CN102138958A - Process for extracting and purifying flavonoids in grosvener siraitia plants - Google Patents
Process for extracting and purifying flavonoids in grosvener siraitia plants Download PDFInfo
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- CN102138958A CN102138958A CN 201110085319 CN201110085319A CN102138958A CN 102138958 A CN102138958 A CN 102138958A CN 201110085319 CN201110085319 CN 201110085319 CN 201110085319 A CN201110085319 A CN 201110085319A CN 102138958 A CN102138958 A CN 102138958A
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Abstract
The invention relates to the technical field of the extraction and purification of flavonoids in medicinal plants, in particular to a process for extracting and purifying flavonoids in grosvener siraitia plants. In the process, ethanol is used as extracting solvent, and extracting solution is purified by macroporous adsorbent resin. The process is characterized by comprising the following steps of: drying, chopping, performing reflux extraction by using the ethanol, filtering, concentrating, adsorbing by using a column, eluting by using water, eluting by using the ethanol, concentrating and drying, dissolving by using the ethanol, filtering, and concentrating and drying. The process has a simple flow, effective substances are high in content, the production cost can be reduced, energy can be saved, and environmental pollution can be controlled.
Description
Technical field
The present invention relates to the extraction purification technique field of medicinal plants flavones ingredient, be specifically related to the extraction and purification process of Momordica grosvenori plant flavones ingredient.
Background technology
Fructus Momordicae be Cucurbitaceae Fructus Momordicae platymiscium (
Siraitia grosvenorii(Swingle) fruit C. Jeffrey ex Lu et Z. Y. Zhang) is Chinese medicine.This natural resources of Chinese medicinal materials also is the distinctive economic plants in Guangxi, is of high nutritive value, and is widely used in medicine, beverage and the flavoring agent.This plant medicinal history among the people in Guangxi had more than 300 year, record in 2010 editions " Chinese pharmacopoeia, be Chinese medicine, effect with clearing heat and moistening lung, loosening bowel to relieve constipation, modern pharmacological research shows, Fructus Momordicae extract has biological activitys such as blood sugar lowering, antioxidation, and health ministry is listed it in first " be food be again the kind list of medicine " in.
Momordica grosvenori plant is tall and big, and branch and leaf are dense, and the utilization of past to Fructus Momordicae mainly is its fruit, and really leaf and rattan were discarded usually after the orchard worker plucked fruit, had caused certain waste.The present invention extracts flavones ingredient from depleted Momordica grosvenori plant, for the development and use of Momordica grosvenori plant resource and flavonoid extraction of active ingredients purification thereof provide a cover feasible technology.
Osmanthus north is among the people to be had leaf is dried the back in order to control the tradition of diseases such as chronic pharyngitis, chronic bronchitis.Have the people that the chemical constituent of Folium Momordicae is studied in recent years, find to contain aminoacid, tea polyphenols in the Folium Momordicae, reach chromocor compound, the glycoside unit of its chromocor compound is Quercetin and kaempferol, and this is consistent with glycosides million in the Lo Han Guo fruit.Find that by experiment in vitro the Momordica grosvenori leaf chromocor composition has very strong antioxidant activity, is better than the antioxidant BHT of synthetic, is a kind of good Natural antioxidant.Other has the people to observe toxicity after mice was taken Momordica grosvenori leaf chromocor in continuous seven days, all animals are strong as a result deposits, and does not see any toxicity, and the body weight natural rate of growth is 25.1%, its maximum dosage-feeding is 60.85g/kg as calculated, shows that Momordica grosvenori leaf chromocor toxicity is very little.
The present invention adopts ethanol as extraction solvent, and extracting solution is by purification with macroreticular resin, and the extract flavone constituents content that obtains is higher, and this extraction purification technique is not seen the related data report both at home and abroad.Its extraction and purification process flow process is simple, and active substance content is higher, has reduced production cost, has saved the energy, has reduced environmental pollution, meets the requirement of modernization of industry of Chinese materia medica.
The method that the present invention adopts positive quadraturing design test and single factor to combine, alcohol extraction technology and purification by macroporous resin technology to the flavones ingredient in the Momordica grosvenori plant have been carried out comprehensive and systematic research, obtained the reliable technique parameter, carried out the pilot scale checking, can be applicable to industrialization production, its extraction and purification process has stronger practical value.
Summary of the invention
The object of the present invention is to provide the extraction and purification process of a kind of efficient height, pollution-free and Momordica grosvenori plant flavones ingredient that can suitability for industrialized production.
Extraction and purification process of the present invention comprises the steps:
(1) with Momordica grosvenori plant chopping, be 40～80% alcohol reflux with the concentration of 6～10 times of volumes, extract 1～3 time, each 1～3 hour, the merging ethanol extract.
(2) concentrate ethanol extract, make amount of liquid medicine be concentrated into 2～5 times of quality of medicinal material, leave standstill filtration after, obtain filtrate.
(3) filtrate is regulated pH to 4 with 1mol/L HCl, and above sample liquid concentration is 0.1～0.6 g/mL, per hour the flow velocity of 3～5 times of bed volumes passes through macroporous adsorptive resins, earlier remove impurity with the water elution of 2～4 times of amount of resin, to be 30～65% ethanol carry out eluting with the flow velocity of 1～3 times of bed volume per hour to the concentration of 4～8 times of bed volumes of reuse, regulate medicinal liquid pH to 5～6 with ammonia, obtain eluent, be dried to Powdered then.
(4) extract powder being added concentration is 95% dissolve with ethanol, and the dissolving number of times is 3～5 times, refilters, and concentrates and drying, obtains the Momordica grosvenori plant flavone extract.
The present invention has the following advantages:
(1) the present invention uses ethanol as the extraction solvent safety non-toxic, cheap recyclable utilization, environmentally safe.
(2) adopt the present invention to utilize in the depleted Momordica grosvenori plant and extract flavone component, made full use of resource, protected environment.
(3) the present invention adopts the macroporous adsorbent resin technology to extract the purification effective part group, and it is simple to have technology, and cost is lower, and resin can use repeatedly, is fit to commercial production, meets the requirement of modernization of industry of Chinese materia medica.
(4) adopt the present invention to extract flavone from Momordica grosvenori plant, general flavone content is greater than 50%, the extraction efficiency height.
Concentration of alcohol described in the present invention is meant in the 100 mL volume ethanol aqueous solutions and contains the ethanol volume fraction.
The specific embodiment
The present invention will be helped to understand by following embodiment, but content of the present invention can not be limited.
Embodiment 1.
Get 12 kg Momordica grosvenori plants choppings, add concentration and be 40% alcohol reflux, extracts 3 times, be 2 hours the first time, and second, third time respectively is 1 hour, and consumption of ethanol is respectively 10 times of amounts of quality of medicinal material, 8 times of amounts, 6 times of amounts, merge extractive liquid.Extracting solution is concentrated into 2 times of quality of medicinal materials, sucking filtration must be gone up the sample medicinal liquid again.Regulate medicinal liquid pH to 4 with 1 mol/L HCl, and above sample liquid concentration is 0.4 g/mL, the application of sample flow velocity is that 3 Bv/h adsorb (the resin bed blade diameter length ratio is 1:8), after absorption finishes, with the distilled water of 3 times of resin volumes flow velocity eluting with 4 Bv/h, be 30% ethanol then with the concentration of 5 times of resin column volumes, carry out eluting with the flow velocity of 2 Bv/h, collect eluent, regulate medicinal liquid pH to 5～6 with ammonia.Eluent is concentrated and recovery ethanol, and the concentrated solution drying obtains the thick product of Momordica grosvenori plant flavones ingredient extract.Be 95% dissolve with ethanol 4 times then with extract powder concentration, the ethanol consumption is respectively 30 times, 20 times, 10 times, 10 times (the thick product amount of powder of flavones ingredient extract), filter, concentrate and reclaim ethanol, the concentrated solution drying obtains Momordica grosvenori plant flavones ingredient extract purified product.Through high pressure liquid phase analysis, Momordica grosvenori plant flavones ingredient content is 54.90%.
Embodiment 2.
Get the chopping of 5 kg Momordica grosvenori plants, the concentration that adds 8 times of quality of medicinal materials is 60% alcohol reflux, extracts 1 time, and extraction time is 2 hours.Again extracting solution is concentrated into 3 times of quality of medicinal materials, leave standstill filtration after, obtain filtrate.Regulate filtrate pH to 3～5 with 1 mol/L HCl, and above sample liquid concentration is 0.1g/mL, flow velocity is that 4 Bv/h pass through macroporous adsorptive resins, earlier with the distilled water of 4 times of resin volumes flow velocity eluting with 4 Bv/h, to be 50% ethanol carry out eluting with the flow velocity of 1 Bv/h to the concentration of 4 times of bed volumes of reuse, regulate medicinal liquid pH to 5～6 with ammonia, obtain ethanol elution.Eluent is concentrated and recovery ethanol, and the concentrated solution drying obtains the thick product of Momordica grosvenori plant flavones ingredient extract.Be 85% dissolve with ethanol 5 times then with extract powder concentration, the ethanol consumption is respectively 30 times, 20 times, 20 times, 10 times, 10 times (the thick product amount of powder of flavones ingredient extract), filter, concentrate and reclaim ethanol, the concentrated solution drying obtains Momordica grosvenori plant flavones ingredient extract purified product.Through high pressure liquid phase analysis, Momordica grosvenori plant flavones ingredient content is 51.49%.
Embodiment 3.
Get the chopping of 10 kg Momordica grosvenori plants, adding concentration is 80% alcohol reflux, extracts twice, is 2 hours for the first time, is 1 hour for the second time, and consumption of ethanol is respectively 10 times of amounts of quality of medicinal material, 6 times of amounts, merge extractive liquid.Again extracting solution is concentrated into 5 times of quality of medicinal materials, leave standstill filtration after, obtain filtrate.Regulate filtrate pH to 4 with 1mol/L HCl, and above sample liquid concentration is 0.5g/mL, flow velocity is that 5 Bv/h pass through macroporous adsorptive resins, use the flow velocity eluting of the distilled water of 2 times of resin volumes then with 4 Bv/h, being 40% ethanol with the concentration of 8 times of bed volumes at last carries out eluting with the flow velocity of 3Bv/h, regulate medicinal liquid pH to 5～6 with ammonia, obtain eluent.Eluent is concentrated and recovery ethanol, and the concentrated solution drying obtains the thick product of Momordica grosvenori plant flavones ingredient extract.Be 90% dissolve with ethanol 3 times then with extract powder concentration, the ethanol consumption is respectively 30 times, 20 times, 10 times (the thick product amount of powder of flavones ingredient extract), filters, reclaim ethanol, concentrate, the concentrated solution drying obtains Momordica grosvenori plant flavones ingredient extract purified product.Through high pressure liquid phase analysis, Momordica grosvenori plant flavones ingredient content is 51.61 ﹪.
Embodiment 4.
Get 15 kg Momordica grosvenori plants choppings, add concentration and be 70% alcohol reflux, extracts three times, be 2 hours the first time, and second, third time respectively is 1 hour, and consumption of ethanol is respectively 10 times of amounts of quality of medicinal material, 8 times of amounts, 6 times of amounts, merge extractive liquid.Again extracting liquid volume is concentrated into 2.5 times of quality of medicinal materials, sucking filtration must be gone up the sample medicinal liquid.Regulate medicinal liquid pH to 4 with 1mol/L HCl, and above sample liquid concentration is 0.6g/mL, the application of sample flow velocity is that 4 Bv/h adsorb (the resin bed blade diameter length ratio is 1:8), after absorption finishes, with the flow velocity flushing of the distilled water of 3 times of resin volumes with 4Bv/h, be 65% ethanol then with the concentration of 5 times of resin column volumes, carry out eluting with the flow velocity of 2Bv/h, collect eluent, regulate eluent pH to 5～6 with ammonia.Eluent is concentrated and recovery ethanol, and the concentrated solution drying obtains the thick product of Momordica grosvenori plant flavones ingredient extract.Be 70% dissolve with ethanol 4 times then with extract powder concentration, each ethanol consumption is 20 times (the thick product amount of powder of flavones ingredient extract), filters, and concentrates and reclaim ethanol, the concentrated solution drying obtains Momordica grosvenori plant flavones ingredient extract purified product.Through high pressure liquid phase analysis, Momordica grosvenori plant flavones ingredient content is 54.52%.
Claims (7)
1. Momordica grosvenori plant flavones ingredient extraction process is characterized in that may further comprise the steps: drying, chopping, alcohol reflux, filtration and concentrate, post absorption, water elution, ethanol elution, concentrate and dry, dissolve with ethanol and filtration after concentrate drying.
2. a kind of Momordica grosvenori plant flavones ingredient extraction process as claimed in claim 1, it is characterized in that the used amount of alcohol of described alcohol reflux is 6～10 times of quality of medicinal material, used ethanol concentration of volume percent is 40～80%, extraction time is 1～3 time, and each extraction time is 1～3 hour.
3. a kind of Momordica grosvenori plant flavones ingredient extraction process as claimed in claim 1 is characterized in that the absorption of described post is meant that sample solution concentration is 0.1～0.6 g/mL, and flow velocity adsorbs by macroporous adsorptive resins for 3～5 times of bed volumes per hour.
4. a kind of Momordica grosvenori plant flavones ingredient extraction process as claimed in claim 1 is characterized in that described water elution is meant with the purified water eluting macroporous resin of 2～4 times of bed volumes to remove impurity.
5. a kind of Momordica grosvenori plant flavones ingredient extraction process as claimed in claim 1, it is characterized in that described ethanol elution is meant that concentration of volume percent with 4～8 times of bed volumes is 30～65% ethanol, carry out eluting with the flow velocity of 1～3 times of bed volume per hour.
6. a kind of Momordica grosvenori plant flavones ingredient extraction process as claimed in claim 1 is characterized in that described dissolve with ethanol is meant that with concentration of volume percent be 70～95% dissolve with ethanols, and the dissolving number of times is 3～5 times.
7. a kind of Momordica grosvenori plant flavones ingredient extraction process as claimed in claim 1 is characterized in that described Momordica grosvenori plant comprises leaf, rattan and the root of Fructus Momordicae.
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| CN 201110085319 CN102138958A (en) | 2011-04-06 | 2011-04-06 | Process for extracting and purifying flavonoids in grosvener siraitia plants |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104798964A (en) * | 2015-05-21 | 2015-07-29 | 叶长东 | Momordica grosvenori and gynostemma pentaphylla tea |
| CN104798965A (en) * | 2015-05-21 | 2015-07-29 | 叶长东 | Siraitia grosvenorii and chrysanthemum tea |
| CN106866759A (en) * | 2017-03-28 | 2017-06-20 | 广西甙元植物制品有限公司 | The technique that grosvenor momordica flavonoid is produced from the waste liquid of Momordica-Glycosides decolorizing resin post discharge |
| CN109021046A (en) * | 2018-09-28 | 2018-12-18 | 湖南华诚生物资源股份有限公司 | A method of extracting quercitin and mountain naphthalene glycosides simultaneously from Siraitia grosvenorii cauline leaf |
| CN109674843A (en) * | 2019-01-30 | 2019-04-26 | 湖南绿蔓生物科技股份有限公司 | A kind of method for extraction and purification of dried fructus momordicae comprehensive utilization |
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| CN1611498A (en) * | 2003-10-28 | 2005-05-04 | 广西师范大学 | Grosvenor momordical flavone and its preparing prcess |
| CN101147751A (en) * | 2006-09-19 | 2008-03-26 | 周英 | Method for extracting biologically active component from momordica grosvenori plant |
| CN101386636A (en) * | 2007-09-14 | 2009-03-18 | 桂林市振达生物科技有限责任公司 | Mogroside extraction method from grosvenor momordica |
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2011
- 2011-04-06 CN CN 201110085319 patent/CN102138958A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1611498A (en) * | 2003-10-28 | 2005-05-04 | 广西师范大学 | Grosvenor momordical flavone and its preparing prcess |
| CN101147751A (en) * | 2006-09-19 | 2008-03-26 | 周英 | Method for extracting biologically active component from momordica grosvenori plant |
| CN101386636A (en) * | 2007-09-14 | 2009-03-18 | 桂林市振达生物科技有限责任公司 | Mogroside extraction method from grosvenor momordica |
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| 《食品研究与开发》 20061231 陈全斌等 《罗汉果叶黄酮抗氧化能力研究》 189-191 1-7 第27卷, 第10期 * |
| 《食品科技》 20101130 梁英等 《罗汉果叶总黄酮的提取及清除自由基活性研究》 211-214 1-7 第35卷, 第11期 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104798964A (en) * | 2015-05-21 | 2015-07-29 | 叶长东 | Momordica grosvenori and gynostemma pentaphylla tea |
| CN104798965A (en) * | 2015-05-21 | 2015-07-29 | 叶长东 | Siraitia grosvenorii and chrysanthemum tea |
| CN104798964B (en) * | 2015-05-21 | 2017-05-31 | 叶长东 | A kind of Momordica grosvenori and gynostemma pentaphylla tea |
| CN104798965B (en) * | 2015-05-21 | 2017-06-06 | 叶长东 | A kind of Momordica grosvenori and chrysanthemum tea |
| CN106866759A (en) * | 2017-03-28 | 2017-06-20 | 广西甙元植物制品有限公司 | The technique that grosvenor momordica flavonoid is produced from the waste liquid of Momordica-Glycosides decolorizing resin post discharge |
| CN106866759B (en) * | 2017-03-28 | 2019-09-10 | 湖南华诚生物资源股份有限公司 | The technique of grosvenor momordica flavonoid is produced from the waste liquid that Momordica-Glycosides decolorizing resin column is discharged |
| CN109021046A (en) * | 2018-09-28 | 2018-12-18 | 湖南华诚生物资源股份有限公司 | A method of extracting quercitin and mountain naphthalene glycosides simultaneously from Siraitia grosvenorii cauline leaf |
| CN109674843A (en) * | 2019-01-30 | 2019-04-26 | 湖南绿蔓生物科技股份有限公司 | A kind of method for extraction and purification of dried fructus momordicae comprehensive utilization |
| CN109674843B (en) * | 2019-01-30 | 2022-03-22 | 湖南绿蔓生物科技股份有限公司 | Extraction and purification method for comprehensively utilizing dried momordica grosvenori |
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Application publication date: 20110803 |