CN104860871A - Method of DNJ extraction and purification - Google Patents
Method of DNJ extraction and purification Download PDFInfo
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- CN104860871A CN104860871A CN201510292340.0A CN201510292340A CN104860871A CN 104860871 A CN104860871 A CN 104860871A CN 201510292340 A CN201510292340 A CN 201510292340A CN 104860871 A CN104860871 A CN 104860871A
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- 238000000034 method Methods 0.000 title claims abstract description 34
- 238000000746 purification Methods 0.000 title claims abstract description 21
- 238000000605 extraction Methods 0.000 title claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 35
- 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 abstract description 15
- 239000003729 cation exchange resin Substances 0.000 claims abstract description 15
- 239000003480 eluent Substances 0.000 claims abstract description 12
- 238000001291 vacuum drying Methods 0.000 claims abstract description 9
- 239000012535 impurity Substances 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 3
- 239000011347 resin Substances 0.000 claims description 44
- 229920005989 resin Polymers 0.000 claims description 44
- 239000008367 deionised water Substances 0.000 claims description 21
- 229910021641 deionized water Inorganic materials 0.000 claims description 21
- 239000000047 product Substances 0.000 claims description 16
- 235000008708 Morus alba Nutrition 0.000 claims description 15
- 240000000249 Morus alba Species 0.000 claims description 15
- 239000000284 extract Substances 0.000 claims description 13
- 239000000706 filtrate Substances 0.000 claims description 12
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 10
- 238000010521 absorption reaction Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 238000013019 agitation Methods 0.000 claims description 6
- 238000010828 elution Methods 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 238000002203 pretreatment Methods 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000013375 chromatographic separation Methods 0.000 description 3
- 235000013305 food Nutrition 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical class [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 229930013930 alkaloid Natural products 0.000 description 2
- 238000004939 coking Methods 0.000 description 2
- 238000002242 deionisation method Methods 0.000 description 2
- 150000002016 disaccharides Chemical class 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000005342 ion exchange Methods 0.000 description 2
- 239000006070 nanosuspension Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 101000925662 Enterobacteria phage PRD1 Endolysin Proteins 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 150000003797 alkaloid derivatives Chemical class 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 206010012601 diabetes mellitus Diseases 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 230000032050 esterification Effects 0.000 description 1
- 238000005886 esterification reaction Methods 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
- 230000002218 hypoglycaemic effect Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229930014626 natural product Natural products 0.000 description 1
- 230000000050 nutritive effect Effects 0.000 description 1
- 230000000144 pharmacologic effect Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 210000000813 small intestine Anatomy 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 229930003231 vitamin Natural products 0.000 description 1
- 239000011782 vitamin Substances 0.000 description 1
- 229940088594 vitamin Drugs 0.000 description 1
- 235000013343 vitamin Nutrition 0.000 description 1
- 150000003722 vitamin derivatives Chemical class 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D211/00—Heterocyclic compounds containing hydrogenated pyridine rings, not condensed with other rings
- C07D211/04—Heterocyclic compounds containing hydrogenated pyridine rings, not condensed with other rings with only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D211/06—Heterocyclic compounds containing hydrogenated pyridine rings, not condensed with other rings with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having no double bonds between ring members or between ring members and non-ring members
- C07D211/36—Heterocyclic compounds containing hydrogenated pyridine rings, not condensed with other rings with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having no double bonds between ring members or between ring members and non-ring members with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D211/40—Oxygen atoms
- C07D211/44—Oxygen atoms attached in position 4
- C07D211/46—Oxygen atoms attached in position 4 having a hydrogen atom as the second substituent in position 4
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention relates to a method of DNJ extraction and purification. The method comprises the following steps: firstly, preparing a DNJ extracting solution, and pretreating the extracting solution, so as to obtain DNJ clear liquor; secondly, adsorbing the DNJ clear liquor through a cation exchange resin column; thirdly, enabling clear water to pass through the cation exchange resin column on which DNJ is absorbed, washing the cation exchange resin column, and removing impurities which are not absorbed; fourthly, eluting the cation exchange resin column on which DNJ is absorbed, and collecting eluent; fifthly, performing concentration and vacuum drying on the eluent, so as to obtain DNJ products. Compared with the prior art, the method has the advantages that the technology is simple and easy, PK216 cation exchange resin can be reused, the method is energy-saving and environment-friendly, raw materials are easy to get and low in cost, and DNJ products with high purity can be obtained through the method.
Description
Technical field
The present invention relates to a kind of natural alkaloid purification process, especially relate to a kind of method of DNJ extraction purification, belong to natural product technical field of purification.
Background technology
Nutritive ingredient is rich in, the several functions compositions such as the amino acid containing needed by human body, VITAMIN, inorganic salt, flavonoid, alkaloids in mulberry leaf.Particularly a kind of alkaloid-1-DNJ (DNJ) of mulberry leaf, there is special function, pharmacological research confirms, mulberry leaf DNJ is inhibited to disaccharides lytic enzyme activity, thus suppress small intestine to the absorption of disaccharide, after reducing food, the peak value of blood sugar reaches hypoglycemic effect [food science and technology, 2010,35 (12): 209-211; Food science and technology, 2009,34 (7): 168-171].
China extracts DNJ and has carried out large quantifier elimination, but the separating-purifying of DNJ waits further research at present.Obtained the DNJ product of high-content by the separating and purifying method of cheap and simple, by the medicine of exploitation treatment diabetes etc. and the development of healthcare products, there is the effect of actively promoting.
Chinese patent CN 104402801 A discloses a kind of DNJ of separation and prepares the method for DNJ nano suspension, the method being separated DNJ take mulberry tree as raw material, extract through pulverizing, microwave coking, isolate I is obtained after being dissolved in water, this isolate forms isolate II by fine sand-gac and silica gel twice chromatographic separation successively, described isolate II obtains isolate III through ion-exchange and alcohol settling, this isolate III is separated through chromatography on alumina post and obtains isolate IV, obtains target product by after isolate IV crystallization and recrystallization.First the method preparing DNJ nano suspension carries out esterification modification to DNJ component, strengthens that it is fat-soluble, is then combined by tensio-active agent and DNJ is dispersed into high dispersing population by high-pressure homogeneous process.The separation method of this patent comprises steps such as pulverizing extraction, microwave coking, chromatographic separation, ion-exchange, chromatographic separation, and program is comparatively complicated, and productive rate is lower.
Summary of the invention
Object of the present invention is exactly provide a kind of rational technology, simple to operate, the method for environmental protection and energy saving, lower-cost DNJ extraction purification to overcome defect that above-mentioned prior art exists.
Object of the present invention can be achieved through the following technical solutions:
A method for DNJ extraction purification, comprises the following steps:
(1) DNJ extracting solution is prepared, and pre-treatment, obtain DNJ clear liquor;
(2) DNJ clear liquor is adsorbed by cation exchange resin column;
(3) with the cation exchange resin column of clear water by absorption DNJ, wash, remove the impurity do not adsorbed;
(4) wash-out is carried out to the Zeo-karb being adsorbed with DNJ, collect elutriant;
(5) namely elutriant is concentrated, vacuum-drying obtain DNJ product.
The method that step (1) prepares DNJ extracting solution is: by the mulberry leaf of drying, adds in deionized water, at 60 ~ 95 DEG C, extract 1 ~ 2h, filters, and reclaims filter residue, filter residue is added deionized water and extract 1 time again, merge all filtrate, obtain DNJ extracting solution.
Dry mulberry leaf or the weight ratio of filter residue and deionized water are 1:5 ~ 1:20.
Pretreatment process described in step (1) is: under agitation add in DNJ extracting solution by ZTC finings solution, leaves standstill 0.2-2h, and filter, gained filtrate is DNJ clear liquor, and ZTC finings solution is 1:5-1:20 with the ratio of DNJ extracting liquid volume.The concentration of described ZTC finings solution is 1wt%.
The condition of absorption is in step (2): the upper column flow rate of DNJ clear liquor be 1 ~ 5 times of resin volume/hour.
The Zeo-karb of to be commercially available model the be PK216 of the Zeo-karb described in step (2).
The condition of washing is in step (3): clear water by resin column flow velocity be 1 ~ 5 times of resin volume/hour.
In step (4), the condition of wash-out is: eluent is ammoniacal liquor, and the concentration of ammoniacal liquor is 0.4mol/L ~ 3mol/L; The volume of eluent is 2 ~ 10 times of resin volumes; Elution flow rate be 1 ~ 4 times of resin volume/hour.
Drying described in step (5) is the vacuum-drying of 30 DEG C ~ 50 DEG C.
In step (5) gained DNJ product, DNJ content is greater than 15wt%.
Compared with prior art, present invention process is simple, and PK216 Zeo-karb can repeatedly use, environmental protection and energy saving, and raw material is easy to get and inexpensive, and the present invention can obtain the DNJ product of higher degree.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.
Embodiment 1
(1) preparation of DNJ extracting solution: the mulberry leaf getting 100g drying, adds the deionized water of 1500mL, at 80 DEG C, extract 1.5h, filters, and reclaims filter residue.Filter residue adopts above method to extract 1 time again, merges above filtrate, i.e. DNJ extracting solution.
(2) PK216 Zeo-karb adopts and soaks 24h with saturated NaCl saline soak, then uses deionized water wash, gets 50mL and fill out post.Be that 5wt% sodium hydroxide water passes through resin column by the concentration of 2 times of resin volumes again; Then washed by resin column with the deionization of 10 times of resin volumes; Be that 1wt% hydrochloric acid soln passes through resin column by the concentration of 2 times of resin volumes again; Then washed by resin column with the deionization of 10 times of resin volumes, the resin column handled well treats that subsequent step is used.
(3) be under agitation that the ZTC finings solution of 1%wt adds in the DNJ extracting solution of the 1000mL of above preparation by 100mL concentration, leave standstill 0.2-2h, filter, gained filtrate is DNJ clear liquor.
(4) get 2 times of resin volumes through pretreated DNJ clear liquor, pass through resin column with 3 times of resin volume/h.
(5) after PK216 cationic exchange resin adsorption DNJ, be that 4 times of resin volume/h are washed by resin column with the deionized water water of 2 times of resin volumes with flow velocity, then use the ammonia soln of the 0.5mol/L of 3 times of resin volumes to carry out wash-out with 2 times of resin volume/h by resin column, collect elutriant.
(6) above elutriant is concentrated into dry at 50 DEG C, and 45 DEG C of vacuum-dryings obtain DNJ product, and in DNJ product, the content of DNJ is 16.2%.
Embodiment 2
A method for DNJ extraction purification, comprises the following steps:
(1) by the mulberry leaf of drying, add in deionized water, dry mulberry leaf and the weight ratio of deionized water are 1:5, at 60 DEG C, extract 2h, filter, reclaim filter residue, filter residue is added deionized water, and the weight ratio of filter residue and deionized water is 1:5, then extracts 1 time, merge all filtrate, obtain DNJ extracting solution;
(2) be under agitation that the ZTC finings solution of 1wt% adds in DNJ extracting solution by concentration, ZTC finings solution is 1:5 with the ratio of DNJ extracting liquid volume, leaves standstill 0.2h, and filter, gained filtrate is DNJ clear liquor;
(3) DNJ clear liquor is adsorbed by PK216 cation exchange resin column, the upper column flow rate of DNJ clear liquor be 1 times of resin volume/hour;
(4) with the cation exchange resin column of clear water by absorption DNJ, wash, clear water by resin column flow velocity be 1 times of resin volume/hour, remove the impurity that do not adsorb;
(5) carry out wash-out to the Zeo-karb being adsorbed with DNJ, the condition of wash-out is: eluent is ammoniacal liquor, and the concentration of ammoniacal liquor is 0.4mol/L; The volume of eluent is 2 times of resin volumes; Elution flow rate be 1 times of resin volume/hour, collect elutriant;
(6) concentrated by elutriant, at 30 DEG C, namely vacuum-drying obtain DNJ product, and in gained DNJ product, DNJ content is 17.2wt%.
Embodiment 3
A method for DNJ extraction purification, comprises the following steps:
(1) by the mulberry leaf of drying, add in deionized water, dry mulberry leaf and the weight ratio of deionized water are 1:10, at 75 DEG C, extract 1.5h, filter, reclaim filter residue, filter residue is added deionized water, and the weight ratio of filter residue and deionized water is 1:10, then extracts 1 time, merge all filtrate, obtain DNJ extracting solution;
(2) be under agitation that the ZTC finings solution of 1wt% adds in DNJ extracting solution by concentration, ZTC finings solution is 1:10 with the ratio of DNJ extracting liquid volume, leaves standstill 1h, and filter, gained filtrate is DNJ clear liquor;
(3) DNJ clear liquor is adsorbed by PK216 cation exchange resin column, the upper column flow rate of DNJ clear liquor be 3 times of resin volumes/hour;
(4) with the cation exchange resin column of clear water by absorption DNJ, wash, clear water by resin column flow velocity be 3 times of resin volumes/hour, remove the impurity that do not adsorb;
(5) carry out wash-out to the Zeo-karb being adsorbed with DNJ, the condition of wash-out is: eluent is ammoniacal liquor, and the concentration of ammoniacal liquor is 1.5mol/L; The volume of eluent is 6 times of resin volumes; Elution flow rate be 2 times of resin volumes/hour, collect elutriant;
(6) concentrated by elutriant, at 40 DEG C, namely vacuum-drying obtain DNJ product, and in gained DNJ product, DNJ content is 16.5wt%.
Embodiment 4
A method for DNJ extraction purification, comprises the following steps:
(1) by the mulberry leaf of drying, add in deionized water, dry mulberry leaf and the weight ratio of deionized water are 1:20, at 95 DEG C, extract 1h, filter, reclaim filter residue, filter residue is added deionized water, and the weight ratio of filter residue and deionized water is 1:20, then extracts 1 time, merge all filtrate, obtain DNJ extracting solution;
(2) be under agitation that the ZTC finings solution of 1wt% adds in DNJ extracting solution by concentration, ZTC finings solution is 1:20 with the ratio of DNJ extracting liquid volume, leaves standstill 2h, and filter, gained filtrate is DNJ clear liquor;
(3) DNJ clear liquor is adsorbed by PK216 cation exchange resin column, the upper column flow rate of DNJ clear liquor be 5 times of resin volumes/hour;
(4) with the cation exchange resin column of clear water by absorption DNJ, wash, clear water by resin column flow velocity be 5 times of resin volumes/hour, remove the impurity that do not adsorb;
(5) carry out wash-out to the Zeo-karb being adsorbed with DNJ, the condition of wash-out is: eluent is ammoniacal liquor, and the concentration of ammoniacal liquor is 3mol/L; The volume of eluent is 10 times of resin volumes; Elution flow rate be 4 times of resin volumes/hour, collect elutriant;
(6) concentrated by elutriant, at 50 DEG C, namely vacuum-drying obtain DNJ product, and in gained DNJ product, DNJ content is 15.4wt%.
Above-mentioned is can understand and use invention for ease of those skilled in the art to the description of embodiment.Person skilled in the art obviously easily can make various amendment to these embodiments, and General Principle described herein is applied in other embodiments and need not through performing creative labour.Therefore, the invention is not restricted to above-described embodiment, those skilled in the art, according to announcement of the present invention, do not depart from improvement that scope makes and amendment all should within protection scope of the present invention.
Claims (10)
1. a method for DNJ extraction purification, is characterized in that, comprises the following steps:
(1) DNJ extracting solution is prepared, and pre-treatment, obtain DNJ clear liquor;
(2) DNJ clear liquor is adsorbed by cation exchange resin column;
(3) with the cation exchange resin column of clear water by absorption DNJ, wash, remove the impurity do not adsorbed;
(4) wash-out is carried out to the Zeo-karb being adsorbed with DNJ, collect elutriant;
(5) namely elutriant is concentrated, vacuum-drying obtain DNJ product.
2. the method for a kind of DNJ extraction purification according to claim 1, it is characterized in that, the method that step (1) prepares DNJ extracting solution is: by the mulberry leaf of drying, add in deionized water, at 60 ~ 95 DEG C, extract 1 ~ 2h, filter, reclaim filter residue, filter residue is added deionized water and extract 1 time again, merge all filtrate, obtain DNJ extracting solution.
3. the method for a kind of DNJ extraction purification according to claim 2, is characterized in that, dry mulberry leaf or the weight ratio of filter residue and deionized water are 1:5 ~ 1:20.
4. the method for a kind of DNJ extraction purification according to claim 1, it is characterized in that, pretreatment process described in step (1) is: under agitation add in DNJ extracting solution by ZTC finings solution, leave standstill 0.2-2h, filter, gained filtrate is DNJ clear liquor, and ZTC finings solution is 1:5-1:20 with the ratio of DNJ extracting liquid volume.
5. the method for a kind of DNJ extraction purification according to claim 1, is characterized in that, the condition of absorption is in step (2): the upper column flow rate of DNJ clear liquor be 1 ~ 5 times of resin volume/hour.
6. the method for a kind of DNJ extraction purification according to claim 1, is characterized in that, the Zeo-karb of to be commercially available model the be PK216 of the Zeo-karb described in step (2).
7. the method for a kind of DNJ extraction purification according to claim 1, is characterized in that, the condition of washing is in step (3): clear water by resin column flow velocity be 1 ~ 5 times of resin volume/hour.
8. the method for a kind of DNJ extraction purification according to claim 1, is characterized in that, in step (4), the condition of wash-out is: eluent is ammoniacal liquor, and the concentration of ammoniacal liquor is 0.4mol/L ~ 3mol/L; The volume of eluent is 2 ~ 10 times of resin volumes; Elution flow rate be 1 ~ 4 times of resin volume/hour.
9. the method for a kind of DNJ extraction purification according to claim 1, is characterized in that, the drying described in step (5) is the vacuum-drying of 30 DEG C ~ 50 DEG C.
10. the method for a kind of DNJ extraction purification according to claim 1, is characterized in that, in step (5) gained DNJ product, DNJ content is greater than 15wt%.
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| CN201510292340.0A CN104860871A (en) | 2015-06-01 | 2015-06-01 | Method of DNJ extraction and purification |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109180563A (en) * | 2018-08-28 | 2019-01-11 | 广东碧桑园科技有限公司 | A method of extracting DNJ from fresh mulberry leaf |
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| CN104257755A (en) * | 2014-09-09 | 2015-01-07 | 南京中医药大学 | Composition with effect of treating diabetes as well as preparation method and application of composition |
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| CN109180563A (en) * | 2018-08-28 | 2019-01-11 | 广东碧桑园科技有限公司 | A method of extracting DNJ from fresh mulberry leaf |
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