CN102512503A - Separation method for flavonoid substances of Chinese toon leaves - Google Patents
Separation method for flavonoid substances of Chinese toon leaves Download PDFInfo
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- CN102512503A CN102512503A CN2011103717224A CN201110371722A CN102512503A CN 102512503 A CN102512503 A CN 102512503A CN 2011103717224 A CN2011103717224 A CN 2011103717224A CN 201110371722 A CN201110371722 A CN 201110371722A CN 102512503 A CN102512503 A CN 102512503A
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Abstract
The invention relates to a process for extracting organic substances, in particular to a separation method for the flavonoid substances of Chinese toon leaves, which comprises the following steps of: carrying out primary extracting by using an ethanol solution through thermal refluxing so as to obtain an ethanol extract, then hydrolyzing by using a sodium hydroxide solution, purifying, afterwards treating a water layer by using a hydrochloric acid solution, extracting by ethyl acetate, decompressing and distilling so as to obtain the coarse products of the flavonoid substances of the Chinese toon leaves. The separation method for the flavonoid substances of the Chinese toon leaves has the beneficial effects of high extracting efficiency, less equipment investment, quick starting of engineering, low cost and easy popularization.
Description
Technical field
The present invention relates to the Organic substance extraction process, especially relate to a kind of separation method of flavonoids from toona sinensis leaves.
Background technology
Tonnae Sinensis has another name called spring bud tree, Chinese toon, Ailanthus altissima, in " Zhiwu Mingshi Tukao ", is called toon, belongs to Meliaceae (Meliaceae) Cedrela deciduous tree; Be the peculiar precious fast growing wood of China, dish, medicine multipurpose seeds, deciduous tree, tree crown is huge; Leaf is in great numbers, and trunk is perfectly straight, and growth rapidly.Tonnae Sinensis has very high medical value, points out in the Compendium of Material Medica, and the leaf of Tonnae Sinensis, bud, root, skin and fruit all can be used as medicine.The modern medicine experimentation show has in the Folium toonae sinensis extract body regulate lipid metabolism, alleviate hyperglycemia, promote motility of sperm, delay hepatic fibrosis, effects such as cancer cell specific induction of apoptosis and the growth of inhibition sarcoma.Folium toonae sinensis extract also has antioxidation in vitro, antibiotic and to the effects such as poisoning, refusing to eat or repellent activity of insect in addition.One of main effective ingredient of Folium toonae sinensis is a flavone compound, and mainly the form with glycosides exists, and the flavone compound of having found mainly contains Quercetin-3-0-glucoside, Quercetin-3-0-rhamnoside, Quercetin-3-0-glucoside (6-1) rhamnose, kaempferol-3-0-glucoside, kaempferol-3-0-arabinose, 6; 7; 8,2 '-tetramethoxy-5,6 '-dihydroxyflavone, 5; 7-dihydroxy-8-methoxy flavone etc.; The aglycon of contained flavonol glycosides mainly is Quercetin, kaempferol, and is roughly the same with the contained flavone aglycone of Folium Ginkgo, and exceeds 2-3 doubly with total-flavonoid aglycone content in the season Folium toonae sinensis than the content in the Folium Ginkgo.
Flavone compound has wide biological activity, as protect the liver, antiinflammatory, antibiotic, antiviral, antitumor, antioxidation and to cardiovascular effect and estrogen-like effects.The existing extraction enrichment and separation method of flavone compound mainly contains methods such as organic solvent extraction, macroporous resin adsorption, the report of also useful aqueous two-phase and hyperfiltration process in the plant.
Summary of the invention
For accelerate development Folium toonae sinensis resource, it is reliable that the present invention aims to provide a kind of steady quality, the technology of the flavonoids from toona sinensis leaves of simple and convenient extraction.
The technical scheme that realizes above-mentioned purpose is following:
From the technology of Folium toonae sinensis extraction flavonoids from toona sinensis leaves, processing step is following:
(1) Folium toonae sinensis is dried, pulverize;
(2) dry powder carries out just carrying with the alcohol reflux of 50-95%, and solid-liquid ratio is 6-10 times, at 50-85 ℃ of backflow 1-2 hour, carries out distilling under reduced pressure again, and pressure is 0.08Mpa, and temperature is 40-50 ℃, reclaims solvent, obtains ethanol extract;
(3) ethanol extract is with the NaOH solution hydrolysising purification of 1%-5%, and the NaOH solution usage of 1%-5% is 4-6 a times of ethanol extract body, fully dissolves after-filtration, removes deposition;
(4) at room temperature with the petroleum ether extraction decolouring, remove petroleum ether layer;
(5) extract with ethyl acetate, the ethyl acetate consumption is 1: 1.5-1: 2, extract 5-6 time, and collect ethyl acetate layer;
(6) add HCl 3-10% solution, acidolysis is carried out in hot reflux, and the hot reflux temperature is 60-80 ℃, backflow 1-2 hour;
(7) add the isoflavone like substance of aqueous phase after the ethyl acetate extraction acidolysis in the water layer, the ethyl acetate consumption is 1: 1.5-1: 2, extracts collection ethyl acetate extraction layer 5-6 time;
(8) combined ethyl acetate extract layer carries out distilling under reduced pressure, and 0.08Mpa, obtains the flavonoids from toona sinensis leaves bullion by 40-50 ℃.
The preferred value of each parameter is in said extracted technology: the concentration of alcohol of hot reflux drawings just is 75%.The sodium hydrate aqueous solution concentration that is used for hydrolysising purification is 2%.Concentration of hydrochloric acid solution is 3% during acidolysis.The amount of ethanol solid-liquid ratio is 10 times when just carrying, and reflux temperature is 70 ℃, return time 1 hour.Reaction temperature is 60 ℃ during the HCl acidolysis, and the response time is 1 hour.
The flavonoids from toona sinensis leaves bullion is carried out HPLC to be detected; With the octadecylsilane chemically bonded silica post as chromatographic column; Phosphate aqueous solution and the acetonitrile solution of getting debita spissitudo respectively are as mobile phase, and through detecting, having incorporated Folium toonae sinensis flavone content of the same clan into can reach more than 20%.
The present invention has following beneficial effect: technology is simple, and extraction efficiency is high; Adopt common apparatus, establish money and lack, engineering starts fast; Cost is low, be easy to promote.
The specific embodiment
Through following examples technical scheme of the present invention is described further at present.
Embodiment 1
(1) Folium toonae sinensis is dried, pulverize;
(2) dry powder carries out just carrying with 75% alcohol reflux, and solid-liquid ratio is 10 times, refluxes 1 hour at 70 ℃, carries out distilling under reduced pressure again, and pressure is 0.08Mpa, and temperature is 45 ℃, reclaims solvent, obtains ethanol extract;
(3) ethanol extract is with NaOH 3% solution hydrolysising purification, and the NaOH solution usage is 5 times of ethanol extract volume, fully dissolves after-filtration, removes deposition;
(4) at room temperature with the petroleum ether extraction decolouring, remove petroleum ether layer;
(5) extract with ethyl acetate, the ethyl acetate consumption is 1: 1.5, extracts 5 times, collects ethyl acetate layer;
(6) add 3% hydrochloric acid solution, acidolysis is carried out in hot reflux, and the hot reflux temperature is 70 ℃, refluxes 1 hour;
(7) add the isoflavone like substance of aqueous phase after the ethyl acetate extraction acidolysis in the water layer, the ethyl acetate consumption is 1: 1.5, extracts collection ethyl acetate extraction layer 5 times;
(8) combined ethyl acetate extract layer carries out distilling under reduced pressure, and 0.08Mpa, obtains the flavonoids from toona sinensis leaves bullion by 45 ℃.
Embodiment 2
(1) Folium toonae sinensis is dried, pulverize;
(2) dry powder carries out just carrying with 95% alcohol reflux, and solid-liquid ratio is 8 times, refluxes 2 hours at 85 ℃, carries out distilling under reduced pressure again, and pressure is 0.08Mpa, and temperature is 50 ℃, reclaims solvent, obtains ethanol extract;
(3) ethanol extract is with NaOH 1% solution hydrolysising purification, and the NaOH solution usage is 6 times of ethanol extract volume, fully dissolves after-filtration, removes deposition;
(4) at room temperature with the petroleum ether extraction decolouring, remove petroleum ether layer;
(5) extract with ethyl acetate, the ethyl acetate consumption is 1: 2, extracts 6 times, collects ethyl acetate layer;
(6) add 10% hydrochloric acid solution, acidolysis is carried out in hot reflux, and the hot reflux temperature is 80 ℃, refluxes 2 hours;
(7) add the isoflavone like substance of aqueous phase after the ethyl acetate extraction acidolysis in the water layer, the ethyl acetate consumption is 1: 2, extracts collection ethyl acetate extraction layer 6 times;
(8) combined ethyl acetate extract layer carries out distilling under reduced pressure, and 0.08Mpa, obtains the flavonoids from toona sinensis leaves bullion by 50 ℃.
Embodiment 3
(1) Folium toonae sinensis is dried, pulverize;
(2) dry powder carries out just carrying with 50% alcohol reflux, and solid-liquid ratio is 6 times, refluxes 1.5 hours at 50 ℃, carries out distilling under reduced pressure again, and pressure is 0.08Mpa, and temperature is 40 ℃, reclaims solvent, obtains ethanol extract;
(3) ethanol extract is with NaOH 5% solution hydrolysising purification, and the NaOH solution usage is 4 times of ethanol extract volume, fully dissolves after-filtration, removes deposition;
(4) at room temperature with the petroleum ether extraction decolouring, remove petroleum ether layer;
(5) extract with ethyl acetate, the ethyl acetate consumption is 1: 2, extracts 6 times, collects ethyl acetate layer;
(6) add 5% hydrochloric acid solution, acidolysis is carried out in hot reflux, and the hot reflux temperature is 60 ℃, refluxes 1 hour;
(7) add the isoflavone like substance of aqueous phase after the ethyl acetate extraction acidolysis in the water layer, the ethyl acetate consumption is 1: 2, extracts collection ethyl acetate extraction layer 6 times;
(8) combined ethyl acetate extract layer carries out distilling under reduced pressure, and 0.08Mpa, obtains the flavonoids from toona sinensis leaves bullion by 40 ℃.
Claims (6)
1. the separation method of a flavonoids from toona sinensis leaves is characterized by: may further comprise the steps:
(1) Folium toonae sinensis is dried, pulverize;
(2) dry powder carries out just carrying with the alcohol reflux of 50%-95%, and solid-liquid ratio is 6-10 times, at 50-85 ℃ of backflow 1-2 hour, carries out distilling under reduced pressure again, and pressure is 0.08Mpa, and temperature is 40-50 ℃, reclaims solvent, obtains ethanol extract;
(3) ethanol extract is with the NaOH solution hydrolysising purification of 1%-5%, and the NaOH solution usage of 1%-5% is 4-6 a times of ethanol extract body, fully dissolves after-filtration, removes deposition;
(4) at room temperature with the petroleum ether extraction decolouring, remove petroleum ether layer;
(5) extract with ethyl acetate, the ethyl acetate consumption is 1: 1.5-1: 2, extract 5-6 time, and collect ethyl acetate layer;
(6) hydrochloric acid solution of adding 3%-10%, acidolysis is carried out in hot reflux, and the hot reflux temperature is 60-80 ℃, backflow 1-2 hour;
(7) add the Flavonoid substances of aqueous phase after the ethyl acetate extraction acidolysis in the water layer, the ethyl acetate consumption is 1: 1.5-1: 2, extracts collection ethyl acetate extraction layer 5-6 time;
(8) combined ethyl acetate extract layer carries out distilling under reduced pressure, and 0.08Mpa, obtains the flavonoids from toona sinensis leaves bullion by 40-50 ℃.
2. the separation method of flavonoids from toona sinensis leaves according to claim 1, the concentration of alcohol that it is characterized by hot reflux drawings just is 75%.
3. the separation method of flavonoids from toona sinensis leaves according to claim 1, it is characterized by the sodium hydrate aqueous solution concentration that is used for hydrolysising purification is 2%.
4. the separation method of flavonoids from toona sinensis leaves according to claim 1, concentration of hydrochloric acid solution is 3% when it is characterized by acidolysis.
5. the separation method of flavonoids from toona sinensis leaves according to claim 1 and 2, it is characterized by: the amount of ethanol solid-liquid ratio is 10 times when just carrying, reflux temperature is 70 ℃, return time 1 hour.
6. according to the separation method of claim 1 or 4 described flavonoids from toona sinensis leaves, reaction temperature is 60 ℃ when it is characterized by hydrochloric acidolysis, and the response time is 1 hour.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2011103717224A CN102512503A (en) | 2011-11-15 | 2011-11-15 | Separation method for flavonoid substances of Chinese toon leaves |
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| CN2011103717224A CN102512503A (en) | 2011-11-15 | 2011-11-15 | Separation method for flavonoid substances of Chinese toon leaves |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103931676A (en) * | 2013-01-17 | 2014-07-23 | 李德财 | Application of Chinese toon extract |
| CN105053367A (en) * | 2015-08-31 | 2015-11-18 | 福建省福鼎市名山茶叶有限公司 | Processing technology of Chinese mahogany leaf health tea |
-
2011
- 2011-11-15 CN CN2011103717224A patent/CN102512503A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103931676A (en) * | 2013-01-17 | 2014-07-23 | 李德财 | Application of Chinese toon extract |
| CN105053367A (en) * | 2015-08-31 | 2015-11-18 | 福建省福鼎市名山茶叶有限公司 | Processing technology of Chinese mahogany leaf health tea |
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Application publication date: 20120627 |