CN1317272C - Process for extracting folium mori flavone - Google Patents
Process for extracting folium mori flavone Download PDFInfo
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- CN1317272C CN1317272C CNB2005100123888A CN200510012388A CN1317272C CN 1317272 C CN1317272 C CN 1317272C CN B2005100123888 A CNB2005100123888 A CN B2005100123888A CN 200510012388 A CN200510012388 A CN 200510012388A CN 1317272 C CN1317272 C CN 1317272C
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- flavones
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Abstract
The present invention relates to a process for extracting folium mori flavone, which adopts folium mori powder as raw materials; alcohol and water are used as extraction solvent and eluting agents; macroporous resin is used as a separating material, and the content of the folium mori flavone in extract is larger than 50%. The present invention has the advantages of safe and nontoxic using solvent, low price, recycled and reused characteristic, no environmental pollution, large extraction quantity, industrialized production and high extraction efficiency.
Description
Technical field:
The present invention relates to a kind of extracting method that from the natural medicinal plant mulberry leaf, extracts its flavonoids effective constituent.
Background technology:
Mulberry leaf different name Herba adianti myriosori belongs to the leaf of mulberry (Morus alba L.) for Moraceae.Mulberry leaf are sweet, bitter, cold, return lung, Liver Channel, energy dispelling wind and heat pathogens, clearing away lung-heat and moistening dryness, clear liver and improve vision, in medical its treatment common cold due to wind-heat, lung-heat type cough, dizzy headache, hot eyes is dim-sighted, and modern pharmacology confirms that mulberry leaf can suppress blood sugar increasing, has the effect of prevention and treatment diabetes.Contain abundant phytomelin, Quercetin, Quercetol 3-monoglucoside and Quercetin-flavonoid compounds such as 3-glycoside in the mulberry leaf, content is about about 3%.Pharmaceutical research finds, flavones in mulberry leaves has stronger anti-oxidant function, hypolipemic function and the rat small intestine Disaccharide hydrolase is active to have a significant hypoglycemic activity by suppressing.In view of flavones in mulberry leaves has diversified biological activity, flavones in mulberry leaves has wide practical use as natural drug, natural antioxidants at medicine and field of food.To so far, the relevant extracting method report that from the medicinal plant mulberry leaf, extracts flavones in mulberry leaves in a large number of Shang Weijian, based on above reason, the present invention studies in great detail the extracting method of flavones in mulberry leaves.
Summary of the invention:
The purpose of this invention is to provide a kind of efficient height, pollution-free and flavones in mulberry leaves extracting method that can suitability for industrialized production.
Extracting method of the present invention comprises the steps:
(1) mulberry leaf are pulverized, used alcohol reflux, merge leaching liquid, leave standstill, filter, filtrate concentrating reclaimed ethanol, makes ethanol extraction medicinal extract;
(2) controlled temperature is 60～80 ℃, and water extracts repeatedly to ethanol extraction medicinal extract, does not have the flavones color reaction to extracting solution, and united extraction liquid leaves standstill, and filters, concentrate concentrated solution;
(3) concentrated solution with sour adjust pH to subacidity;
(4) add salts contg to 1%～5% that inorganic salt are adjusted solution;
(5) above-mentioned sample is with nonpolar or low-pole macroporous adsorbent resin column chromatography, and the abundant drip washing of first water is become clear, become faint yellowly by muddiness to leacheate, uses 2～5 column volumes of 30～70% ethanol drip washing again, collects leacheate, concentrates, is drying to obtain product.
Mulberry leaf described in the step (1) can be crushed to 20～50 orders, use alcohol reflux 3～4 times.The alcohol concn that described alcohol reflux uses is preferably 50%～80%.The extraction efficiency height of flavones in mulberry leaves like this, foreign matter content is low in the extracting solution.
The volume of the concentrated liquid described in the step (2) and mulberry leaf weight ratio be preferably: (4～8): 1 (v/w).
PH value described in the step (3) is 2～6, and in this acidity scope, macroporous adsorbent resin is to the adsorption efficiency height of flavones in mulberry leaves.
Inorganic salt described in the step (4) can be any one of sodium-chlor, sodium sulfate, ammonium sulfate etc.The adding of inorganic salt can improve the adsorption efficiency of macroporous adsorbent resin to flavones in mulberry leaves.
Macroporous adsorbent resin can be D described in the step (5)
101, D
1-10, among the AB-8 any, during column chromatography for separation, macroporous adsorbent resin bed volume and mulberry leaf usage ratio to be separated are preferably: (0.5～1): 1 (v/w).Macroporous resin column chromatography drip washing speed is preferably 1-5ml/cm
2.min.Macroporous adsorbent resin carries out the sepn process of post layer and can carry out 1-3 time, to satisfy the requirement of flavones in mulberry leaves content.The macroporous adsorbent resin reproducible utilization, as making resin regeneration with 95% ethanol drip washing cylinder, after the use repeatedly, the also available 3% soaking with sodium hydroxide drip washing of resin is again with a large amount of water wash regeneration.
The present invention has following advantage:
(1) the present invention uses solvent safety nontoxic, cheap recyclable usefulness again, environmentally safe.
(2) the present invention uses parting material to be macroporous adsorbent resin.Macroporous adsorbent resin is the class organic polymer sorbent material that development in recent years is got up, and it has absorption property preferably.For separating the effective means of the organic compound compound that especially polarity is big, shown unique effect at the aspects such as extraction of natural product chemistry composition.Not only physico-chemical property is stable for it, is insoluble to acid, alkali and organic solvent, and is better to the organism selectivity, the influence that not existed by inorganic salts and strong ion low molecular compound, and be easy to wash-out regeneration, can repeatedly utilize.
(3) adopt the present invention's extraction separation flavones in mulberry leaves from the medicinal plant mulberry leaf, extracted amount is big, but suitability for industrialized production.
(4) adopt the present invention's extraction separation flavones in mulberry leaves from the medicinal plant mulberry leaf, flavones content is greater than 50%, the extraction efficiency height.
Embodiment:
Embodiment 1:
Take by weighing the 500g mulberry leaf, pulverized 20 mesh sieves, three refluxing extraction of 3 liters, 2 liters, 2 liters branches of the ethanolic soln with 80%, refluxed first 2.0 hours, and secondary, refluxed united extraction liquid for three times respectively 1.0 hours, refrigeration was left standstill 24 hours, filter, filtrate decompression concentrate ethanol extraction; The ethanol extraction water extracts respectively five times, and each 500ml extracted 1 hour, and temperature remains on 75 ℃, merges aqueous extract, leaves standstill filtration, is evaporated to about 2 liters; With the hydrochloric acid adjust pH is 3.5; It is 3% that adding NaCl makes salts contg; The concentrated solution upper prop separates, and its post height is 60cm, and post directly is 3.0cm, and column packing is D
101Macroporous adsorbent resin, elder generation uses 5 times of column volumes of 40% ethanol drip washing instead after becoming clearly with water wash to effluent liquid, and drip washing speed is: 20ml/min, collect leacheate, concentrating under reduced pressure, vacuum-drying promptly get brown xanchromatic flavones in mulberry leaves product.With the rutin is reference substance, utilizes difference spectrophotometry to measure the content of total flavonoids of Folium Mori, and flavones in mulberry leaves content is 61%.
Embodiment 2:
Take by weighing the 1Kg mulberry leaf, pulverized 40 mesh sieves, three refluxing extraction of 5 liters, 4 liters, 4 liters branches of the ethanolic soln with 75%, refluxed first 2.0 hours, and secondary, refluxed united extraction liquid for three times respectively 1.0 hours, refrigeration was left standstill 24 hours, filter, filtrate decompression concentrate ethanol extraction; The ethanol extraction water extracts respectively five times, and each 800ml extracted 1 hour, and temperature remains on 75 ℃, merges aqueous extract, leaves standstill filtration; With the hydrochloric acid adjust pH is 4; It is 3% that adding NaCl makes salts contg; Upper prop separates, and its post height is 60cm, and post directly is 4.0cm, and column packing is D
101Macroporous adsorbent resin; After becoming clearly with water wash to effluent liquid earlier, use 4 times of column volumes of 50% ethanol drip washing instead, drip washing speed is: 25ml/min, collect leacheate, and concentrating under reduced pressure, vacuum-drying promptly get brown xanchromatic flavones in mulberry leaves product.With the rutin is reference substance, utilizes difference spectrophotometry to measure the content of total flavonoids of Folium Mori, and flavones in mulberry leaves content is 54%.
Embodiment 3:
Take by weighing the 500g mulberry leaf, pulverized 20 mesh sieves, three refluxing extraction of 3 liters, 2 liters, 2 liters branches of the ethanolic soln with 80%, refluxed first 2.0 hours, and secondary, refluxed united extraction liquid for three times respectively 1.0 hours, refrigeration was left standstill 24 hours, filter, filtrate decompression concentrate ethanol extraction; The ethanol extraction water extracts respectively five times, and each 500ml extracted 1 hour, and temperature remains on 75 ℃, merges aqueous extract, and leave standstill filtration, be evaporated to about 2 liters, be 3.5 with the hydrochloric acid adjust pH; It is 2% that adding NaCl makes salts contg; The concentrated solution upper prop separates, its post height is 60cm, post directly is 3.0cm, column packing is the AB-8 macroporous adsorbent resin, after becoming clearly with water wash to effluent liquid earlier, use 5 times of column volumes of 40% ethanol drip washing instead, drip washing speed is: 20ml/min, collect leacheate, concentrating under reduced pressure, vacuum-drying promptly get brown xanchromatic flavones in mulberry leaves product.With the rutin is reference substance, utilizes difference spectrophotometry to measure the content of total flavonoids of Folium Mori, and flavones in mulberry leaves content is 63%.
Claims (9)
1. a flavones in mulberry leaves extracting method is characterized in that comprising the steps:
(1) mulberry leaf are pulverized, use alcohol reflux, merge leaching liquid, leave standstill, filter, filtrate concentrated ethanol extraction medicinal extract;
(2) controlled temperature is 60～80 ℃, and water extracts repeatedly to ethanol extraction medicinal extract, does not have the flavones color reaction to extracting solution, and united extraction liquid leaves standstill, and filters, concentrate concentrated solution;
(3) concentrated solution with sour adjust pH to subacidity;
(4) add salts contg to 1%～5% that inorganic salt are adjusted solution;
(5) above-mentioned sample is with nonpolar or low-pole macroporous adsorbent resin column chromatography, and 2～5 column volumes of 30～70% ethanol drip washing are used in the abundant drip washing of first water again, collects leacheate, concentrates, is drying to obtain product.
2. a kind of flavones in mulberry leaves extracting method as claimed in claim 1 is characterized in that the alcohol concn that the described alcohol reflux of step (1) uses is 50%～80%.
3. a kind of flavones in mulberry leaves extracting method as claimed in claim 1 is characterized in that the volume and the mulberry leaf weight ratio of the described concentrated solution of step (2) is: (4～8): 1 (v/w).
4. a kind of flavones in mulberry leaves extracting method as claimed in claim 1 is characterized in that the described pH value of step (3) is 2～6.
5. a kind of flavones in mulberry leaves extracting method as claimed in claim 1 is characterized in that the described inorganic salt of step (4) are any one in sodium-chlor, sodium sulfate, the ammonium sulfate.
6. a kind of flavones in mulberry leaves extracting method as claimed in claim 1 is characterized in that described macroporous adsorbent resin bed volume of step (5) and mulberry leaf usage ratio to be separated are: (0.5～1): 1 (v/w).
7. a kind of flavones in mulberry leaves extracting method as claimed in claim 1 is characterized in that the described column chromatography drip washing of step (5) speed is 1-5ml/cm
2.min.
8. a kind of flavones in mulberry leaves extracting method as claimed in claim 1 is characterized in that the described column chromatography for separation chromatography of step (5) number of times is 1-3 time.
9. a kind of flavones in mulberry leaves extracting method as claimed in claim 1 is characterized in that the described macroporous adsorbent resin of step (5) is D
101, D
110, among the AB-8 any.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100123888A CN1317272C (en) | 2005-03-12 | 2005-03-12 | Process for extracting folium mori flavone |
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2005100123888A CN1317272C (en) | 2005-03-12 | 2005-03-12 | Process for extracting folium mori flavone |
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| CN1683360A CN1683360A (en) | 2005-10-19 |
| CN1317272C true CN1317272C (en) | 2007-05-23 |
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| CNB2005100123888A Expired - Fee Related CN1317272C (en) | 2005-03-12 | 2005-03-12 | Process for extracting folium mori flavone |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101153031B (en) * | 2006-09-27 | 2011-05-04 | 徐奎根 | Method for extracting proanthocyanidins |
| CN103159724A (en) * | 2013-04-09 | 2013-06-19 | 云南森源化工有限公司 | Method for simultaneously extracting australian tea tree flavone and beta-sitosterol |
| CN106619821A (en) * | 2015-10-28 | 2017-05-10 | 丹阳华都园艺有限公司 | Mulberry leaf flavonol extraction technology |
| CN105325907A (en) * | 2015-11-25 | 2016-02-17 | 吴军 | Processing method for low-salt ham |
| CN108208646A (en) * | 2017-12-22 | 2018-06-29 | 温州三特食品科技有限公司 | A kind of preparation method of hypoglycemic nutrient powder |
| CN113786642A (en) * | 2021-10-18 | 2021-12-14 | 山东一方制药有限公司 | A new method for extracting folium Mori by countercurrent extraction |
| CN116617292A (en) * | 2022-07-27 | 2023-08-22 | 广西中医药大学 | Method for preparing mulberry leaf flavone with in-vitro antioxidant activity |
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2005
- 2005-03-12 CN CNB2005100123888A patent/CN1317272C/en not_active Expired - Fee Related
Non-Patent Citations (1)
| Title |
|---|
| 桑叶黄酮类化合物提取方法研究 李莉，中国林副特产，第1卷 2003 * |
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| CN1683360A (en) | 2005-10-19 |
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