CN105603018A - Method for indirectly preparing D-sodium erythorbate - Google Patents
Method for indirectly preparing D-sodium erythorbate Download PDFInfo
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Abstract
The invention discloses a method for indirectly preparing D-sodium erythorbate, belonging to the technical field of biochemical separation synthesis. The method comprises the following steps: by using a Serratia marcescens SDSPY-136 strain fermentation liquid as a raw material, carrying out fermentation liquid pretreatment, methyl 2-keto-D-gluconate reaction and conversion reaction to obtain crude D-sodium erythorbate; and carrying out refinement and purification to obtain the D-sodium erythorbate product. The Serratia marcescens is used as a production strain to obtain the calcium 2-keto-D-gluconate, and multiple impurity removal modes are combined to convert the treatment liquid into the D-sodium erythorbate. The obtained fermentation liquid has the advantages of high 2-keto-D-gluconic acid yield and high conversion rate; the crude D-sodium erythorbate product has high purity and is easy to refine, so the total yield is enhanced; and the method has favorable popularization and application prospects.
Description
Technical field
Biochemistry of the present invention separates synthesis technical field, particularly a kind of method of indirectly preparing D-araboascorbic acid sodium.
Background technology
The different ascorbic acid of D-(Erythorbicacid, EA), has another name called erythorbic acid or Arabic ascorbic acid, is a kind of optical isomer of L-AA sodium, is called for short different Vc. The different ascorbic acid of D-and sodium salt (Sodiumerythorbate, EN) thereof have very strong reproducibility, and the effect of anticorrosion antioxygen is better than vitamin C greatly, also strong than vitamin C to hot stability, and price only has ascorbic 1/2. Arabo-ascorbic acid and sodium salt thereof are safe and effective food additives, are widely used in varieties of food items. Sodium isoascorbate is white or micro-yellow acicular crystal, odorless, and taste is slightly salty, more stable in air, meets photochromic gradual change dark, easily molten in water, at methyl alcohol, micro dissolution in alcohol. The preparation method of D-araboascorbic acid sodium mainly contains indirect fermentation method, direct fermentation and enzyme process. In industrial production, adopting at present indirect fermentation method to ferment produces with synthetic combining.
2-KDG (2-keto-D-gluconicacid, 2-KGA) is the key intermediate in food additives (antioxidant) D-araboascorbic acid and sodium salt commercial process thereof. 2-KGA molecular formula is C6H10O7, molecular weight is 194. 2-KGA is white grain body in appearance, is slightly with saline taste, odorless, and it is acid that the soluble in water and aqueous solution shows slightly, and has optical activity, and its specific rotatory power is [α] 25D=-88 °. The generation bacterium of 2-KGA distributes comparatively extensive, most bacterial strains are wild type, belong to pseudomonas (Pseudomonas), Erwinia (Erwinia), Serratia (serratia) and acetobacter (Acetobacter).
The bacterium of 2-KGA production both at home and abroad adopts the bacterial strain of pseudomonas conventionally at present, and D-araboascorbic acid sodium yield and purity that the zymotic fluid of this kind of bacterial strain obtains through processing such as over-churnings are lower. Develop a kind of D-araboascorbic acid sodium yield method high and that purity is high significant.
The Chinese invention patent " a kind of serratia marcescens strain of production of high purity 2-KDG " that application publication number is " CN104830712A " discloses employing serratia marcescens (Serratiamarcescens) SDSPY-136 strain fermentation production of high purity 2-KDG, this bacterial strain is preserved in China Committee for Culture Collection of Microorganisms's common micro-organisms center (CGMCC), deposit number is N0.10548, the preservation time: on February 9th, 2015.
Summary of the invention
In order to make up the deficiencies in the prior art, the zymotic fluid that the invention provides a kind of serratia marcescens (Serratiamarcescens) SDSPY-136 bacterial strain that adopts production of high purity 2-KDG is prepared the method for the different ascorbic acid of D-.
Technical scheme of the present invention is:
A kind of preparation method who indirectly prepares D-araboascorbic acid sodium, taking the zymotic fluid of serratia marcescens (Serratiamarcescens) SDSPY-136 bacterial strain as raw material, obtain the thick sodium salt of D-araboascorbic acid through fermentation liquor pretreatment, 2-KDG esterification reaction of organic acid, conversion reaction; Obtain D-araboascorbic acid sodium product through refining purifying again; Described serratia marcescens (Serratiamarcescens) SDSPY-136 bacterial strain has been preserved in China Committee for Culture Collection of Microorganisms's common micro-organisms center, and its deposit number is CGMCCNo:10548, and its preservation time is: on February 9th, 2015.
As preferred version, the described preparation method who indirectly prepares D-araboascorbic acid sodium, concrete steps are:
1) strain fermentation
According to the inoculum concentration of 8-12%, the seed liquor of described serratia marcescens (Serratiamarcescens) SDSPY-136 bacterial strain is inoculated in fermentation medium, at 29-31 DEG C, 400-600r/min condition bottom fermentation cultivation 30-40h, obtain 2-KDG zymotic fluid;
2) fermentation liquor pretreatment
Described 2-KDG zymotic fluid adds the concentrated sulfuric acid in the centrifugal rear gained stillness of night, then under the water bath condition of 50-95 DEG C, in the stillness of night after acidifying, adds active carbon, stirs decolouring; Filtering active carbon after decolouring, gained filtrate is crossed cation exchange resin column, and by the treatment fluid decompression distillation of collecting after cation exchange resin column removal of impurities, obtaining solid content is that 70-90% obtains 2-KDG concentrate;
3) esterification reaction of organic acid
In described 2-KDG concentrate, add methyl alcohol, and using sulfuric acid as catalyst, in 60-100 DEG C of reaction 5-10h, react complete, concentrated, crystallization at 4 DEG C, suction filtration is also dried to obtain 2-KDG methyl esters salt;
4) conversion reaction
Described 2-KDG methyl esters salt is added in methyl alcohol and dissolved, then add methanol-hydrogen sodium oxide molybdena mixed liquor, at 55-70 DEG C, reaction 13-20min then places crystallization at 4 DEG C, and suction filtration obtains the thick sodium salt of D-araboascorbic acid;
5) D-araboascorbic acid sodium is refining
The thick sodium salt of gained D-araboascorbic acid is soluble in water, adds active carbon and oxalic acid, is heated to 50-70 DEG C, insulated and stirred 3-8min, and then suction filtration obtains filtrate while hot; Gained filtrate is cooling, crystallization, suction filtration with the dry D-araboascorbic acid sodium product that to obtain after the washing of 90-100% ethanol.
As preferred version, in step 1), obtain seed liquor seed culture medium used and consist of peptone 5g/L, sodium chloride 5g/L, beef extract 3g/L, pH value is 7.0; Described fermentation medium consists of glucose 180g/L, corn steep liquor 9.01g/L, potassium dihydrogen sulfate 1g/L, magnesium sulfate 0.4g/L, manganese chloride 0.037g/L, ferrous sulfate 0.036g/L, calcium carbonate 65g/L.
As preferred version, step 2) in the addition of the active carbon 5-15% that is solid content, bleaching time is at least 0.5h.
As preferred version, step 2) in, described cation exchange resin column is 732# cation exchange resin column, described cation exchange resin column ratio of height to diameter is 9:1-10:1, flow velocity 1-1.1 per hour times column volume.
As preferred version, in step 3), the addition of methyl alcohol meets: in every gram of 2-KDG concentrate, add 5-1.5mL methyl alcohol.
As preferred version, in step 4), in 2-KDG methyl esters salt, the addition of methyl alcohol meets: in every gram of 2-KDG methyl esters salt, add 10-10.5mL methyl alcohol; The addition of methanol-hydrogen sodium oxide molybdena mixed liquor meets: in every gram of 2-KDG methyl esters salt, add 4-4.5mL methanol-hydrogen sodium oxide molybdena mixed liquor.
As preferred version, in step 5), the addition of active carbon and oxalic acid is the 0.5%-0.7% of solid content.
Beneficial effect of the present invention:
The present invention obtains 2-KDG calcium taking serratia marcescens as producing strain fermentation, in conjunction with multiple removal of impurities mode, by treatment fluid Synthesis D-araboascorbic acid sodium, the zymotic fluid 2-KDG output that obtains is high, conversion ratio is high, D-araboascorbic acid sodium crude product purity is high, be easy to refine, total recovery is improved, and has good popularizing application prospect.
Brief description of the drawings
Below in conjunction with accompanying drawing, the present invention is further illustrated.
Fig. 1 is the D-araboascorbic acid sodium sample that the embodiment of the present invention 1 obtains;
Fig. 2 is the D-araboascorbic acid sodium sample liquid chromatogram that the embodiment of the present invention 1 obtains;
Fig. 3 is standard D-araboascorbic acid sodium sample liquid chromatogram.
Serratia marcescens (Serratiamarcescens) SDSPY-136 bacterial strain, this bacterial strain is preserved in China Committee for Culture Collection of Microorganisms's common micro-organisms center (CGMCC), preservation address: Yard 1, BeiChen xi Road, Chaoyang District, Beijing City, deposit number is N0.10548, the preservation time: on February 9th, 2015.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention will be further described, but the present invention is not limited only to this.
Seed culture medium consists of: peptone 5g/L, sodium chloride 5g/L, beef extract 3g/L, pH value is 7.0.
Fermentation medium consists of: glucose 180g/L, corn steep liquor 9.01g/L, potassium dihydrogen sulfate 1g/L, magnesium sulfate 0.4g/L, manganese chloride 0.037g/L, ferrous sulfate 0.036g/L, calcium carbonate 65g/L.
Embodiment 1
Indirectly prepare the preparation method of D-araboascorbic acid sodium, concrete steps are:
1) strain fermentation
Serratia marcescens (Serratiamarcescens) CGMCCN0.10548 bacterial strain is moved and connects slant activation.
Press the composition preparation seed culture medium of aforesaid liquid seed culture medium, 500ml triangular flask liquid amount is 50ml, 121 DEG C of steam sterilizings 20 minutes, be cooled to room temperature, inoculation slant strains 2 is encircled, and on to put rotation rotating speed and be 200r/min, radius of turn be 40mm shaking table, cultivates 12 hours for 30 DEG C, seed liquor, get seed liquor put 600nm survey light absorption value be 0.262;
Press 3L liquid amount preparation fermentation medium with 5L fermentation tank, adjust pH7.0,115 DEG C of real tank sterilizings 20 minutes, the good seed liquor 300ml of inoculated and cultured after circulating water to 30 DEG C, after inoculation, sampling and measuring concentration of glucose is 185g/L immediately.
Initial fermentation tank parameter is set to: speed of agitator is 350r/min, throughput 0.7 ~ 0.8Nm3/ h, tank internal pressure 0.065MPa. 30 ± 0.2 DEG C of controlled fermentation temperature in sweat are 35% by regulating speed of agitator and throughput control dissolved oxygen.
Sampling in every 4 hours in sweat, measure glucose, 2-KDG content and cell concentration in zymotic fluid, when glucose content is during lower than 10g/L, glucose, 2-KDG content in every 2 hours sampling and measuring zymotic fluids, in the time that 2-KDG content in zymotic fluid no longer increases, finish fermentation, fermentation period is 36 hours.
After fermentation ends, get zymotic fluid with 4000r/min centrifugal 10 minutes, get supernatant and measure the content of glucose, 2-KDG and be respectively 0.02g/L, 188.9g/L, the conversion ratio that conversion of glucose generates 2-KDG is 102.11%.
2) pretreatment of zymotic fluid
The centrifugal rear mensuration Ca of zymotic fluid2+Content is 0.66mol/L, adds the concentrated sulfuric acid of 0.66mol/L, makes Ca2+Be converted into calcium sulfate precipitation and get off, obtain acidifying clear liquid 2.7L after centrifugal; Solid content 19.2%, under 80 DEG C of water bath condition, adds the active carbon that accounts for solid content 5%, constantly stirs decolouring 0.5h, suction filtration after decolouring; Filtrate is through 732# cationic ion-exchange resin, efflux 3.1L; The treatment fluid of collecting through pillar removal of impurities is carried out to reduced pressure concentration in 55 DEG C, and being concentrated into solid content is 80%, altogether 501.3g.
3) esterification reaction of organic acid
Get 100g2-keto-D-gluconic acid concentrate, add 500ml methyl alcohol, make catalyst with the concentrated sulfuric acid, under 80 DEG C of water-baths, react 7h, and supplement methyl alcohol in reactor. After concentrated, in 4 DEG C of placements, after suction filtration, by washed with methanol, washing lotion is incorporated in clear liquid. Be deposited in 40 DEG C of oven dry, obtain methyl esters salt 64.12g.
4) conversion reaction
60g methyl esters salt is joined in 600ml methanol solution, stir it is dissolved completely, add methyl alcohol-NaOH solution 250ml, under 65 DEG C of water-baths, react 17min, suction filtration after 4 DEG C of placement a period of times, obtains thick sodium salt 50.82g, and purity is 98.1%. Wherein, methyl alcohol--in NaOH solution, the mass ratio of methyl alcohol and NaOH is 10:1.
5) D-araboascorbic acid sodium is refining
By soluble in water thick 50.5g sodium salt, add 0.3g oxalic acid and 0.3g active carbon, water bath heat preservation to 60 DEG C, insulated and stirred 5min, suction filtration obtains filtrate 150ml while hot. Through crystallisation by cooling, suction filtration, 95% ethanol washing crystal, 50 DEG C are dry, make D-araboascorbic acid sodium product 48.82g, and yield is 95.6%, and purity is 99.5%. Product is carried out to liquid phase analysis, show that product is sodium isoascorbate.
Embodiment 2
Indirectly prepare the preparation method of D-araboascorbic acid sodium, concrete steps are:
1) strain fermentation
Serratia marcescens (Serratiamarcescens) CGMCCN0.10548 bacterial strain is moved and connects slant activation.
Press the composition preparation seed culture medium of aforesaid liquid seed culture medium, 500ml triangular flask liquid amount is 50ml, 121 DEG C of steam sterilizings 20 minutes, be cooled to room temperature, inoculation slant strains 2 is encircled, and on to put rotation rotating speed and be 200r/min, radius of turn be 40mm shaking table, cultivates 12 hours for 30 DEG C, seed liquor, get seed liquor put 600nm survey light absorption value be 0.265;
Press 7L liquid amount preparation fermentation medium with 10L fermentation tank, adjust pH7.0,115 DEG C of real tank sterilizings 20 minutes, the good seed liquor 700ml of inoculated and cultured after circulating water to 30 DEG C, after inoculation, sampling and measuring concentration of glucose is 180g/L immediately.
Initial fermentation tank parameter is set to: speed of agitator is 350r/min, throughput 0.8 ~ 0.9Nm3/ h, tank internal pressure 0.065MPa. 30 ± 0.2 DEG C of controlled fermentation temperature in sweat are 35% by regulating speed of agitator and throughput control dissolved oxygen.
Sampling in every 4 hours in sweat, measure glucose, 2-KDG content and cell concentration in zymotic fluid, when glucose content is during lower than 10g/L, glucose, 2-KDG content in every 2 hours sampling and measuring zymotic fluids, in the time that 2-KDG content in zymotic fluid no longer increases, finish fermentation, fermentation period is 35 hours.
After fermentation ends, get zymotic fluid with 4000r/min centrifugal 10 minutes, get supernatant and measure the content of glucose, 2-KDG and be respectively 0.03g/L, 183.12g/L, the conversion ratio that conversion of glucose generates 2-KDG is 101.73%.
2) pretreatment of zymotic fluid
The centrifugal rear mensuration Ca of zymotic fluid2+Content is 0.67mol/L, adds the concentrated sulfuric acid of 0.67mol/L, makes Ca2+Be converted into calcium sulfate precipitation and get off, obtain acidifying clear liquid 6.5L after centrifugal; Solid content 19.5%, under 80 DEG C of water bath condition, adds the active carbon that accounts for solid content 5%, constantly stirs decolouring 0.5h, suction filtration after decolouring; Filtrate is through 732# cation exchange resin column, efflux 7.2L; The treatment fluid of collecting through pillar removal of impurities is carried out to reduced pressure concentration in 55 DEG C, and being concentrated into solid content is 79.5%, altogether 1.1kg.
3) esterification reaction of organic acid
Get 100g2-keto-D-gluconic acid concentrate, add 500ml methyl alcohol, make catalyst with the concentrated sulfuric acid, under 80 DEG C of water-baths, react 7h, and supplement methyl alcohol in reactor. After concentrated, in 4 DEG C of placements, after suction filtration, by washed with methanol, washing lotion is incorporated in clear liquid. Be deposited in 40 DEG C of oven dry, obtain methyl esters salt 64.10g.
4) conversion reaction
60g methyl esters salt is joined in 600ml methanol solution, stir it is dissolved completely, add methyl alcohol-NaOH solution 250ml, under 65 DEG C of water-baths, react 17min, suction filtration after 4 DEG C of placement a period of times, obtains thick sodium salt 50.93g, and purity is 98.0%. Wherein, methyl alcohol--in NaOH solution, the mass ratio of methyl alcohol and NaOH is 9:1.
5) D-araboascorbic acid sodium is refining
By soluble in water thick 50.0g sodium salt, add 0.3g oxalic acid and 0.3g active carbon, water bath heat preservation to 60 DEG C, insulated and stirred 5min, suction filtration obtains filtrate 155ml while hot. Through crystallisation by cooling, suction filtration, 95% ethanol washing crystal, 50 DEG C are dry, make D-araboascorbic acid sodium product 48.79g, and yield is 96.1%, and purity is 99.6%. Product is carried out to liquid phase analysis, show that product is sodium isoascorbate.
Comparative example 1
By serratia marcescens (SerratiamarcescensSDSPY-136) zymotic fluid replaces with the zymotic fluid of the bacterial strain of pseudomonas, and all the other are with embodiment 1.
The yield of this comparative example D-araboascorbic acid sodium is 90.2, and purity is 93.3.
Comparative example 2
Delete step 2) in the operation of " filtrate is through 732# cation exchange resin column ", filtrate is directly concentrated, and all the other are identical with embodiment 1.
The yield of this comparative example D-araboascorbic acid sodium is 85.2%, and purity is 90.1%.
Comparative example 3
In step 5), after the thick sodium salt of D-araboascorbic acid is water-soluble, only adds 0.3g active carbon, and do not add oxalic acid; All the other are identical with embodiment 1.
The yield of this comparative example D-araboascorbic acid sodium is 87.3%, and purity is 91.8%.
Above-mentioned glucose is measured as follows:
Use the SBA-4D type membrane bioreactor that Shandong Province academy sciences Biology Research Institute produces to measure. Measuring principle is to utilize the single-minded mensuration glucose content of fixation glucose dehydrogenation enzyme membrane.
Above-mentioned 2-KDG is measured as follows:
Use iodometric determination. Measuring principle is: 2-KDG molecule contains carboxyl and alcoholic extract hydroxyl group that esterification can directly occur, also contain the carbonyl that tautomerization can occur, under strong acidic condition, heating the 2-KDG aqueous solution can be D-araboascorbic acid by its Quantitative yield. Utilize D-araboascorbic acid and I2Redox reaction can quantitative assay D-araboascorbic acid mass concentration, be then converted into the mass concentration of 2-KDG.
Above-mentioned 2-KDG conversion ratio is measured as follows:
2-KDG conversion ratio (%)=2-KDG output (g/L)/[glucose content (g/L) in the rear culture medium of glucose content in initial medium (g/L)-fermentation]
Above-mentioned Ca2+Measure as follows and measure: the mensuration EDTA titration of GB/T7476-1987 water quality calcium
Above-mentioned D-araboascorbic acid sodium is measured as follows: the mensuration of GB8273-2008 food additives D-araboascorbic acid sodium.
The qualification of above-mentioned D-araboascorbic acid sodium is by the following method: high performance liquid chromatography. Chromatographic condition is: UltiMate3000 series VWD-3000 variable-wavelenght detector; Chromatographic column is Prontosil1202102C18 post (10 μ m, 4.6mmi.d. × 250mm); Mobile phase is prepared 0.1mol/LKH with redistilled water2PO4, phosphorus acid for adjusting pH to 2.5; Flow velocity is 0.5mL/min; Sampling volume is 20 μ L; Detection wavelength is 210nm; Column temperature is 30 DEG C.
Claims (8)
1. indirectly prepare the preparation method of D-araboascorbic acid sodium for one kind, it is characterized in that: taking the zymotic fluid of serratia marcescens (Serratiamarcescens) SDSPY-136 bacterial strain as raw material, obtain the thick sodium salt of D-araboascorbic acid through fermentation liquor pretreatment, 2-KDG esterification reaction of organic acid, conversion reaction; Obtain D-araboascorbic acid sodium product through refining purifying again; Described serratia marcescens (Serratiamarcescens) SDSPY-136 bacterial strain has been preserved in China Committee for Culture Collection of Microorganisms's common micro-organisms center, and its deposit number is CGMCCNo:10548, and its preservation time is: on February 9th, 2015.
2. the preparation method who indirectly prepares as claimed in claim 1 D-araboascorbic acid sodium, is characterized in that, concrete steps are:
1) strain fermentation
According to the inoculum concentration of 8-12%, the seed liquor of described serratia marcescens (Serratiamarcescens) SDSPY-136 bacterial strain is inoculated in fermentation medium, at 29-31 DEG C, 400-600r/min condition bottom fermentation cultivation 30-40h, obtain 2-KDG zymotic fluid;
2) fermentation liquor pretreatment
Described 2-KDG zymotic fluid adds the concentrated sulfuric acid in the centrifugal rear gained stillness of night, then under the water bath condition of 50-95 DEG C, in the stillness of night after acidifying, adds active carbon, stirs decolouring; Filtering active carbon after decolouring, gained filtrate is crossed cation exchange resin column, and by the treatment fluid decompression distillation of collecting after cation exchange resin column removal of impurities, obtaining solid content is that 70-90% obtains 2-KDG concentrate;
3) esterification reaction of organic acid
In described 2-KDG concentrate, add methyl alcohol, and using sulfuric acid as catalyst, in 60-100 DEG C of reaction 5-10h, react complete, concentrated, crystallization at 4 DEG C, suction filtration is also dried to obtain 2-KDG methyl esters salt;
4) conversion reaction
Described 2-KDG methyl esters salt is added in methyl alcohol and dissolved, then add methanol-hydrogen sodium oxide molybdena mixed liquor, at 55-70 DEG C, reaction 13-20min then places crystallization at 4 DEG C, and suction filtration obtains the thick sodium salt of D-araboascorbic acid;
5) D-araboascorbic acid sodium is refining
The thick sodium salt of gained D-araboascorbic acid is soluble in water, adds active carbon and oxalic acid, is heated to 50-70 DEG C, insulated and stirred 3-8min, and then suction filtration obtains filtrate while hot; Gained filtrate is cooling, crystallization, suction filtration with the dry D-araboascorbic acid sodium product that to obtain after the washing of 90-100% ethanol.
3. the preparation method who indirectly prepares as claimed in claim 2 D-araboascorbic acid sodium, is characterized in that: in step 1), obtain seed liquor seed culture medium used and consist of peptone 5g/L, sodium chloride 5g/L, beef extract 3g/L, pH value is 7.0; Described fermentation medium consists of glucose 180g/L, corn steep liquor 9.01g/L, potassium dihydrogen sulfate 1g/L, magnesium sulfate 0.4g/L, manganese chloride 0.037g/L, ferrous sulfate 0.036g/L, calcium carbonate 65g/L.
4. the preparation method who indirectly prepares D-araboascorbic acid sodium as described in claim 2 or 3, is characterized in that: step 2) in the addition of the active carbon 5-15% that is solid content, bleaching time is at least 0.5h.
5. indirectly prepare as claimed in claim 2 the preparation method of D-araboascorbic acid sodium, it is characterized in that: step 2) in, described cation exchange resin column is 732# cation exchange resin column, and described cation exchange resin column ratio of height to diameter is 9:1-10:1, flow velocity 1-1.1 per hour times column volume.
6. the preparation method who indirectly prepares as claimed in claim 2 D-araboascorbic acid sodium, is characterized in that, in step 3), the addition of methyl alcohol meets: in every gram of 2-KDG concentrate, add 5-1.5mL methyl alcohol.
7. indirectly prepare as claimed in claim 2 the preparation method of D-araboascorbic acid sodium, it is characterized in that, in step 4), in 2-KDG methyl esters salt, the addition of methyl alcohol meets: in every gram of 2-KDG methyl esters salt, add 10-10.5mL methyl alcohol; The addition of methanol-hydrogen sodium oxide molybdena mixed liquor meets: in every gram of 2-KDG methyl esters salt, add 4-4.5mL methanol-hydrogen sodium oxide molybdena mixed liquor.
8. the preparation method who indirectly prepares as claimed in claim 2 D-araboascorbic acid sodium, is characterized in that, in step 5), the addition of active carbon and oxalic acid is the 0.5%-0.7% of solid content.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108129427A (en) * | 2017-12-29 | 2018-06-08 | 郑州拓洋生物工程有限公司 | ISOASCORBIC ACID potassium and its preparation method and application |
| CN110294726A (en) * | 2019-07-29 | 2019-10-01 | 新拓洋生物工程股份有限公司 | The preparation method of ISOASCORBIC ACID potassium |
| CN110642817A (en) * | 2019-10-22 | 2020-01-03 | 新拓洋生物工程股份有限公司 | Isovitamin C potassium refining method |
| CN111337613A (en) * | 2020-04-18 | 2020-06-26 | 新拓洋生物工程有限公司 | High performance liquid detection method for D-isoascorbic acid potassium |
| CN111909864A (en) * | 2020-06-29 | 2020-11-10 | 山东省食品发酵工业研究设计院 | Method for one-bacterium multiple use of serratia marcescens strain |
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| 秦汝杰等: "异抗坏血酸的制备", 《河南化工》 * |
| 虞炳钧等: "食品抗氧化剂——D-异抗坏血酸钠生产工艺的研究", 《食品与发酵工业》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108129427A (en) * | 2017-12-29 | 2018-06-08 | 郑州拓洋生物工程有限公司 | ISOASCORBIC ACID potassium and its preparation method and application |
| CN110294726A (en) * | 2019-07-29 | 2019-10-01 | 新拓洋生物工程股份有限公司 | The preparation method of ISOASCORBIC ACID potassium |
| CN110642817A (en) * | 2019-10-22 | 2020-01-03 | 新拓洋生物工程股份有限公司 | Isovitamin C potassium refining method |
| CN111337613A (en) * | 2020-04-18 | 2020-06-26 | 新拓洋生物工程有限公司 | High performance liquid detection method for D-isoascorbic acid potassium |
| CN111909864A (en) * | 2020-06-29 | 2020-11-10 | 山东省食品发酵工业研究设计院 | Method for one-bacterium multiple use of serratia marcescens strain |
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