, produce synergy when mixing use with Sodium Glutamate, simultaneously sweet taste, meat flavour there is synergism, salty, sour, 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 intermediate-t-inosinic acid (5 '-IMP) quality played conclusive effect to the finished product.By direct fermentation produce 5 '-production technique of inosine acid disodium is known in this field, the important key of economic aspect be high density and high yield produce 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 crude product.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, consume simultaneously cold big, the power cost height, the crude product yield is low, solution purity is also not high enough.
Summary of the invention
Purpose of the present invention provides a kind of production technique of 5 '-inosine acid disodium, and it can overcome the deficiencies in the 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 precipitation, is cooled to below 10 ℃, with B filter paper vacuum filtration, mother liquor and IMPBa salt, calculate the mother liquor rate of loss, IMPBa salt is 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 to get BaSO with B filter paper vacuum filtration
4Precipitation and filtrate, calculate in the filtrate 5 '-inosine acid disodium yield and 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 precipitation, normal temperature, and 5 minutes time, with B filter paper vacuum filtration, get mother liquor and IMPBa salt, calculating mother liquor rate of loss adds to Na with IMPBa salt
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
4Precipitation and filtrate, calculate in the filtrate 5 '-inosine acid disodium yield and 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 precipitation, and 0 ℃, 5 minutes time, with B filter paper vacuum filtration, get mother liquor and IMPBa salt, calculating mother liquor rate of loss adds to Na with IMPBa salt
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
4Precipitation and filtrate, calculate in the filtrate 5 '-inosine acid disodium yield and 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 precipitation, is cooled to below 10 ℃, and 40 minutes time, with B filter paper vacuum filtration, get mother liquor and IMPBa salt, calculating mother liquor rate of loss adds to Na with IMPBa salt
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
4Precipitation and filtrate, calculate in the filtrate 5 '-inosine acid disodium yield and 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 precipitation, is cooled to below 10 ℃, and 40 minutes time, with B filter paper vacuum filtration, get mother liquor and IMPBa salt, calculating mother liquor rate of loss adds to Na with IMPBa salt
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
4Precipitation and filtrate, calculate in the filtrate 5 '-inosine acid disodium yield and 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 precipitation, is cooled to below 4 ℃, and 30 minutes time, with B filter paper vacuum filtration, get mother liquor and IMPBa salt, calculating mother liquor rate of loss adds to Na with IMPBa salt
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
4Precipitation and filtrate, calculate in the filtrate 5 '-inosine acid disodium yield and 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 precipitation, is cooled to below 4 ℃, and 120 minutes time, with B filter paper vacuum filtration, get mother liquor and IMPBa salt, calculating mother liquor rate of loss adds to Na with IMPBa salt
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
4Precipitation and filtrate, calculate in the filtrate 5 '-inosine acid disodium yield and 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 precipitation, is cooled to below 10 ℃, and 120 minutes time, with B filter paper vacuum filtration, get mother liquor and IMPBa salt, calculating mother liquor rate of loss adds to Na with IMPBa salt
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
4Precipitation and filtrate, calculate in the filtrate 5 '-inosine acid disodium yield and 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 results are shown in table 1:
Table 1
The purity of 5 ' Sodium Inosinate disodium is to measure the present invention BaCl with HPLC
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 (8)
1, a kind of production technique of 5 '-inosine acid disodium is characterized in that having following steps: 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 precipitation, is cooled to below 10 ℃, with B filter paper vacuum filtration, mother liquor and IMPBa salt, calculate the mother liquor rate of loss, IMPBa salt is 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 to get BaSO with B filter paper vacuum filtration
4Precipitation and filtrate, calculate in the filtrate 5 '-inosine acid disodium yield and survey purity.
2, the production technique of a kind of 5 '-inosine acid disodium according to claim 1 is characterized in that having following steps: 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 precipitation, normal temperature, and 5 minutes time, with B filter paper vacuum filtration, get mother liquor and IMPBa salt, calculating mother liquor rate of loss adds to Na with IMPBa salt
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
4Precipitation and filtrate, calculate in the filtrate 5 '-inosine acid disodium yield and survey purity.
3, the production technique of a kind of 5 '-inosine acid disodium according to claim 1 is characterized in that having following steps: 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 precipitation, and 0 ℃, 5 minutes time, with B filter paper vacuum filtration, get mother liquor and IMPBa salt, calculating mother liquor rate of loss adds to Na with IMPBa salt
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
4Precipitation and filtrate, calculate in the filtrate 5 '-inosine acid disodium yield and survey purity.
4, the production technique of a kind of 5 '-inosine acid disodium according to claim 1 is characterized in that having following steps: 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 precipitation, is cooled to below 10 ℃, and 40 minutes time, with B filter paper vacuum filtration, get mother liquor and IMPBa salt, calculating mother liquor rate of loss adds to Na with IMPBa salt
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
4Precipitation and filtrate, calculate in the filtrate 5 '-inosine acid disodium yield and survey purity.
5, the production technique of a kind of 5 '-inosine acid disodium according to claim 1 is characterized in that having following steps: 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 precipitation, is cooled to below 10 ℃, and 40 minutes time, with B filter paper vacuum filtration, get mother liquor and IMPBa salt, calculating mother liquor rate of loss adds to Na with IMPBa salt
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
4Precipitation and filtrate, calculate in the filtrate 5 '-inosine acid disodium yield and survey purity.
6, the production technique of a kind of 5 '-inosine acid disodium according to claim 1 is characterized in that having following steps: 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 precipitation, is cooled to below 4 ℃, and 30 minutes time, with B filter paper vacuum filtration, get mother liquor and IMPBa salt, calculating mother liquor rate of loss adds to Na with IMPBa salt
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
4Precipitation and filtrate, calculate in the filtrate 5 '-inosine acid disodium yield and survey purity.
7, the production technique of a kind of 5 '-inosine acid disodium according to claim 1 is characterized in that having following steps: 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 precipitation, is cooled to below 4 ℃, and 120 minutes time, with B filter paper vacuum filtration, get mother liquor and IMPBa salt, calculating mother liquor rate of loss adds to Na with IMPBa salt
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
4Precipitation and filtrate, calculate in the filtrate 5 '-inosine acid disodium yield and survey purity.
8, the production technique of a kind of 5 '-inosine acid disodium according to claim 1 is characterized in that having following steps: 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 precipitation, is cooled to below 10 ℃, and 120 minutes time, with B filter paper vacuum filtration, get mother liquor and IMPBa salt, calculating mother liquor rate of loss adds to Na with IMPBa salt
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
4Precipitation and filtrate, calculate in the filtrate 5 '-inosine acid disodium yield and survey purity.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
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 |
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 |
Family Cites Families (2)
Publication number | Priority date | Publication date | Assignee | Title |
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JP4010230B2 (en) * | 2002-11-22 | 2007-11-21 | 味の素株式会社 | Method for producing purine derivative nucleotide disodium crystal and method for removing methanol |
CN1243009C (en) * | 2003-10-29 | 2006-02-22 | 徐昌洪 | Technique for preparing 5'nucleotide bi-sodium |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
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 |
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 |
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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