CN105461760A - A method of purifying low-purity galactooligosaccharide - Google Patents
A method of purifying low-purity galactooligosaccharide Download PDFInfo
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- CN105461760A CN105461760A CN201510803656.1A CN201510803656A CN105461760A CN 105461760 A CN105461760 A CN 105461760A CN 201510803656 A CN201510803656 A CN 201510803656A CN 105461760 A CN105461760 A CN 105461760A
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- oligomeric galactose
- described step
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- syrup
- membrane
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- 238000000034 method Methods 0.000 title claims abstract description 21
- 235000021255 galacto-oligosaccharides Nutrition 0.000 title abstract 6
- 150000003271 galactooligosaccharides Chemical class 0.000 title abstract 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000012530 fluid Substances 0.000 claims abstract description 9
- 239000012466 permeate Substances 0.000 claims abstract description 9
- 238000005374 membrane filtration Methods 0.000 claims abstract description 8
- 229930182830 galactose Natural products 0.000 claims description 41
- 239000006188 syrup Substances 0.000 claims description 21
- 235000020357 syrup Nutrition 0.000 claims description 21
- 239000012528 membrane Substances 0.000 claims description 17
- 239000000463 material Substances 0.000 claims description 12
- GUBGYTABKSRVRQ-QKKXKWKRSA-N Lactose Natural products OC[C@H]1O[C@@H](O[C@H]2[C@H](O)[C@@H](O)C(O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@H]1O GUBGYTABKSRVRQ-QKKXKWKRSA-N 0.000 claims description 9
- 239000008101 lactose Substances 0.000 claims description 9
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 8
- 239000008103 glucose Substances 0.000 claims description 8
- -1 polyethylene Polymers 0.000 claims description 4
- 230000008719 thickening Effects 0.000 claims description 4
- 239000004698 Polyethylene Substances 0.000 claims description 3
- 239000001913 cellulose Substances 0.000 claims description 3
- 229920002678 cellulose Polymers 0.000 claims description 3
- 229920002647 polyamide Polymers 0.000 claims description 3
- 229920000573 polyethylene Polymers 0.000 claims description 3
- 229920001721 polyimide Polymers 0.000 claims description 3
- 229920000098 polyolefin Polymers 0.000 claims description 3
- 239000004952 Polyamide Substances 0.000 claims description 2
- 229920002492 poly(sulfone) Polymers 0.000 claims description 2
- 229920006267 polyester film Polymers 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 7
- 239000002002 slurry Substances 0.000 abstract 3
- 150000001720 carbohydrates Chemical class 0.000 abstract 2
- 238000000926 separation method Methods 0.000 description 7
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000000108 ultra-filtration Methods 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 102000004190 Enzymes Human genes 0.000 description 2
- 108090000790 Enzymes Proteins 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 125000002519 galactosyl group Chemical group C1([C@H](O)[C@@H](O)[C@@H](O)[C@H](O1)CO)* 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229910010272 inorganic material Inorganic materials 0.000 description 2
- 239000011147 inorganic material Substances 0.000 description 2
- 229920001542 oligosaccharide Polymers 0.000 description 2
- 150000002482 oligosaccharides Chemical class 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- WQZGKKKJIJFFOK-SVZMEOIVSA-N (+)-Galactose Chemical compound OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@H]1O WQZGKKKJIJFFOK-SVZMEOIVSA-N 0.000 description 1
- 241000193830 Bacillus <bacterium> Species 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 239000004642 Polyimide Substances 0.000 description 1
- 240000000111 Saccharum officinarum Species 0.000 description 1
- 235000007201 Saccharum officinarum Nutrition 0.000 description 1
- 241000700605 Viruses Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 235000013405 beer Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000004440 column chromatography Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003480 eluent Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 235000011389 fruit/vegetable juice Nutrition 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 244000005709 gut microbiome Species 0.000 description 1
- 235000020256 human milk Nutrition 0.000 description 1
- 210000004251 human milk Anatomy 0.000 description 1
- 208000015181 infectious disease Diseases 0.000 description 1
- 230000002458 infectious effect Effects 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 238000010999 medical injection Methods 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000001471 micro-filtration Methods 0.000 description 1
- 235000013336 milk Nutrition 0.000 description 1
- 239000008267 milk Substances 0.000 description 1
- 210000004080 milk Anatomy 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- LPUQAYUQRXPFSQ-DFWYDOINSA-M monosodium L-glutamate Chemical compound [Na+].[O-]C(=O)[C@@H](N)CCC(O)=O LPUQAYUQRXPFSQ-DFWYDOINSA-M 0.000 description 1
- 235000013923 monosodium glutamate Nutrition 0.000 description 1
- 239000004223 monosodium glutamate Substances 0.000 description 1
- 238000001728 nano-filtration Methods 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 230000035790 physiological processes and functions Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000001223 reverse osmosis Methods 0.000 description 1
- 235000019991 rice wine Nutrition 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 235000013555 soy sauce Nutrition 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 150000003538 tetroses Chemical class 0.000 description 1
- 150000004043 trisaccharides Chemical class 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 235000020097 white wine Nutrition 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H3/00—Compounds containing only hydrogen atoms and saccharide radicals having only carbon, hydrogen, and oxygen atoms
- C07H3/06—Oligosaccharides, i.e. having three to five saccharide radicals attached to each other by glycosidic linkages
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Biotechnology (AREA)
- General Health & Medical Sciences (AREA)
- Genetics & Genomics (AREA)
- Molecular Biology (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention relates to a method of purifying low-purity galactooligosaccharide. The method includes (1) preparing commercially available galactooligosaccharide into saccharide slurry by using water, (2) subjecting the galactooligosaccharide slurry to membrane filtration, and respectively collecting permeate and trapped fluid, and (3) concentrating the collected permeate at 50-90 DEG C under vacuum until the concentration of the saccharide slurry is 40-90%. The purity of the galactooligosaccharide is 75% or above by one time of the membrane filtration for the first time, thus overcoming a problem in the prior art that the galactooligosaccharide is low in purity.
Description
Technical field
The present invention relates to a kind of method of low levels oligomeric galactose purifying, belong to sugared industrial technical field.
Background technology
Oligomeric galactose (GOS) is the oligosaccharides of 1-4 galactosyl on the galactosyl side of lactose molecule connects.The foundation of infant's intestinal microflora relies on the oligomeric galactose component in breast milk to a great extent.The oligomeric galactose not still multiplicaiton factor of bifidus bacillus in enteron aisle, also has and improves metabolism of fat, promotes the effects such as calcium absorption.Oligomeric galactose product on current domestic and international market is substantially all with biological enzyme synthesis, and product oligomeric sugar (oligomeric trisaccharide, tetrose and pentasaccharides) content is 24% ~ 57%, also there is the lactose of a great deal of, glucose and a small amount of semi-lactosi.The existence of small molecular sugar greatly reduces the physiological function of oligomeric galactose.Therefore, oligomeric galactose product is purified there is very high economic worth and significance of scientific research.
The method of oligose separating-purifying mainly contains enzyme process, microbe fermentation method, chromatographic column partition method and membrane separation process.The former two consumes small molecular sugar by biotechnology, but reaction may introduce other much new materials, and complicated operation, cost are high.Column chromatography method needs a large amount of eluents, and separation cycle is long, the energy that product needs vacuum-evaporation and at substantial because concentration is low.And the advantage such as membrane separation technique has simple and compact device, high and energy expenditure is low without phase transformation and chemical reaction, selectivity, therefore can adopt membrane technique separation and purification or concentrated various oligosaccharide solution.
Film is the material with selective separation function.According to the performance of ultra-filtration membrane, the material of ultra-filtration membrane can be divided into macromolecular material and the large class of inorganic materials two.Macromolecular material mainly contains cellulose family, poly-maple class, polyamide-based, polyolefine, fluorinated etc.; Inorganic materials mainly contains pottery, metal, glass, molecular sieve etc.The aperture of film is generally micron order, according to the difference (or aperture) of its molecular weight cut-off, film can be divided into microfiltration membrane, ultra-filtration membrane, nanofiltration membrane and reverse osmosis membrane.Ultrafiltration membrane technique both can remove disease caused by infectious water bacterium, virus, thermal source, colloid, etc. objectionable impurities, can to dialyse again inorganic salt, be widely used in milk separation, concentration of juices, yellow rice wine purifying, aging of white wine, beer sterilization, monosodium glutamate purified, the decolouring of sugarcane chaff, amino acid is concentrated, soy sauce is degerming etc. produces, but also be widely used in medical injection water, preparation that transfusion water, bottle-washing water, surgical operation wash clean water.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, optimize and utilize film to carry out the method for separation and purification to oligomeric galactose.
The technical solution used in the present invention is:
A method for low levels oligomeric galactose purifying, comprises the following steps.
(1) commercial oligomeric galactose deionized water boils dissolving, is prepared into certain density syrup.
(2) oligomeric galactose syrup is carried out membrane filtration operation.Collect permeate and trapped fluid respectively.
(3) permeate of collection is carried out at 50-90 DEG C vacuum concentration to syrup concentration 40-90%.
The made syrup mass concentration 20-500g/L of described step (1).In order to improve the speed of filtration, the mass concentration of preferred syrup is 50-80g/L.
Described step (2) material used is macromolecular material, comprises any in cellulose membrane, polyethylene film, polyamide membrane, polysulfone membrane, polyimide film, polyester film, polyolefin film or several combinations.
Temperature during described step (2) operation need adopt lesser temps to avoid feed liquid color and luster to deepen, preferred 15-50 DEG C.
Described step (2) membrane molecule amount 200-2000Da used, preferred 200-1000Da.
Improve working pressure in described step (2) and improve filtration velocity, the scope of working pressure is 0.01Mpa-2.0Mpa, preferred 0.4-0.8Mpa.
Described step (3) described vacuum concentration operation vacuum tightness is 0.01Mpa-0.2Mpa, preferred 0.06-0.1Mpa.
Beneficial effect
1, the present invention adopts method processing requirement simple, and without phase transformation and chemical reaction, safety, reliability is high.
2, non-oligomeric galactose component also reclaims by method provided by the invention, can further develop, and improves the utilising efficiency of resource.
3, the present invention adopts physical method to purify, and avoids creating other impurity in operating process.
Embodiment
Below in conjunction with embodiment, technical scheme of the present invention is further elaborated, but institute of the present invention protection domain is not limited thereto.
Embodiment 1
A method for low levels oligomeric galactose purifying, comprises the following steps:
Commercial available quality concentration 75% oligomeric galactose syrup detects, and detecting oligomeric galactose component in oligomeric galactose syrup is 57.2%, glucose 16.4%, semi-lactosi 11.4%, lactose 15%.Take 1T75% oligomeric galactose syrup and be placed in mixing kettle, adopt deionized water to add water quality of regulation concentration to 10%.The polymeric amide material rolled film equipment of molecular weight 500Da is adopted to carry out filter operation.Service temperature 20-25 DEG C, working pressure 0.4Mpa, collect permeate and trapped fluid respectively.Trapped fluid is carried out vacuum concentration, and concentrated vacuum tightness is-0.1Mpa, and thickening temperature 70 DEG C, is concentrated into mass concentration 70%.
After testing, after membrane filtration is purified the oligomeric galactose component of oligomeric galactose syrup be 78.6%, glucose 1.2%, semi-lactosi 0.3%, lactose 20.3%.
Embodiment 2
A method for low levels oligomeric galactose purifying, comprises the following steps:
Commercial available quality concentration 75% oligomeric galactose syrup detects, and detecting oligomeric galactose component in oligomeric galactose syrup is 58.9%, glucose 17.4%, semi-lactosi 6.4%, lactose 17.3%.Take 500 gram of 75% oligomeric galactose syrup, adopt deionized water to add water quality of regulation concentration to 8%.The polyimide material rolled film equipment of molecular weight 300Da is adopted to carry out filter operation.Service temperature 25-30 DEG C, working pressure 0.6Mpa, collect permeate and trapped fluid respectively.Trapped fluid is carried out vacuum concentration, and concentrated vacuum tightness is-0.07Mpa, and thickening temperature 75 DEG C, is concentrated into mass concentration 75%.
After testing, after membrane filtration is purified the oligomeric galactose component of oligomeric galactose syrup be 76.2%, glucose 0.8%, semi-lactosi 1.1%, lactose 21.9%.
Embodiment 3
A method for low levels oligomeric galactose purifying, comprises the following steps:
Commercial available quality concentration 75% oligomeric galactose syrup detects, and detecting oligomeric galactose component in oligomeric galactose syrup is 58.2%, glucose 19.4%, semi-lactosi 9.5%, lactose 12.9%.Take 600 grams of oligomeric galactose syrup, adopt deionized water to add water quality of regulation concentration to 12%.The polyethylene material rolled film equipment of molecular weight 1000Da is adopted to carry out filter operation.Service temperature 30-35 DEG C, working pressure 0.5Mpa, collect permeate and trapped fluid respectively.Trapped fluid is carried out vacuum concentration, and concentrated vacuum tightness is-0.09Mpa, and thickening temperature 65-68 DEG C, is concentrated into mass concentration 75%.
After testing, after membrane filtration is purified the oligomeric galactose component of oligomeric galactose syrup be 76.6%, glucose 1.7%, semi-lactosi 0.5%, lactose 21.2%.
Claims (8)
1. a method for low levels oligomeric galactose purifying, is characterized in that, comprises the following steps:
(1) commercial oligomeric galactose spends ionized water and is prepared into certain density syrup;
(2) oligomeric galactose syrup is carried out membrane filtration operation, collect permeate and trapped fluid respectively;
(3) permeate of collection is carried out at 50-90 DEG C vacuum concentration to syrup concentration 40-90%.
2. production method as claimed in claim 1, is characterized in that, in described step (1), low levels oligomeric galactose component comprises the non-oligomeric galactose components such as glucose, semi-lactosi, lactose.
3. production method as claimed in claim 1, is characterized in that, oligomeric galactose syrup concentration 20-500g/L in described step (1).
4. production method as claimed in claim 1, is characterized in that, in described step (2), service temperature is 10-75 DEG C.
5. production method as claimed in claim 1, is characterized in that, working pressure 0.01-1.6MPa in described step (2).
6. production method as claimed in claim 1, is characterized in that, in described step (2), membrane filtration precision is molecular weight 200-5000Da.
7. production method as claimed in claim 1, it is characterized in that, core rod material macromolecular material in described step (2), comprises any in cellulose membrane, polyethylene film, polyamide membrane, polysulfone membrane, polyimide film, polyester film, polyolefin film or several combinations.
8. production method as claimed in claim 1, is characterized in that, in described step (3), thickening temperature is 40-90 DEG C, and vacuum tightness is 0.01Mpa-0.2Mpa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510803656.1A CN105461760A (en) | 2015-11-20 | 2015-11-20 | A method of purifying low-purity galactooligosaccharide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510803656.1A CN105461760A (en) | 2015-11-20 | 2015-11-20 | A method of purifying low-purity galactooligosaccharide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105461760A true CN105461760A (en) | 2016-04-06 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510803656.1A Pending CN105461760A (en) | 2015-11-20 | 2015-11-20 | A method of purifying low-purity galactooligosaccharide |
Country Status (1)
| Country | Link |
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| CN (1) | CN105461760A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02195894A (en) * | 1989-01-24 | 1990-08-02 | Nitto Denko Corp | Production of galacto-oligosaccharide |
| WO2009113030A2 (en) * | 2008-03-12 | 2009-09-17 | Tata Chemicals Ltd. | Process for the production of galactooligosaccharides by free cells |
| CN101781371A (en) * | 2009-12-02 | 2010-07-21 | 烟台大学 | Galactooligosaccharides economic purification method |
| CN104004799A (en) * | 2014-06-12 | 2014-08-27 | 南京工业大学 | Method for continuously preparing galacto-oligosaccharide |
-
2015
- 2015-11-20 CN CN201510803656.1A patent/CN105461760A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02195894A (en) * | 1989-01-24 | 1990-08-02 | Nitto Denko Corp | Production of galacto-oligosaccharide |
| WO2009113030A2 (en) * | 2008-03-12 | 2009-09-17 | Tata Chemicals Ltd. | Process for the production of galactooligosaccharides by free cells |
| CN101781371A (en) * | 2009-12-02 | 2010-07-21 | 烟台大学 | Galactooligosaccharides economic purification method |
| CN104004799A (en) * | 2014-06-12 | 2014-08-27 | 南京工业大学 | Method for continuously preparing galacto-oligosaccharide |
Non-Patent Citations (1)
| Title |
|---|
| 冯咏梅: "膜技术分离纯化低聚半乳糖", 《精细化工》 * |
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Application publication date: 20160406 |
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