CN108640953A - Using macroreticular resin to the process for purification of pumpkin oligosaccharide - Google Patents
Using macroreticular resin to the process for purification of pumpkin oligosaccharide Download PDFInfo
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- CN108640953A CN108640953A CN201810394655.XA CN201810394655A CN108640953A CN 108640953 A CN108640953 A CN 108640953A CN 201810394655 A CN201810394655 A CN 201810394655A CN 108640953 A CN108640953 A CN 108640953A
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- Prior art keywords
- pumpkin
- oligosaccharide
- resin
- macroreticular resin
- washed
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- 239000011347 resin Substances 0.000 title claims abstract description 130
- 229920005989 resin Polymers 0.000 title claims abstract description 130
- 150000002482 oligosaccharides Chemical class 0.000 title claims abstract description 113
- 235000009854 Cucurbita moschata Nutrition 0.000 title claims abstract description 111
- 240000001980 Cucurbita pepo Species 0.000 title claims abstract description 111
- 229920001542 oligosaccharide Polymers 0.000 title claims abstract description 111
- 235000000832 Ayote Nutrition 0.000 title claims abstract description 108
- 235000009804 Cucurbita pepo subsp pepo Nutrition 0.000 title claims abstract description 108
- 235000015136 pumpkin Nutrition 0.000 title claims abstract description 108
- 238000000034 method Methods 0.000 title claims abstract description 57
- 238000000746 purification Methods 0.000 title claims abstract description 39
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 99
- 235000019441 ethanol Nutrition 0.000 claims abstract description 49
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000000287 crude extract Substances 0.000 claims abstract description 22
- 239000000049 pigment Substances 0.000 claims abstract description 19
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000008367 deionised water Substances 0.000 claims abstract description 11
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 11
- 238000001704 evaporation Methods 0.000 claims abstract description 7
- 230000008020 evaporation Effects 0.000 claims abstract description 7
- 239000006228 supernatant Substances 0.000 claims description 18
- 238000010828 elution Methods 0.000 claims description 13
- 239000002250 absorbent Substances 0.000 claims description 9
- 230000002745 absorbent Effects 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 9
- 238000010521 absorption reaction Methods 0.000 claims description 8
- 238000000108 ultra-filtration Methods 0.000 claims description 8
- 238000002360 preparation method Methods 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 6
- 238000001728 nano-filtration Methods 0.000 claims description 6
- 238000003809 water extraction Methods 0.000 claims description 6
- 239000012141 concentrate Substances 0.000 claims description 5
- 239000000706 filtrate Substances 0.000 claims description 4
- 239000006058 strengthened glass Substances 0.000 claims description 4
- 239000003480 eluent Substances 0.000 claims description 3
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims description 2
- 239000003456 ion exchange resin Substances 0.000 claims description 2
- 229920003303 ion-exchange polymer Polymers 0.000 claims description 2
- 239000012467 final product Substances 0.000 claims 1
- 150000002772 monosaccharides Chemical class 0.000 abstract description 9
- 239000012535 impurity Substances 0.000 abstract description 8
- 102000004169 proteins and genes Human genes 0.000 abstract description 6
- 108090000623 proteins and genes Proteins 0.000 abstract description 6
- 238000004108 freeze drying Methods 0.000 abstract description 5
- 238000012545 processing Methods 0.000 abstract description 4
- 239000002253 acid Substances 0.000 abstract description 3
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 abstract description 2
- 230000015556 catabolic process Effects 0.000 abstract description 2
- 238000006731 degradation reaction Methods 0.000 abstract description 2
- 235000000346 sugar Nutrition 0.000 description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 238000004042 decolorization Methods 0.000 description 5
- 238000001514 detection method Methods 0.000 description 4
- 238000001179 sorption measurement Methods 0.000 description 4
- 235000009852 Cucurbita pepo Nutrition 0.000 description 3
- 235000008504 concentrate Nutrition 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- 238000004128 high performance liquid chromatography Methods 0.000 description 3
- 239000012528 membrane Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 235000020354 squash Nutrition 0.000 description 3
- 239000003643 water by type Substances 0.000 description 3
- 239000003463 adsorbent Substances 0.000 description 2
- 230000000675 anti-caries Effects 0.000 description 2
- 239000008280 blood Substances 0.000 description 2
- 210000004369 blood Anatomy 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000004587 chromatography analysis Methods 0.000 description 2
- 238000004040 coloring Methods 0.000 description 2
- 239000012043 crude product Substances 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 238000002845 discoloration Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000012869 ethanol precipitation Methods 0.000 description 2
- 150000004676 glycans Chemical class 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 239000002808 molecular sieve Substances 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 229920001282 polysaccharide Polymers 0.000 description 2
- 239000005017 polysaccharide Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 206010012735 Diarrhoea Diseases 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 235000014633 carbohydrates Nutrition 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- HVYWMOMLDIMFJA-DPAQBDIFSA-N cholesterol Chemical compound C1C=C2C[C@@H](O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@H](C)CCCC(C)C)[C@@]1(C)CC2 HVYWMOMLDIMFJA-DPAQBDIFSA-N 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 229930003935 flavonoid Natural products 0.000 description 1
- 150000002215 flavonoids Chemical class 0.000 description 1
- 235000017173 flavonoids Nutrition 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000013538 functional additive Substances 0.000 description 1
- 235000013376 functional food Nutrition 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 230000002496 gastric effect Effects 0.000 description 1
- 210000004051 gastric juice Anatomy 0.000 description 1
- 229930182478 glucoside Natural products 0.000 description 1
- 150000008131 glucosides Chemical class 0.000 description 1
- 235000001497 healthy food Nutrition 0.000 description 1
- 230000031891 intestinal absorption Effects 0.000 description 1
- 210000002429 large intestine Anatomy 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005360 mashing Methods 0.000 description 1
- 230000009149 molecular binding Effects 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 244000052769 pathogen Species 0.000 description 1
- 230000001717 pathogenic effect Effects 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 230000035755 proliferation Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 150000008163 sugars Chemical class 0.000 description 1
- 235000019605 sweet taste sensations Nutrition 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- 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
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L5/00—Preparation or treatment of foods or foodstuffs, in general; Food or foodstuffs obtained thereby; Materials therefor
- A23L5/40—Colouring or decolouring of foods
- A23L5/42—Addition of dyes or pigments, e.g. in combination with optical brighteners
- A23L5/43—Addition of dyes or pigments, e.g. in combination with optical brighteners using naturally occurring organic dyes or pigments, their artificial duplicates or their derivatives
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P1/00—Drugs for disorders of the alimentary tract or the digestive system
- A61P1/02—Stomatological preparations, e.g. drugs for caries, aphtae, periodontitis
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P3/00—Drugs for disorders of the metabolism
- A61P3/08—Drugs for disorders of the metabolism for glucose homeostasis
- A61P3/10—Drugs for disorders of the metabolism for glucose homeostasis for hyperglycaemia, e.g. antidiabetics
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P39/00—General protective or antinoxious agents
- A61P39/06—Free radical scavengers or antioxidants
-
- 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
- C07H3/04—Disaccharides
-
- 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
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0024—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid beta-D-Glucans; (beta-1,3)-D-Glucans, e.g. paramylon, coriolan, sclerotan, pachyman, callose, scleroglucan, schizophyllan, laminaran, lentinan or curdlan; (beta-1,6)-D-Glucans, e.g. pustulan; (beta-1,4)-D-Glucans; (beta-1,3)(beta-1,4)-D-Glucans, e.g. lichenan; Derivatives thereof
- C08B37/0027—2-Acetamido-2-deoxy-beta-glucans; Derivatives thereof
- C08B37/003—Chitin, i.e. 2-acetamido-2-deoxy-(beta-1,4)-D-glucan or N-acetyl-beta-1,4-D-glucosamine; Chitosan, i.e. deacetylated product of chitin or (beta-1,4)-D-glucosamine; Derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B61/00—Dyes of natural origin prepared from natural sources, e.g. vegetable sources
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
Abstract
Refined method carries out pumpkin oligosaccharide using macroreticular resin the invention discloses a kind of, step includes：Add water to be made into pumpkin oligosaccharide upper prop solution pumpkin oligosaccharide crude extract, adsorbed by the chromatographic column equipped with macroreticular resin, collects efflux；It stands, macroreticular resin is eluted with deionized water, be concentrated by evaporation, freeze-drying, obtain colourless pumpkin oligosaccharide；It is washed using ethanol solution, is impregnated using ethyl alcohol, NaOH solution is by resin column and impregnates, and is washed to neutrality；It by resin column and is impregnated using hydrochloric acid, recycles macroreticular resin；Revolving evaporation and freeze-drying, recycle foreign pigment and ethyl alcohol.The process for purification can remove monosaccharide and protein impurities simultaneously while reaching pumpkin oligosaccharide efficient decolorizing, and the purity of gained pumpkin oligosaccharide is up to 95~96%；And the process mild condition, should not high temperature or soda acid processing, without causing the degradation of pumpkin oligosaccharide, gained foreign pigment melanoidin that can recycle.
Description
Technical field
The invention belongs to the technical field of purification of pumpkin oligosaccharide, and in particular to a kind of oligomeric to pumpkin using macroreticular resin
The process for purification of sugar.
Background technology
Numerous studies have demonstrated that the functional sugars ingredient such as polysaccharide, oligosaccharide in pumpkin has the function of blood glucose-control, and
The functional sugar is also widely approved as a kind of ingredient of natural botanical source, safety.Oligosaccharide
(oligosaccharide) and oligosaccharides is can be described as, is the minuent by 2-10 monosaccharide by glucosides key connection at linear chain or branched chain
Polymerization sugar, molecular weight is between 200~3000D.Due to monosaccharide molecule binding site and bond type difference, it is rich to form type
Rich oligosaccharide.Oligosaccharide has good functional characteristic, can be used as sweet taste source, but do not degraded by human body hydrochloric acid in gastric juice, gastric enzyme, does not exist
Intestinal absorption, into large intestine after selectively promote the proliferation of beneficial bacterium and inhibit pathogen and diarrhea, also protect liver, reduce
The functions such as serum cholesterol, anti-caries tooth.Oligosaccharide is because its unique functional characteristic is concerned, and future is in functional food, feed
There are good researching value and application potential with fields such as additives.
Currently, mostly using water extraction and alcohol precipitation method prepares squash polyoses, in separation process in macromolecular polysaccharide supernatants after precipitation
Still contain a large amount of carbohydrate, thus it is speculated that be the lower oligosaccharide of molecular weight.Supernatant is generally efficiently separated using membrane filter method
In pumpkin oligosaccharide crude product, however product be in dark brown brown, be by pumpkin pigment and process in generate it is coloured
Impurity causes, and obstacle is caused to the purifying of pumpkin oligosaccharide, structural research and industrial applications.
Common discoloration method has in the food industry at present, such as organic solvent decoloring method, activated carbon decolorizing method, activated carbon
Adsorption decoloring method, hydrogen peroxide for decoloration method.It is low, broken that there are decolorizing efficiencies when however, these methods being decolourized applied to pumpkin oligosaccharide
Bad oligosaccharide structures such as hydrogen peroxide oxidation destroys the problems such as sugar chain, operation cost are high and recycling is difficult.Therefore, it studies a kind of high
Effect, the pumpkin oligosaccharide decoloration of environmental protection, impurity-removing method are of great significance.
Macroreticular resin has been developed in recent years a kind of organic polymer adsorbent, is decolourized for natural extract
Effective ways.Compared with traditional discoloration method, macroreticular resin decoloring method has easy to operate, and separative efficiency is high, is easily recycled, at
This is low and pollutes the features such as small.
Invention content
The purpose of the present invention is to provide a kind of using macroreticular resin to the process for purification of pumpkin oligosaccharide, existing to overcome
There is in pumpkin oligosaccharide the shortcomings that coloring matter decolorizing effect is poor, removal of impurity is low, destruction oligosaccharide structures.
To realize said one or multiple purposes, in one embodiment of the invention, the present invention provides one kind to adopt
With macroreticular resin to the process for purification of pumpkin oligosaccharide, include the following steps：
(1) pumpkin oligosaccharide crude extract is added into water, is made into pumpkin oligosaccharide upper prop solution；By 0.8~1.5 times of column volume
(BV) the pumpkin oligosaccharide upper prop solution carries out upper prop absorption by the chromatographic column equipped with macroreticular resin, then collects outflow
Liquid；
(2) it stands, then macroreticular resin is eluted with deionized water, by remaining pumpkin oligosaccharide eluent and step in column
(1) gained efflux merges in, is then concentrated by evaporation, is lyophilized, obtains colourless pumpkin oligosaccharide；
(3) foreign pigment on the ethanol solution elution absorption macroreticular resin of 1.5~2.2BV is used；It is impregnated using ethyl alcohol,
It is washed with water to no alcohol taste, by resin column and is impregnated using NaOH solution, be washed to neutrality；Then resin column is passed through using hydrochloric acid
And impregnate, it is washed to neutrality, recycles macroreticular resin；Finally, it evaporates and is freeze-dried through revolving, recycle foreign pigment and ethyl alcohol.
In above-mentioned process for purification, the part monosaccharide and albumen in pumpkin oligosaccharide crude extract can be removed by macroreticular resin
Matter.Specifically removal principle is：It is acted on by the molecular sieve of macroreticular resin so that the different oligosaccharide of molecular weight and monosaccharide are divided
From；It is different with physics, chemical property further according to protein and the sugared structure of itself, lead to the albumen in pumpkin oligosaccharide crude extract
The absorption on macroreticular resin of matter and oligosaccharide, elution property are different so that partially protein is removed；In short, by big
Macroporous adsorbent resin finally eliminates part monosaccharide and protein in pumpkin oligosaccharide.
In a preferred embodiment of the invention, the present invention provides a kind of using macroreticular resin to pumpkin oligosaccharide
Process for purification, the mass percent concentration of pumpkin oligosaccharide upper prop solution described in above-mentioned steps (1) is 230~280mg/
ml；
And/or the pumpkin oligosaccharide upper prop solution passes through the layer equipped with macroreticular resin with the flow velocity of 0.8~1.5BV/h
Analyse column.
In the case that wherein, macroreticular resin amount is certain, loading flow velocity is slow, applied sample amount is few experimental group and elution speed be slow,
It is more preferable to elute the big experimental group decolorizing effect of liquid measure, but speed is excessively slow and measured conference and leads to cost increase.
In a preferred embodiment of the invention, the present invention provides a kind of using macroreticular resin to pumpkin oligosaccharide
Process for purification, using preceding being pre-processed, concrete operations are macroreticular resin described in above-mentioned steps (1)：First using go from
Sub- water impregnates macroreticular resin, is washed till with ethyl alcohol not muddy；Then it is impregnated, is washed with deionized water to no alcohol taste with ethyl alcohol；Matter is used again
The NaOH solution that amount percent concentration is 5% by resin column and impregnates resin, is washed to neutrality, is by mass percent concentration
5% hydrochloric acid is by resin column and impregnates resin, is finally washed to neutral to get to the macroreticular resin handled well.
In a preferred embodiment of the invention, the present invention provides a kind of using macroreticular resin to pumpkin oligosaccharide
Process for purification, in above-mentioned pretreatment, using deionized water impregnate and ethyl alcohol impregnate time be 20~30h.
In a preferred embodiment of the invention, the present invention provides a kind of using macroreticular resin to pumpkin oligosaccharide
Process for purification, in above-mentioned pretreatment, resin impregnated using NaOH solution or be 1~4h using time of salt acid soak resin.
In a preferred embodiment of the invention, the present invention provides a kind of using macroreticular resin to pumpkin oligosaccharide
Process for purification, in above-mentioned steps (2), the time of the standing is 45~60min；
And/or the deionized water elutes macroreticular resin with the speed of 1.0~3.0BV/h.
In a preferred embodiment of the invention, the present invention provides a kind of using macroreticular resin to pumpkin oligosaccharide
Process for purification, the concentration of volume percent of ethanol solution is 60~80% described in above-mentioned steps (3).
In a preferred embodiment of the invention, the present invention provides a kind of using macroreticular resin to pumpkin oligosaccharide
Process for purification, the macroreticular resin is selected from ion exchange resin, one or both of non-polar macroporous resin, preferably right and wrong
Polar macroporous resin.
In a preferred embodiment of the invention, the present invention provides a kind of using macroreticular resin to pumpkin oligosaccharide
Process for purification, the non-polar macroporous resin in DM21 types macroporous absorbent resin, DM28 type macroporous absorbent resins one
Kind is several.
In a preferred embodiment of the invention, the present invention provides a kind of using macroreticular resin to pumpkin oligosaccharide
Process for purification, the material of the chromatographic column is strengthened glass, and specification is 6cm × 80cm；
And/or the macroreticular resin is packed at the 3/4 of chromatographic column when using.
In a preferred embodiment of the invention, the present invention provides a kind of using macroreticular resin to pumpkin oligosaccharide
Process for purification, it is 1: 10 that resin ratio of height to diameter is packed into the chromatographic column.Wherein, in the case of macroreticular resin amount is certain, chromatographic column
Ratio of height to diameter is big, is conducive to remove monosaccharide impurity.
In a preferred embodiment of the invention, the present invention provides a kind of using macroreticular resin to pumpkin oligosaccharide
Process for purification, the preparation method of pumpkin oligosaccharide crude extract described in above-mentioned steps (1) includes：
(1) by pumpkin remove seed, stripping and slicing, water is added to be beaten, hot water extraction, centrifuging and taking supernatant is concentrated into former supernatant volume
1/2~1/5, obtain concentrate；
(2) ethyl alcohol is added to be precipitated, centrifuging and taking supernatant；
(3) supernatant is diluted to and is crossed 20 μm of filter bags, filtrate first passes through ultrafiltration section, and ultrafiltration retaining molecular weight is
3000Da, permeate are 300Da by nanofiltration section, nanofiltration retaining molecular weight, and it is pumpkin oligosaccharide crude extract to be trapped liquid.
In a preferred embodiment of the invention, the present invention provides a kind of using macroreticular resin to pumpkin oligosaccharide
Process for purification, in the preparation method of above-mentioned pumpkin oligosaccharide crude extract, the temperature of hot water is 80~90 DEG C in step (1), institute
The time for stating hot water extraction is 1~3h.
In a preferred embodiment of the invention, the present invention provides a kind of using macroreticular resin to pumpkin oligosaccharide
Process for purification, in the preparation method of above-mentioned pumpkin oligosaccharide crude extract, the percent by volume of ethanol solution described in step (2)
A concentration of 70~90%, preferably 80%.
In a preferred embodiment of the invention, the present invention provides a kind of using macroreticular resin to pumpkin oligosaccharide
Process for purification, in the preparation method of above-mentioned pumpkin oligosaccharide crude extract, ethanol solution described in step (2) and step (1) institute
The volume ratio for obtaining concentrate is 2~5: 1.
Compared with prior art, the present invention has the advantages that：
(1) macroporous adsorption resin technology is applied in the production technology of pumpkin oligosaccharide by the present invention, macroporous resin adsorption
Foreign pigment in solution, since molecular sieve effect also has certain removal to make the monosaccharide impurity in pumpkin oligosaccharide crude product
With while reaching pumpkin oligosaccharide efficient decolorizing, monosaccharide and protein impurities can be removed simultaneously, and recoverable is coloured miscellaneous
Matter；The purity of gained pumpkin oligosaccharide is high, and up to 94~96%, it is found without apparent impurity, into one through high performance liquid chromatography detection
Step improves the quality of the oligomeric sugar product of pumpkin.
(2) in the process for purification that the present invention uses, pH value need not have been adjusted both when preparing pumpkin oligosaccharide upper prop solution
Its impurity and color can efficiently be removed；The waste that the process for purification treatment conditions of the present invention are mild, low energy consumption, generate is few,
In macroreticular resin decolorization, should not high temperature or soda acid processing, without causing the degradation of pumpkin oligosaccharide, and by before refined
The infrared spectrum of pumpkin oligosaccharide compares it can be proved that the structure of principal component oligosaccharide does not change afterwards.
(3) foreign pigment that process for purification of the invention is removed is that Maillard reaction produces in pumpkin oligosaccharide extraction process
It is de- can to collect oligosaccharide compared with traditional activated carbon decolorizing and hydrogen peroxide decoloring method respectively for raw coloring matter melanoidin
Color liquid (washing) and foreign pigment eluent (70% ethyl alcohol is washed), while retaining the structure feature and property of oligosaccharide itself
Colored component (rate of recovery 79%) can be recycled；In addition, since the color product melanoidin of Maillard reaction is in some researchs
Report has anti-oxidant, anti-caries and a blood glucose-control effect, thus the colored component that recycles of the present invention in healthy food material and
There is preferable application prospect in terms of functional additive.
Description of the drawings
Attached drawing described herein is used to provide further understanding of the present invention, and is constituted part of this application.Attached
In figure：
Fig. 1 is the comparison of the refined front and back color of pumpkin oligosaccharide solution according to the present invention.
Fig. 2 is the high-efficient liquid phase chromatogram of the pumpkin oligosaccharide solution molecular weight detection of 1 gained according to embodiments of the present invention
(HPLC)。
Fig. 3 is the pumpkin oligosaccharide solution ultraviolet-visible light full wavelength scanner figure of 2 gained according to embodiments of the present invention.
Fig. 4 is the pumpkin oligosaccharide solution infrared spectrogram of 1 gained according to embodiments of the present invention.
Specific implementation mode
Below in conjunction with the accompanying drawings, the specific implementation mode of the present invention is described in detail, it is to be understood that the guarantor of the present invention
Shield range is not restricted by specific implementation.
Experimental method used in following embodiments is conventional method unless otherwise specified.
Material used in above-described embodiment, reagent etc., are commercially available unless otherwise specified.
The experimental facilities and condition that ultraviolet-visible full wavelength scanner uses：Ultraviolet-visible spectrophotometer UV-
visspectrophotometer(T6-1650E)。
The experimental facilities and condition that molecular weight high performance liquid chromatography uses：German Nore Knauer high performance liquid chromatographs,
Sample size 20ul, detection time 20min, sample introduction concentration 1%, 38 DEG C of column temperature.
The experimental facilities and condition that infrared spectrum uses：Fourier infrared spectrograph Nicolet 6700FTIR
spectrometer(Madison,WI,U.S.A)。
Embodiment 1
It is a kind of using macroreticular resin to the process for purification of pumpkin oligosaccharide, carry out in accordance with the following steps：
(1) macroreticular resin pre-processes：DM28 types macroporous absorbent resin is impregnated for 24 hours using deionized water, is washed till not with ethyl alcohol
Muddiness, ethyl alcohol are impregnated for 24 hours, are washed with water to no alcohol taste, and the NaOH solution for being 5% with mass percent concentration by resin column and is soaked
2h is steeped, neutrality is washed to, the HCl that mass percent concentration is 5% by resin column and is impregnated into 4h, is washed to neutrality, 4 DEG C standby
With；It is packed at chromatographic column (6cm × 80cm) 3/4 when use, it is ensured that uniform filling is smooth and bubble-free；
(2) water is added to be made into the solution of a concentration of 250mg/ml pumpkin oligosaccharide crude extract, by 1.0 times of column volumes (BV)
Above-mentioned solution, by the chromatographic column equipped with macroreticular resin, is carried out upper prop absorption, then collects efflux with the flow velocity of 1.0BV/h；
(3) after pumpkin oligosaccharide solution all by the splitter equipped with macroreticular resin after, stand 50min, then use
2.0BV deionized waters have adsorbed the macroreticular resin of foreign pigment with the speed elution of 1.5BV/h, and remaining pumpkin in column is oligomeric
Sugar elution is concentrated by evaporation after merging with efflux obtained by step (2), and colourless pumpkin oligosaccharide is obtained after freeze-drying；
(4) ethanol solution that the concentration of volume percent for reusing 2.0BV is 70% will be adsorbed on the speed of 1.5BV/h
Foreign pigment elution on macroreticular resin；
(5) macroreticular resin clean and reuse is carried out after the completion of operation every time, is impregnated for 24 hours, is washed with water to no alcohol taste using ethyl alcohol,
2h by resin column and is impregnated using 5%NaOH solution, is washed to neutrality, 5%HCl is by resin column and impregnates 2h, is washed to
Neutrality recycles macroreticular resin；Finally, it evaporates and is freeze-dried using revolving, recycle foreign pigment and ethyl alcohol.
The preparation method of above-mentioned pumpkin oligosaccharide crude extract includes：By pumpkin remove seed, stripping and slicing, the water of 2~5 times of weight is added to beat
Slurry, uses temperature for 85 DEG C of hot water extraction 2h, and centrifuging and taking supernatant is concentrated into the 1/2 of former supernatant volume；
Then, 2 times of 80% ethanol precipitations of volume, centrifuging and taking supernatant is added；Supernatant after extraction squash polyoses is dilute
It releases and crosses 20 μm of filter bags；
Filtrate first passes through ultrafiltration section, and ultrafiltration retaining molecular weight is 3000Da, then passes through nanofiltration section, NF membrane retention point
Son amount is 300Da, and it is pumpkin oligosaccharide crude extract to be trapped liquid.
Big pore resin model is DM28 type macroporous absorbent resins in implementation；Chromatography column material is strengthened glass, specification
For (6cm × 80cm), it is 1: 10 to be packed into resin blade diameter length ratio；After the chromatographic column equipped with macroreticular resin, quiescent time is
55min。
The refined front and back color contrast of pumpkin oligosaccharide solution manufactured in the present embodiment is as shown in Figure 1, refined by macroreticular resin
After processing, the percent of decolourization of pumpkin oligosaccharide reaches 92.6%, and color contrast can be seen that by macroporous absorbent resin from Fig. 1
After processing, dark brown solution becomes close to transparent solution, and therefore, the process for purification of this implementation achieves preferable decoloration effect
Fruit.
According to fig. 2 shown in the high-efficient liquid phase chromatogram of 1 gained pumpkin oligosaccharide solution molecular weight detection of middle embodiment, by essence
The molecular weight distribution of pumpkin oligosaccharide solution concentrates on 1000~1300Da after system, and molecular weight ranges belong to the molecular weight of oligosaccharide distribution
Range, purity 96%, percent of decolourization 92.4%.
Show the front and back pumpkin oligosaccharide of decoloration according to the infrared spectrogram of 1 gained pumpkin oligosaccharide solution of embodiment in Fig. 4
The chemical constitution of key component illustrates that Flavonoids by Macroporous Adsorption Resin will not be to pumpkin oligosaccharide in subtractive process without significant difference
Structure damages, and can protect the functional group in pumpkin oligosaccharide well.
Embodiment 2
It is a kind of using macroreticular resin to the process for purification of pumpkin oligosaccharide, carry out in accordance with the following steps：
(1) macroreticular resin pre-processes：DM21 type macroporous absorbent resin 30h are impregnated using deionized water, are washed till not with ethyl alcohol
Muddiness, ethyl alcohol impregnate 30h, are washed with water to no alcohol taste, and the NaOH solution for being 5% with mass percent concentration by resin column and is soaked
4h is steeped, neutrality is washed to, the HCl that mass percent concentration is 5% by resin column and is impregnated into 4h, is washed to neutrality, 4 DEG C standby
With；It is packed at the 3/4 of chromatographic column when use, it is ensured that uniform filling is smooth and bubble-free；
(2) water is added to be made into the solution of a concentration of 280mg/ml pumpkin oligosaccharide crude extract, by 1.5 times of column volumes (BV)
Above-mentioned solution, by the chromatographic column equipped with macroreticular resin, is carried out upper prop absorption, then collects efflux with the flow velocity of 1.5BV/h；
(3) after pumpkin oligosaccharide solution all by the splitter equipped with macroreticular resin after, stand 60min, then use
2.5BV deionized waters have adsorbed the macroreticular resin of foreign pigment with the speed elution of 1.0BV/h, and remaining pumpkin in column is oligomeric
Sugar elution is concentrated by evaporation after merging with efflux obtained by step (2), and colourless pumpkin oligosaccharide is obtained after freeze-drying；
(4) ethanol solution that the concentration of volume percent for reusing 2.2BV is 80% will be adsorbed on the speed of 1.0BV/h
Foreign pigment elution on macroreticular resin；
(5) macroreticular resin clean and reuse is carried out after the completion of operation every time, is impregnated for 24 hours, is washed with water to no alcohol taste using ethyl alcohol,
4h by resin column and is impregnated using 5%NaOH solution, is washed to neutrality, 5%HCl is by resin column and impregnates 4h, is washed to
It is neutral；Finally, macroreticular resin is recycled；Finally, it evaporates and is freeze-dried using revolving, recycle foreign pigment and ethyl alcohol.
The preparation method of above-mentioned pumpkin oligosaccharide crude extract includes：By pumpkin remove seed, stripping and slicing, add the water mashing of 5 times of weight,
Then row uses hot water extraction 2h at a temperature of 90 °C, centrifuging and taking supernatant is concentrated into the 1/5 of former supernatant volume；
Then, 5 times of 80% ethanol precipitations of volume, centrifuging and taking supernatant is added；Supernatant after extraction squash polyoses is dilute
It releases and crosses 20 μm of filter bags；
Filtrate first passes through ultrafiltration section, and ultrafiltration retaining molecular weight is 3000Da, then passes through nanofiltration section, NF membrane retention point
Son amount is 300Da, and it is pumpkin oligosaccharide crude extract to be trapped liquid.
Big pore resin model is DM21 type macroporous absorbent resins in this implementation；Chromatography column material is strengthened glass, rule
Lattice are 6cm × 80cm, and it is 1: 10 to be packed into resin blade diameter length ratio；After the chromatographic column equipped with macroreticular resin, quiescent time is
50min。
Pumpkin oligosaccharide percent of decolourization manufactured in the present embodiment is 89.1%, purity 95%, and pumpkin according to Fig.3,
The front and back ultraviolet-visible spectrum comparison of oligosaccharide solution decoloration is it is found that absorbing proteins peak declines at 280nm, therefore, the present embodiment
2 can remove the albumen in pumpkin oligosaccharide crude extract.
Embodiment 3
The pumpkin oligosaccharide crude extract that the present embodiment uses for embodiment 1 in pumpkin oligosaccharide crude extract obtained.
It is a kind of using macroreticular resin to the process for purification of pumpkin oligosaccharide, carry out in accordance with the following steps：
(1) macroreticular resin pre-processes：DM28 type macroporous absorbent resin 20h are impregnated using deionized water, are washed till not with ethyl alcohol
Muddiness, ethyl alcohol impregnate 20h, are washed with water to no alcohol taste, and the NaOH solution for being 5% with mass percent concentration by resin column and is soaked
1h is steeped, neutrality is washed to, the HCl that mass percent concentration is 5% by resin column and is impregnated into 1h, is washed to neutrality, 4 DEG C standby
With；It is packed at chromatographic column (6cm × 80cm) 3/4 when use, it is ensured that uniform filling is smooth and bubble-free；
(2) water is added to be made into the solution of a concentration of 230mg/ml pumpkin oligosaccharide crude extract, by 0.8 times of column volume (BV)
Above-mentioned solution, by the chromatographic column equipped with macroreticular resin, is carried out upper prop absorption, then collects efflux with the flow velocity of 0.8BV/h；
(3) after pumpkin oligosaccharide solution all by the splitter equipped with macroreticular resin after, stand 45min, then use
1.5BV deionized waters have adsorbed the macroreticular resin of foreign pigment with the speed elution of 1.0BV/h, and remaining pumpkin in column is oligomeric
Sugar elution is concentrated by evaporation after merging with efflux obtained by step (2), and colourless pumpkin oligosaccharide is obtained after freeze-drying；
(4) ethanol solution that the concentration of volume percent for reusing 2.2BV is 60% will be adsorbed on the speed of 1.5BV/h
Foreign pigment elution on macroreticular resin；
(5) macroreticular resin clean and reuse is carried out after the completion of operation every time, is impregnated for 24 hours, is washed with water to no alcohol taste using ethyl alcohol,
2h by resin column and is impregnated using 5%NaOH solution, is washed to neutrality, 5%HCl is by resin column and impregnates 2h, is washed to
Neutrality recycles macroreticular resin；Finally, it evaporates and is freeze-dried using revolving, recycle foreign pigment and ethyl alcohol.
Pumpkin oligosaccharide percent of decolourization manufactured in the present embodiment is 88.6%, purity 94%.
The description of the aforementioned specific exemplary embodiment to the present invention is in order to illustrate and illustration purpose.These descriptions
It is not wishing to limit the invention to disclosed precise forms, and it will be apparent that according to the above instruction, can much be changed
And variation.The purpose of selecting and describing the exemplary embodiment is that explaining the specific principle of the present invention and its actually answering
With so that those skilled in the art can realize and utilize the present invention a variety of different exemplary implementation schemes and
Various chooses and changes.The scope of the present invention is intended to be limited by claims and its equivalents.
Claims (10)
1. it is a kind of using macroreticular resin to the process for purification of pumpkin oligosaccharide, which is characterized in that include the following steps：
(1) pumpkin oligosaccharide crude extract is added into water, is made into pumpkin oligosaccharide upper prop solution；By 0.8~1.5 times of column volume (BV) institute
Pumpkin oligosaccharide upper prop solution is stated by the chromatographic column equipped with macroreticular resin, upper prop absorption is carried out, then collects efflux；
(2) it stands, then macroreticular resin is eluted with deionized water, by remaining pumpkin oligosaccharide eluent in column and step (1)
Middle gained efflux merges, and is then concentrated by evaporation, is lyophilized, obtains colourless pumpkin oligosaccharide；
(3) foreign pigment on the ethanol solution elution absorption macroreticular resin of 1.5~2.2BV is used；It is impregnated using ethyl alcohol, uses water
It is washed till no alcohol taste, by resin column and is impregnated using NaOH solution, is washed to neutrality；Then it by resin column and is soaked using hydrochloric acid
Bubble is washed to neutrality, recycles macroreticular resin；Finally, it evaporates and is freeze-dried through revolving, recycle foreign pigment and ethyl alcohol.
2. process for purification according to claim 1, which is characterized in that pumpkin oligosaccharide upper prop solution described in step (1)
Mass percent concentration be 230~280mg/ml.
3. process for purification according to claim 1, which is characterized in that macroreticular resin described in step (1) uses preceding progress
Pretreatment, concrete operations are：It uses deionized water to impregnate macroreticular resin first, is washed till with ethyl alcohol not muddy；Then it is soaked with ethyl alcohol
Bubble, is washed with deionized water to no alcohol taste；The NaOH solution for being again 5% with mass percent concentration by resin column and impregnates tree
Fat is washed to neutrality, and the hydrochloric acid that mass percent concentration is 5% by resin column and is impregnated resin, is finally washed to neutrality,
To obtain the final product to the macroreticular resin handled well.
4. process for purification according to claim 1, which is characterized in that the volume basis of ethanol solution described in step (3)
Specific concentration is 60~80%.
5. process for purification according to claim 1, which is characterized in that the macroreticular resin is selected from ion exchange resin, non-
One or both of polar macroporous resin, preferably non-polar macroporous resin.
6. process for purification according to claim 5, which is characterized in that the non-polar macroporous resin is selected from DM21 type macropores
Adsorb one or more of resin, DM28 type macroporous absorbent resins.
7. process for purification according to claim 1, which is characterized in that the material of the chromatographic column is strengthened glass, specification
For 6cm × 80cm.
8. process for purification according to claim 1, which is characterized in that pumpkin oligosaccharide crude extract described in step (1)
Preparation method includes：
(1) by pumpkin remove seed, stripping and slicing, water is added to be beaten, hot water extraction, centrifuging and taking supernatant is concentrated into the 1/2 of former supernatant volume
~1/5, obtain concentrate；
(2) ethyl alcohol is added to be precipitated, centrifuging and taking supernatant；
(3) supernatant is diluted to and is crossed 20 μm of filter bags, filtrate first passes through ultrafiltration section, and ultrafiltration retaining molecular weight is 3000Da, thoroughly
Liquid is crossed by nanofiltration section, nanofiltration retaining molecular weight is 300Da, and it is pumpkin oligosaccharide crude extract to be trapped liquid.
9. process for purification according to claim 8, which is characterized in that the volume basis of ethanol solution described in step (2)
Specific concentration is 70~90%, preferably 80%.
10. process for purification according to claim 8, which is characterized in that ethanol solution described in step (2) and step (1)
The volume ratio of gained concentrate is 2~5: 1.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112480283A (en) * | 2020-12-28 | 2021-03-12 | 湖南中医药大学 | Method for preparing neutral oligosaccharide from rhizoma polygonati |
| CN112899326A (en) * | 2021-03-31 | 2021-06-04 | 新疆大学 | Method for preparing melon peel pectin oligosaccharide with antibacterial activity by using immobilized enzyme |
| CN114163486A (en) * | 2021-12-22 | 2022-03-11 | 云南三七科技有限公司 | Method for preparing oligosaccharide from pseudo-ginseng |
| CN114210312A (en) * | 2021-12-17 | 2022-03-22 | 金七药业股份有限公司 | Low-temperature freezing regeneration treatment method for macroporous resin |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104543802A (en) * | 2014-12-17 | 2015-04-29 | 方萌 | Method for extracting soybean oligosaccharides from soybeans |
| CN105112475A (en) * | 2015-10-10 | 2015-12-02 | 中国农业大学 | Preparation method of soluble syrup of castanea mollissima BL. |
| CN106799167A (en) * | 2017-01-11 | 2017-06-06 | 中国农业大学 | The method that a kind of double films of ultrafiltration/nanofiltration efficiently purify pumpkin oligosaccharide |
| CN106957344A (en) * | 2017-05-24 | 2017-07-18 | 中国农业大学 | A kind of method that subcritical water prepares oligosaccharide |
-
2018
- 2018-04-27 CN CN201810394655.XA patent/CN108640953B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104543802A (en) * | 2014-12-17 | 2015-04-29 | 方萌 | Method for extracting soybean oligosaccharides from soybeans |
| CN105112475A (en) * | 2015-10-10 | 2015-12-02 | 中国农业大学 | Preparation method of soluble syrup of castanea mollissima BL. |
| CN106799167A (en) * | 2017-01-11 | 2017-06-06 | 中国农业大学 | The method that a kind of double films of ultrafiltration/nanofiltration efficiently purify pumpkin oligosaccharide |
| CN106957344A (en) * | 2017-05-24 | 2017-07-18 | 中国农业大学 | A kind of method that subcritical water prepares oligosaccharide |
Non-Patent Citations (1)
| Title |
|---|
| 蔡宝昌，等: "《中药制剂前处理新技术与新设备》", 30 November 2005 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112480283A (en) * | 2020-12-28 | 2021-03-12 | 湖南中医药大学 | Method for preparing neutral oligosaccharide from rhizoma polygonati |
| CN112480283B (en) * | 2020-12-28 | 2023-02-24 | 湖南中医药大学 | Method for preparing neutral oligosaccharide from rhizoma polygonati |
| CN112899326A (en) * | 2021-03-31 | 2021-06-04 | 新疆大学 | Method for preparing melon peel pectin oligosaccharide with antibacterial activity by using immobilized enzyme |
| CN114210312A (en) * | 2021-12-17 | 2022-03-22 | 金七药业股份有限公司 | Low-temperature freezing regeneration treatment method for macroporous resin |
| CN114210312B (en) * | 2021-12-17 | 2024-03-22 | 金七药业股份有限公司 | Regeneration treatment method for macroporous resin low-temperature freezing |
| CN114163486A (en) * | 2021-12-22 | 2022-03-11 | 云南三七科技有限公司 | Method for preparing oligosaccharide from pseudo-ginseng |
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