CN102101840A - Method for extracting and separating high-purity 1-Deoxynojirimycin from folium mori - Google Patents
Method for extracting and separating high-purity 1-Deoxynojirimycin from folium mori Download PDFInfo
- Publication number
- CN102101840A CN102101840A CN 201110038204 CN201110038204A CN102101840A CN 102101840 A CN102101840 A CN 102101840A CN 201110038204 CN201110038204 CN 201110038204 CN 201110038204 A CN201110038204 A CN 201110038204A CN 102101840 A CN102101840 A CN 102101840A
- Authority
- CN
- China
- Prior art keywords
- mulberry leaf
- high purity
- column
- extraction separation
- described method
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Medicines Containing Plant Substances (AREA)
Abstract
The invention relates to a technology for extracting and separating active ingredients of traditional Chinese medicines, in particular to a method for extracting and separating high-purity 1-deoxynojirimycin from folium mori, which comprises the following steps of: extracting a powder material by using an aqueous solvent, filtering off dregs, and centrifuging the material to obtain extracting solution; concentrating the extracting solution until ethanol does not exist, and filtering by using an ultrafiltration membrane; regulating the pH to be 3.0-4.0 by using inorganic acid, precipitating, and centrifuging to removing impurities; applying acidified feed to a strong acid cation resin column, washing with water, and eluting by using ammonia water; applying feed liquid to a porous resin column, washing with water, performing gradient elution by using ethanol with different concentrations, and collecting target eluent; concentrating the target eluent under reduced pressure, and drying to obtain a crude product; dissolving the crude product by using absolute ethanol, making the solution pass through an alkaline adsorbing column to remove impurities, and collecting effluent liquid; and concentrating the effluent liquid under reduced pressure, and performing normal temperature crystallization and recrystallization to obtain the refined 1-DNJ product. In the whole technological process, except ethanol, other organic solvents are not used, the operation is safe, and the 1-DNJ content can reach 98.3 percent.
Description
Technical field
The present invention relates to a kind of Chinese medicine extracts active ingredients and isolating technology, refer in particular to a kind of method by extraction separation high purity 1-S-GI in the mulberry leaf.
Background technology
Mulberry leaf are the leaf of Moraceae (Moraceae) Morus plant (Morus L.), it is the medicine food dual purpose plant that health ministry is announced, all there is cultivation and production in most of area, the whole nation, and is maximum with southern silkworm and mulberry main producing region output, as Jiangsu, Guangxi, Zhejiang, Anhui, Sichuan etc.China Morus plant has 4 mutation of 15 kinds, and the person of wherein not being used as medicine mostly is Bai Sang (Morus alba).Mulberry leaf are abundant in china natural resources, are again a kind of conventional Chinese medicines in the hospital in ancient times.Mulberry is on the books in " Book of Songs ", and the mulberry leaf head that is used as medicine sees Shennong's Herbal.Mulberry leaf bitter, sweet, cold in nature, return lung, Liver Channel, have that dispelling wind and heat pathogens, clearing away lung-heat and moistening dryness, flat liver make eye bright, the effect of cooling blood for hemostasis.The record mulberry leaf can be treated diabetes in the successive dynasties Chinese materia medica books.Modern medicine finds that mulberry leaf have functions such as hypotensive, hypoglycemic, reducing cholesterol, antitumor, antianaphylaxis, anti-oxidant, anti-capillary penetration and diuresis on research mulberry leaf chemical ingredients and experimentation on animals basis.
1-S-GI (1-DNJ) is a kind of piperidines polyhydroxylated alkaloid, and English name is 1-Deoxynojirimycin, is called for short 1-DNJ, and chemical name is 3,4,5-trihydroxy--2-methylol tetrahydropyridine, and molecular formula is C
6H
13NO
4, molecular weight is 163, has multiple biological activitys such as hypoglycemic, antiviral, anti metastasis.Result of study so far, occurring in nature is the highest with content in the mulberry leaf.1-DNJ is as a kind of glycosidase inhibitor, can prevent that blood sugar concentration from raising, have effects such as hypoglycemic, antiviral and anti metastasis, have excellent development prospect and using value, thereby by extracting the focus that 1-DNJ has become Chinese scholars research in the mulberry leaf.
In the existing patent, as the patent No. be the patent of invention of CN1579445A be by add flocculation agent again alcohol precipitation obtain Folium Mori extract, 1-DNJ content 1.0-3.0%; As the patent No. is that the patent of invention of CN1175818C is by flocculation, column chromatography separation and purification, obtains the mulberry extract of high level, and wherein 1-DNJ content is greater than 50% of the medicinal extract gross weight.CN1430964A adopts flocculation, ion column chromatographic separation technology; CN101654428A does not use flocculation agent, the extracting solution acidifying, and concentrating and impurity removing, through yin, yang ion column chromatography, steps such as gel filtration chromatography get purified product again; CN101020655A does not use flocculation agent, and the mulberry leaf extracting solution adds the mineral acid acidification, the cooling removal of impurities, and column chromatography obtains extract again, and 1-DNJ content is greater than 10%.Chinese patent CN101020655A provides a kind of method of extracting 1 one S-GIs (DNJ) from mulberry leaf, be by in the extracting solution of mulberry leaf, adding the mineral acid acidification, remove impurity through cooling, be not less than 10% Folium Mori extract again through column chromatography acquisition 1-DNJ content.This inventive method is not owing to need to add flocculation agent, having guaranteed when reducing cost, improving content does not have ectogenic material to bring in the last handling process, again acidizing fluid is concentrated the back and directly adopt homemade ion-exchange chromatography to separate, greatly reduce cost; This patent greatest drawback is that the 1-S-GI content that makes is lower, only is about 10%.
And yet there are no report relevant for a whole set of technology by extraction separation high purity 1-DNJ in the mulberry leaf.
Summary of the invention
In order to solve above-mentioned the deficiencies in the prior art and shortcoming, the invention provides a kind of method by extraction separation high purity 1-S-GI in the mulberry leaf.
Technical scheme of the present invention is: a kind of method by extraction separation high purity 1-S-GI in the mulberry leaf comprises following sequential steps:
(1) gets the mulberry leaf pulverizing medicinal materials, sieve, must extract and use Mulberry Leaf;
(2) raw material powder extracts with water-containing solvent, filters the dregs of a decoction, and material is centrifugal, gets extracting solution;
(3) extracting solution is concentrated into no ethanol, ultrafiltration membrance filter;
(4) feed liquid is transferred pH to 3.0-4.0 with mineral acid, precipitation, centrifugal removal of impurities;
(5) strong acidic ion resin post on the acidifying feed liquid, the ammoniacal liquor wash-out is carried out in washing again, collects the pH9-12 elutriant, transfers to pH value neutrality with hydrochloric acid;
(6) macroporous resin column on the feed liquid, the Different concentrations of alcohol gradient elution is used in washing again, collects the target elutriant;
(7) target elutriant concentrating under reduced pressure, drying get crude product;
(8) crude product anhydrous alcohol solution, effluent liquid is collected in the removal of impurities of parlkaline adsorption column;
(9) effluent liquid concentrating under reduced pressure carries out normal temperature crystallization and recrystallization, obtains mass content and is higher than 98% 1-DNJ highly finished product.
Preferably, cross 40 mesh sieves in the step (1) after the mulberry leaf pulverizing medicinal materials.
Preferably, the water-containing solvent in the step (2) is mixed by water and ethanol and forms; Mineral acid is a hydrochloric acid in the step (4), and its mass concentration is 10%.
Preferably, ultra-filtration membrane is the hollow cellulose acetate membrane in the step (3).
Preferably, resin cation (R.C.) is selected from model 002SC, D001,001 * 4,001 * 7 or 001 * 8 in the step (5), and water and ammoniacal liquor elution volume are 3 times of column volumes, and ammonia concn is 0.5-1.0%, and flow velocity is 0.5-1 times of column volume/h.
Preferably, macroporous resin is selected from model D101, HP20, AB-8, CAD-40, DM301 or HPD-400 in the step (6), and water and ethanol elution volume are 2 times of column volumes, and flow velocity is 0.5-1 times of column volume/h.
Preferably, resin cation (R.C.) is selected from model 001 * 8 in the step (5), and macroporous resin is selected from model AB-8 in the step (6).
Preferably, vacuum decompression concentrates in the step (7), and drying temperature is 55-60 ℃.
Preferably, be provided with alkali alumina as alkaline adsorbent in step (8) the neutral and alkali adsorption column.
Preferably, vacuum decompression concentrates in the step (9), and thickening temperature is 55-60 ℃, naturally cooling, crystallization, recrystallization 1-2 time.
Extraction and separation method of the present invention has following beneficial effect:
(1) whole technological process is not used other organic solvent except that ethanol, operational safety, and avoid dissolvent residual;
(2) whole technological process, demineralizing acid, ammoniacal liquor are not brought other allogenic materials into, and all can remove in the macroporous resin chromatography;
(3) adopt the ultrafiltration removal of impurities, filter out macromole impurity, avoid it to bring subsequent technique into;
(4) acidizing fluid is directly used the resin cation (R.C.) column chromatography, goes up macroporous resin column chromatography again, greatly improves purity, and has avoided adjusting repeatedly the repetitive operation of pH;
(5) go up the removal of impurities of alkali alumina adsorption column, further remove impurity and pigment, be convenient to crystallization, help guaranteeing product purity, 1-DNJ content can reach 98.3%.
Description of drawings
Fig. 1 is the process flow sheet of the inventive method.
Embodiment
Below by specific embodiment the present invention is described in further detail, but is not limiting the scope of the invention.
Embodiment 1
With reference to Fig. 1, a kind of method by extraction separation high purity 1-S-GI in the mulberry leaf comprises following sequential steps:
With the mulberry leaf pulverizing medicinal materials, cross 40 mesh sieves;
Get the 10kg raw material powder, adopt 75% ethanol under 60 ℃ of conditions, to extract (solvent is doubly measured and is respectively 10 times and 8 times) twice, each 1h;
United extraction liquid, centrifugal, 60 ℃ of vacuum decompressions are concentrated into about 20L;
Concentrated solution is crossed ultra-filtration membrane, and ultrafiltrated adds hydrochloric acid and transfers pH to 3.0, and is centrifugal, gets acidizing fluid;
Get the 2L acidizing fluid, last column volume is 001 * 8 resin column of 1L, wash 3 times of column volumes after, be 1.0% ammoniacal liquor wash-out with 3 times of column volume concentration again, flow velocity is 1 times of column volume/h, collects the elutriant of pH9-12;
Get ammoniacal liquor elutriant 3L, transfer to neutrality with hydrochloric acid; Last column volume is the D101 macroporous resin column of 1L, wash 2 times of column volumes after, the ethanolic soln gradient elution that is 10-70% with 2 times of column volume concentration again, flow velocity is 1 times of column volume/h, substep is collected elutriant;
Merging alcohol concn is the elutriant of 20%-40%, after vacuum decompression concentrates (55 ℃-60 ℃), vacuum-drying, content is 45.2% crude product, total conversion rate is 85.4%, yield is 0.51%;
Get the crude product 8.0g that makes, the 200ml anhydrous alcohol solution, parlkaline alumina adsorption post is collected effluent liquid, and vacuum decompression concentrates (55 ℃-60 ℃) to proper volume, normal temperature crystallization, recrystallization 1-2 time, 1-DNJ highly finished product that must content 98.3%.
Embodiment 2
Get the ammoniacal liquor elutriant 3L among the embodiment 1, transfer to neutrality with hydrochloric acid;
Last column volume is the HP20 macroporous resin column of 1L, wash 2 times of column volumes after, the ethanolic soln gradient elution that is 10-70% with 2 times of column volume concentration again, flow velocity is 1 times of column volume/h, substep is collected elutriant;
Merging alcohol concn is the elutriant of 20%-40%, after vacuum decompression concentrates (55 ℃-60 ℃), vacuum-drying, content is 52.8% crude product, total conversion rate is 84.2%, yield is 0.43%;
Get the crude product 8.0g that makes, the 200ml anhydrous alcohol solution by the alkali alumina adsorption column, is collected effluent liquid, and vacuum decompression concentrates (55 ℃-60 ℃) to proper volume, normal temperature crystallization, recrystallization 1-2 time, 1-DNJ highly finished product that must content 98.4%.
Embodiment 3
Get the ammoniacal liquor elutriant 3L among the embodiment 1, transfer to neutrality with hydrochloric acid;
Last column volume is the CAD-40 macroporous resin column of 1L, wash 2 times of column volumes after, the ethanolic soln gradient elution that is 10-70% with 2 times of column volume concentration again, flow velocity is 1 times of column volume/h, substep is collected elutriant;
Merging alcohol concn is the elutriant of 20%-40%, after vacuum decompression concentrates (55 ℃-60 ℃), vacuum-drying, content is 54.1% crude product, total conversion rate is 86.1%, yield is 0.42%;
Get the crude product 8.0g that makes, the 200ml anhydrous alcohol solution by the alkali alumina adsorption column, is collected effluent liquid, and vacuum decompression concentrates (55 ℃-60 ℃) to proper volume, and normal temperature crystallization, recrystallization 1-2 time get content and be higher than 98% 1-DNJ highly finished product.
Embodiment 4
Get the ammoniacal liquor elutriant 3L among the embodiment 1, transfer to neutrality with hydrochloric acid;
Last column volume is the DM301 macroporous resin column of 1L, wash 2 times of column volumes after, the ethanolic soln gradient elution that is 10-70% with 2 times of column volume concentration again, flow velocity is 1 times of column volume/h, distributes to collect elutriant;
Merging alcohol concn is the elutriant of 20%-40%, after vacuum decompression concentrates (55 ℃-60 ℃), vacuum-drying, content is 55.3% crude product, total conversion rate is 77.9%, yield is 0.38%;
Get the crude product 8.0g that makes, the 200ml anhydrous alcohol solution by the alkali alumina adsorption column, is collected effluent liquid, and vacuum decompression concentrates (55 ℃-60 ℃) to proper volume, and normal temperature crystallization, recrystallization 1-2 time get content and be higher than 98% 1-DNJ highly finished product.
Embodiment 5
Get the ammoniacal liquor elutriant 3L among the embodiment 1, transfer to neutrality with hydrochloric acid;
Last column volume is the HPD-400 macroporous resin column of 1L, wash 2 times of column volumes after, the ethanolic soln gradient elution that is 10-70% with 2 times of column volume concentration again, flow velocity is 1 times of column volume/h, substep is collected elutriant;
Merging alcohol concn is the elutriant of 20%-40%, after vacuum decompression concentrates (55 ℃-60 ℃), vacuum-drying, content is 54.3% crude product, total conversion rate is 80.4%, yield is 0.4%;
Get the crude product 8.0g that makes, the 200ml anhydrous alcohol solution by the alkali alumina adsorption column, is collected effluent liquid, and vacuum decompression concentrates (55 ℃-60 ℃) to proper volume, normal temperature crystallization, recrystallization 1-2 time, 1-DNJ highly finished product that must content 98.3%.
Embodiment 6
Get the ammoniacal liquor elutriant 3L among the embodiment 1, transfer to neutrality with hydrochloric acid;
Last column volume is the AB-8 macroporous resin column of 1L, wash 2 times of column volumes after, the ethanolic soln gradient elution that is 10-70% with 2 times of column volume concentration again, flow velocity is 1 times of column volume/h, substep is collected elutriant;
Merging alcohol concn is the elutriant of 20%-40%, after vacuum decompression concentrates (55 ℃-60 ℃), vacuum-drying, content is 58.3% crude product, total conversion rate is 87.5%, yield is 0.4%;
Get the crude product 8.0g that makes, the 200ml anhydrous alcohol solution by the alkali alumina adsorption column, is collected effluent liquid, and vacuum decompression concentrates (55 ℃-60 ℃) to proper volume, normal temperature crystallization, recrystallization 1-2 time, 1-DNJ highly finished product that must content 98.5%.
Content assaying method
1-DNJ assay of the present invention adopts high-efficient liquid phase technique, comprises following steps:
The HPLC condition: the C18 post, 25 ℃ of column temperatures, moving phase is acetonitrile: 0.1% aqueous acetic acid (35 ︰ 65), flow velocity 1ml/min detects wavelength 254nm.
Specimen preparation: get the 0.2g sample powder, the 250ml Erlenmeyer flask of packing into adds 0.05mol/LHCl solution by 50 times of amounts, supersound extraction 30min, and centrifugal, residue extracts once more as a rule, and is centrifugal, merges supernatant liquor, and distilled water is settled to 50ml.
Pre-column derivatization: get said extracted liquid 1OuL in the centrifuge tube of 1.5mL, add 1OuLK
3BO
3Damping fluid (pH8.5), the acetonitrile solution that adds 2OuL5mmol/L FMOC-Cl again, behind the mixing in 2O ℃ of water-bath 20min, the glycine that adds 1OuL0.1 mol/L, allow remaining derivatization reagent react, add the aqueous acetic acid of 950uL0.1% (V/V) at last, mixing, filter the sample introduction analysis with syringe filters (0.45um).
Claims (10)
1. method by extraction separation high purity 1-S-GI in the mulberry leaf is characterized in that comprising following sequential steps:
(1) gets the mulberry leaf pulverizing medicinal materials, sieve, must extract and use Mulberry Leaf;
(2) raw material powder extracts with water-containing solvent, filters the dregs of a decoction, and material is centrifugal, gets extracting solution;
(3) extracting solution is concentrated into no ethanol, ultrafiltration membrance filter;
(4) feed liquid is transferred pH to 3.0-4.0 with mineral acid, precipitation, centrifugal removal of impurities;
(5) strong acidic ion resin post on the acidifying feed liquid, the ammoniacal liquor wash-out is carried out in washing again, collects the pH9-12 elutriant, transfers to pH value neutrality with hydrochloric acid;
(6) macroporous resin column on the feed liquid, the Different concentrations of alcohol gradient elution is used in washing again, collects the target elutriant;
(7) target elutriant concentrating under reduced pressure, drying get crude product;
(8) crude product anhydrous alcohol solution, effluent liquid is collected in the removal of impurities of parlkaline adsorption column;
(9) effluent liquid concentrating under reduced pressure carries out normal temperature crystallization and recrystallization, obtains mass content and is higher than 98% 1-DNJ highly finished product.
2. according to the described method of claim 1, it is characterized in that: cross 40 mesh sieves in the step (1) after the mulberry leaf pulverizing medicinal materials by extraction separation high purity 1-S-GI in the mulberry leaf.
3. according to the described method by extraction separation high purity 1-S-GI in the mulberry leaf of claim 1, it is characterized in that: the water-containing solvent in the step (2) is mixed by water and ethanol and forms; Mineral acid is a hydrochloric acid in the step (4), and its mass concentration is 10%.
4. according to the described method by extraction separation high purity 1-S-GI in the mulberry leaf of claim 1, it is characterized in that: ultra-filtration membrane is the hollow cellulose acetate membrane in the step (3).
5. according to the described method of claim 1 by extraction separation high purity 1-S-GI in the mulberry leaf, it is characterized in that: resin cation (R.C.) is selected from model 002SC, D001,001 * 4,001 * 7 or 001 * 8 in the step (5), water and ammoniacal liquor elution volume are 3 times of column volumes, ammonia concn is 0.5-1.0%, and flow velocity is 0.5-1 times of column volume/h.
6. according to the described method of claim 1 by extraction separation high purity 1-S-GI in the mulberry leaf, it is characterized in that: macroporous resin is selected from model D101, HP20, AB-8, CAD-40, DM301 or HPD-400 in the step (6), water and ethanol elution volume are 2 times of column volumes, and flow velocity is 0.5-1 times of column volume/h.
7. according to the described method by extraction separation high purity 1-S-GI in the mulberry leaf of claim 1, it is characterized in that: resin cation (R.C.) is selected from model 001 * 8 in the step (5), and macroporous resin is selected from model AB-8 in the step (6).
8. according to the described method by extraction separation high purity 1-S-GI in the mulberry leaf of claim 1, it is characterized in that: vacuum decompression concentrates in the step (7), and drying temperature is 55-60 ℃.
9. according to the described method of claim 1, it is characterized in that: be provided with alkali alumina as alkaline adsorbent in step (8) the neutral and alkali adsorption column by extraction separation high purity 1-S-GI in the mulberry leaf.
10. according to the described method by extraction separation high purity 1-S-GI in the mulberry leaf of claim 1, it is characterized in that: vacuum decompression concentrates in the step (9), and thickening temperature is 55-60 ℃, naturally cooling, crystallization, recrystallization 1-2 time.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110038204A CN102101840B (en) | 2011-02-15 | 2011-02-15 | Method for extracting and separating high-purity 1-Deoxynojirimycin from folium mori |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110038204A CN102101840B (en) | 2011-02-15 | 2011-02-15 | Method for extracting and separating high-purity 1-Deoxynojirimycin from folium mori |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102101840A true CN102101840A (en) | 2011-06-22 |
| CN102101840B CN102101840B (en) | 2012-09-26 |
Family
ID=44154929
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201110038204A Expired - Fee Related CN102101840B (en) | 2011-02-15 | 2011-02-15 | Method for extracting and separating high-purity 1-Deoxynojirimycin from folium mori |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102101840B (en) |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102718697A (en) * | 2012-06-06 | 2012-10-10 | 浙江工业大学 | Method for preparing mulberry leaf 1-deoxynojirimycin extract with filter membrane and resin |
| CN104402801A (en) * | 2014-10-31 | 2015-03-11 | 西南大学 | Methods for separating DNJ (1-deoxynojirimycin) and preparing DNJ nanometer suspension |
| CN107162956A (en) * | 2017-06-30 | 2017-09-15 | 江苏耐雀生物工程技术有限公司 | A kind of method that 1 DNJ is extracted from mulberry leaf |
| 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 |
| CN111269171A (en) * | 2020-04-08 | 2020-06-12 | 劲牌持正堂药业有限公司 | Preparation method of high-purity 1-deoxynojirimycin |
| CN111533680A (en) * | 2020-05-28 | 2020-08-14 | 成都医学院 | Folium Mori extract and folium Mori multicomponent mixture with blood sugar lowering effect prepared from the same |
| CN111965278A (en) * | 2020-08-07 | 2020-11-20 | 广西壮族自治区蚕业技术推广站 | Kit and method for detecting content of 1-deoxynojirimycin in mulberry twigs |
| CN112300058A (en) * | 2020-12-03 | 2021-02-02 | 中国热带农业科学院热带作物品种资源研究所 | Method for extracting 1-deoxynojirimycin from fresh mulberry leaves |
| CN113929615A (en) * | 2021-11-02 | 2022-01-14 | 浙江珲达生物科技有限公司 | Purification method of nojirimycin |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101314586A (en) * | 2008-06-20 | 2008-12-03 | 江苏大学 | Method for separating 1-deoxidized nojirimycin monomer from mulberry leaf total alkaloid |
| CN101491579A (en) * | 2007-04-18 | 2009-07-29 | 北京和润创新医药科技发展有限公司 | Method for extracting mulberry leaf total alkaloid from mulberry leaf extract liquid |
| CN101654428A (en) * | 2009-09-11 | 2010-02-24 | 成都市金医生科技健康产业有限公司 | Method for extracting and separating 1-deoxynojirimycin with high purity from natural products |
-
2011
- 2011-02-15 CN CN201110038204A patent/CN102101840B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101491579A (en) * | 2007-04-18 | 2009-07-29 | 北京和润创新医药科技发展有限公司 | Method for extracting mulberry leaf total alkaloid from mulberry leaf extract liquid |
| CN101314586A (en) * | 2008-06-20 | 2008-12-03 | 江苏大学 | Method for separating 1-deoxidized nojirimycin monomer from mulberry leaf total alkaloid |
| CN101654428A (en) * | 2009-09-11 | 2010-02-24 | 成都市金医生科技健康产业有限公司 | Method for extracting and separating 1-deoxynojirimycin with high purity from natural products |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102718697A (en) * | 2012-06-06 | 2012-10-10 | 浙江工业大学 | Method for preparing mulberry leaf 1-deoxynojirimycin extract with filter membrane and resin |
| CN102718697B (en) * | 2012-06-06 | 2014-11-12 | 浙江工业大学 | Method for preparing mulberry leaf 1-deoxynojirimycin extract with filter membrane and resin |
| CN104402801A (en) * | 2014-10-31 | 2015-03-11 | 西南大学 | Methods for separating DNJ (1-deoxynojirimycin) and preparing DNJ nanometer suspension |
| CN104402801B (en) * | 2014-10-31 | 2016-06-15 | 西南大学 | Separate DNJ and the method preparing DNJ nano suspension |
| CN107162956A (en) * | 2017-06-30 | 2017-09-15 | 江苏耐雀生物工程技术有限公司 | A kind of method that 1 DNJ is extracted from mulberry leaf |
| 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 |
| CN111269171A (en) * | 2020-04-08 | 2020-06-12 | 劲牌持正堂药业有限公司 | Preparation method of high-purity 1-deoxynojirimycin |
| CN111269171B (en) * | 2020-04-08 | 2023-05-05 | 劲牌持正堂药业有限公司 | Preparation method of high-purity 1-deoxynojirimycin |
| CN111533680A (en) * | 2020-05-28 | 2020-08-14 | 成都医学院 | Folium Mori extract and folium Mori multicomponent mixture with blood sugar lowering effect prepared from the same |
| CN111965278A (en) * | 2020-08-07 | 2020-11-20 | 广西壮族自治区蚕业技术推广站 | Kit and method for detecting content of 1-deoxynojirimycin in mulberry twigs |
| CN112300058A (en) * | 2020-12-03 | 2021-02-02 | 中国热带农业科学院热带作物品种资源研究所 | Method for extracting 1-deoxynojirimycin from fresh mulberry leaves |
| CN113929615A (en) * | 2021-11-02 | 2022-01-14 | 浙江珲达生物科技有限公司 | Purification method of nojirimycin |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102101840B (en) | 2012-09-26 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102101840B (en) | Method for extracting and separating high-purity 1-Deoxynojirimycin from folium mori | |
| CN107362200B (en) | Method for extracting and separating alkaloid and flavone from mulberry leaves | |
| CN108314608A (en) | A kind of extraction separation method of cannabidiol | |
| CN101343305B (en) | Preparation method for astragaloside | |
| CN102399187B (en) | Preparation method of sinomenine | |
| CN102718697B (en) | Method for preparing mulberry leaf 1-deoxynojirimycin extract with filter membrane and resin | |
| CN106892949B (en) | A method of extracting separation glycyrrhizic acid, glycyrrhiza total flavonoid simultaneously based on continuous chromatography technology | |
| CN103204800B (en) | A kind of extracting method of 1 DNJ | |
| CN102453075A (en) | Separation and purification process of glycyrrhizic acid | |
| CN102964460A (en) | Method for continuously extracting and separating polysaccharides and 1-deoxynojirimycin from mulberry leaves | |
| CN105753917B (en) | A kind of isolation and purification method of liquiritin | |
| CN101348474A (en) | Method for preparing salvianolic acid B and tanshinol from Salvia miltiorrhiza stem | |
| CN103992260A (en) | Method for extracting indirubin from folium isatidis | |
| CN103180334B (en) | Prepare the method for lactone glucoside of Radix Paeoniae and peoniflorin | |
| CN102391115B (en) | Method for preparing honeysuckle flower extract by jointly adopting membrane separation and column chromatography | |
| CN101973985A (en) | Method for preparing mangiferin | |
| CN101759731B (en) | Extraction method of linseed gum and secoisolariciresin-ol diglucoside | |
| CN102276515B (en) | Method for extracting deoxynojirimycin | |
| CN1813834A (en) | Method for preparing total flavone extract of many prickle acanthopanax | |
| CN102329345A (en) | Method for extracting and purifying sarmentosin in Sedum sarmentosum Bunge | |
| CN102920727B (en) | Method for preparing extracts rich in vitexin rhamnoside and vitexin glucoside | |
| CN100418543C (en) | Double resin process for preparing high quality active gingko leaf component extract | |
| CN102697838B (en) | Method for extracting and separating flavone enrichment substance, saponin enrichment substance and polysaccharide from astragalus simultaneously | |
| CN105646620B (en) | The preparation method of fleabane flower A prime | |
| CN107235988A (en) | A kind of extracting method of qinghaosu and Artemisitene |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20120926 Termination date: 20180215 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |