CN104644702A - Method for enrichment and purification of suaeda heteroptera stem and leaf total flavonoids employing macroporous resin - Google Patents
Method for enrichment and purification of suaeda heteroptera stem and leaf total flavonoids employing macroporous resin Download PDFInfo
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- CN104644702A CN104644702A CN201510015606.7A CN201510015606A CN104644702A CN 104644702 A CN104644702 A CN 104644702A CN 201510015606 A CN201510015606 A CN 201510015606A CN 104644702 A CN104644702 A CN 104644702A
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Abstract
The invention discloses a method for enrichment and purification of suaeda heteroptera stem and leaf total flavonoids employing macroporous resin. The method is characterized by comprising the following specific steps: (1) crushing dried suaeda heteroptera stem and leaf, screening through a 20-mesh sieve, adding an extraction agent which is 8-12fold of weight of the suaeda heteroptera stem and leaf, extracting by a reflux extraction method for 2-3 times, wherein the extraction agent is ethanol of which the concentration is 50%-90%, extracting for 1-2 hours each time, filtering by virtue of 200-300mesh filter cloth, and merging extract liquids; (2) concentrating the extract liquids obtained from the step (1) until the mass concentration of the total flavonoids is 0.5-3.0mg/mL, adjusting the pH of a concentrated liquid to be 5-6 with diluted hydrochloric acid, loading the concentrated liquid by virtue of the macroporous resin at the flow rate of 1.0mL/min, wherein the maximal loading amount 1.5fold column volume, firstly, washing after loading, washing with ethanol, and eluting with 70% of ethanol of which the concentration is 5-fold column volume at the flow rate of 2.0mL/min; and (3) collecting an ethanol eluent, evaporating, concentrating and drying to obtain the required target. The method has the beneficial effects that the method is simple in process, low in cost, easy to operate, and high in efficiency; the content of total flavonoids in the purified extract exceeds 20%; and the method has further development and utilization value.
Description
Technical field
The present invention relates to a kind of preparation method of effective ingredients in plant, particularly relate to a kind of method of purification total flavones from Suaeda heteroptera stem and leaf.
Background technology
Suaeda heteroptera (Suaedasalsa), have another name called salt and inhale dish, Suaeda salsa, belonging to Centrospermae, Li Ke (Chenopodiaceac), Suaeda (SuaedaForsk), is annual salt tolerant humidogene herbosa.Suaeda heteroptera, for habitat change quite sensitive, is the indicative plant of northern seashore wetland variation of ecology and environment.And at Dongying, have the custom of edible Suaeda heteroptera.Its tender Seedling can supply cooked food.Pluck the seedling before blooming summer, after cleaning, lower boiling water pot is scalded, can cold and dressed with sauce, boil in water for a while, then dress with soy, vinegar, etc., fry, filling processed, cook soup etc.Suaeda heteroptera has plurality of health care functions: containing several mineral materials, and its composition meets human body needs.In addition containing abundant dietary fiber, can wriggle by stimulating gastrointestinal, help digest, the diseases such as rectal cancer, diabetes, cholelithiasis, hemorrhoid can be prevented.
Flavone compound is ubiquitous secondary metabolites in plant, has physiological effect and the pharmacological action of multiple beneficial.Research finds that flavone compound has protection cardiovascular system, hepatoprotective, antitumor, antiviral, anti-peptic ulcer, analgesia, cough-relieving, the important medical value such as to relieving asthma; also can be used as the natural additive of food, cosmetics; also there is the biological activity such as scavenging free radicals, antioxidation; using value is extensive, and market development potential is very large.Mainly from Folium Ginkgo, Semen sojae atricolor, Folium Crataegi, Folium Nelumbinis, leaf of Herba Apii graveolentis, Herba Oenanthes Javanicae, Pericarppium arachidis hypogaeae etc., extract flavone compound both at home and abroad at present, wherein especially deep with the research of Semen Ginkgo and Semen sojae atricolor.But, to Suaeda heteroptera Flavone class thing Quality Research rarely seen report.
Macroporous adsorbent resin is that a class does not contain cation exchange groups and has the preparation of macroporous structure, and aperture and specific surface area are all larger.Compared with gel resin and natural adsorbent, macroporous adsorbent resin has that adsorption capacity is large, adsorption rate is fast, selectivity is good, be easy to the advantages such as desorption, mechanical strength is high, Regeneration Treatment is easy, be particularly suitable for from aqueous solution, be separated low polarity or nonpolar compound, be widely used in recent years in the extracting and developing purification work of Chinese herbal medicine effective ingredients.
The present invention for raw material with Suaeda heteroptera stem and leaf, adopts Amberlyst process enriching and purifying main component flavone compound wherein, makes such component content in the extract after purification reach more than 20%, for the comprehensive development and utilization of Suaeda heteroptera stem and leaf resource lays the foundation.
Summary of the invention
The object of the invention is to be to provide a kind of technique simple, cost is low, the method for a kind of macroporous resin enrichment purification Suaeda heteroptera stem leaf total flavones that purification efficiency is high
Technical scheme of the present invention is: a kind of method of macroporous resin enrichment purification Suaeda heteroptera stem leaf total flavones, it is characterized in that: concrete steps are as follows: 1) get dry Herba suadeae glaucae stem and leaf, pulverize, cross 20 mesh, add Suaeda heteroptera stem and leaf weight 8-12 extraction reagent doubly, adopt reflux extraction to extract 2-3 time, described extraction reagent is the ethanol within the scope of concentration 50-90%, each extraction 1-2 hour, with 200-300 order filter-cloth filtering, merge extractive liquid;
2) extracting solution that step (1) obtains is concentrated into total flavones mass concentration 0.5-3.0mg/mL, concentrated solution pH to 5-6 is adjusted with dilute hydrochloric acid, adopt macroporous resin, by concentrated solution loading, loading flow velocity 1.0mL/min, maximum applied sample amount is 1.5 times of column volumes, first washes, and then wash with ethanol after completion of the sample.Be the ethanol of 70% by 5 times of column volume concentration, elution flow rate is 2.0mL/min;
3) ethanol elution is collected, evaporation and concentration, dry, be required target.
In described step (2), macroporous resin selects HPD-100, HPD-400, HPD600, HPD-700, D-101, AB-8, preferred HPD-100, HPD-400, most preferably D-101.
In described step (2), extracting solution concentrate is transparence yellowish-brown liquid.
Obtain the Suaeda heteroptera stem leaf total flavones mass content >20% of purification.
Compared with prior art, tool has the following advantages and good effect in the present invention:
Present invention process is simple, and cost is low, easy to operate, and efficiency is high, with D101(AB-8) macroporous adsorbent resin is adsorbent, sample solution flow velocity is 1.0mL/min, and sample solution concentration is 0.5-3.0mg/mL, when pH value is 5, has best adsorption effect; When eluent is 70% ethanol, eluent flow rate is 2mL/min, when eluent consumption is 5BV, has best parsing effect.In extract after purification, general flavone content is more than 20%, has the value developed further.
Detailed description of the invention
Following illustrative example is done more specifically and detailed description foregoing of the present invention.But this should be interpreted as that the scope of the above-mentioned theme of the present invention is only limitted to following instance.
Embodiment 1:
The Suaeda heteroptera stem and leaf pulverizer of oven dry is pulverized, cross 10 object sieves, the ethanol adding 50% of raw material weight 8 times is to the raw material reflux, extract, after pulverizing 3 times, each extraction 2 hours, filter, merging filtrate, ethanol is reclaimed to the extracting solution concentrating under reduced pressure after filtering, detect concentrated concentration to macroporous resin sample concentration, i.e. total flavones mass concentration 1.5mg/mL, extracting solution concentrate is transparence brown color liquid, adjust concentrated solution pH to 5-6, solution is joined in D101 (AB-8) macroporous resin column and carry out saturated adsorption, loading flow velocity 1.0mL/min, maximum applied sample amount is 1.5 times of column volumes, first with the water elution removing impurity of 5 times of column volumes, use 70% ethanol of 5 times of column volumes as eluant again, recycling design and concentration are carried out to eluant, finally carry out drying, the Suaeda heteroptera stem leaf total flavones mass content obtaining purification reaches 22%.
Embodiment 2:
The Suaeda heteroptera stem and leaf pulverizer of oven dry is pulverized, 10 object sieves, the ethanol adding 70% of raw material weight 10 times is to the raw material reflux, extract, after pulverizing 3 times, each extraction 2 hours, filter, merging filtrate, ethanol is reclaimed to the extracting solution concentrating under reduced pressure after filtering, detect concentrated concentration to macroporous resin sample concentration, i.e. total flavones mass concentration 2.4mg/mL, extracting solution concentrate is transparence brown color liquid, adjust concentrated solution pH to 5-6, solution is joined in D101 macroporous resin column and carry out saturated adsorption, loading flow velocity 1.0mL/min, maximum applied sample amount is 1.5 times of column volumes, first with the water elution removing impurity of 5 times of column volumes, use 70% ethanol of 5 times of column volumes as eluant again, recycling design and concentration are carried out to eluant, finally carry out drying, the Suaeda heteroptera stem leaf total flavones mass content obtained after purification reaches 24%.
Embodiment 3:
The Suaeda heteroptera stem and leaf pulverizer of oven dry is pulverized, cross 10 object sieves, the ethanol adding 90% of raw material weight 12 times is to the raw material reflux, extract, after pulverizing 3 times, each extraction 2 hours, filter, merging filtrate, ethanol is reclaimed to the extracting solution concentrating under reduced pressure after filtering, detect concentrated concentration to macroporous resin sample concentration, i.e. total flavones mass concentration 3.6mg/mL, extracting solution concentrate is transparence brown color liquid, adjust concentrated solution pH to 5-6, solution is joined D101(AB-8) carry out saturated adsorption in macroporous resin column, loading flow velocity 1.0mL/min, maximum applied sample amount is 1.5 times of column volumes, first with the water elution removing impurity of 5 times of column volumes, use 70% ethanol of 5 times of column volumes as eluant again, recycling design and concentration are carried out to eluant, finally carry out drying, the Suaeda heteroptera stem leaf total flavones mass content obtaining purification reaches 27%.
Claims (4)
1. the method for a macroporous resin enrichment purification Suaeda heteroptera stem leaf total flavones, it is characterized in that: concrete steps are as follows: 1) get dry Herba suadeae glaucae stem and leaf, pulverize, cross 20 mesh, add Suaeda heteroptera stem and leaf weight 8-12 extraction reagent doubly, adopt reflux extraction to extract 2-3 time, described extraction reagent is the ethanol within the scope of concentration 50-90%, each extraction 1-2 hour, with 200-300 order filter-cloth filtering, merge extractive liquid;
2) extracting solution that step (1) obtains is concentrated into total flavones mass concentration 0.5-3.0mg/mL, concentrated solution pH to 5-6 is adjusted with dilute hydrochloric acid, adopt macroporous resin, by concentrated solution loading, loading flow velocity 1.0mL/min, maximum applied sample amount is 1.5 times of column volumes, first washes, and then wash with ethanol after completion of the sample; Be the ethanol of 70% by 5 times of column volume concentration, elution flow rate is 2.0mL/min;
3) ethanol elution is collected, evaporation and concentration, dry, be required target.
2. the method for total flavones in a macroporous resin enrichment purification Suaeda heteroptera stem and leaf, it is characterized in that: in described step (2), macroporous resin selects HPD-100, HPD-400, HPD600, HPD-700, D-101, AB-8, preferred HPD-100, HPD-400, most preferably D-101.
3. the method for a kind of macroporous resin enrichment purification Suaeda heteroptera stem leaf total flavones according to claim 1, is characterized in that: in described step (2), extracting solution concentrate is transparence yellowish-brown liquid.
4. the method for a kind of macroporous resin enrichment purification Suaeda heteroptera stem leaf total flavones according to claim 1, is characterized in that: the Suaeda heteroptera stem leaf total flavones mass content >20% obtaining purification.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105769947A (en) * | 2016-05-26 | 2016-07-20 | 佛山科学技术学院 | Method for extracting flavone in cratoxylum cochinchinense |
| CN112939826A (en) * | 2021-02-05 | 2021-06-11 | 浙江工业大学 | Method for extracting and separating mesotrione from reaction liquid by using macroporous adsorption resin |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2005154411A (en) * | 2003-11-27 | 2005-06-16 | Sarusu Biotech Corp | Composition for preventing/removing hangover |
| CN101040711A (en) * | 2006-03-24 | 2007-09-26 | 孙贻超 | The application of Suaeda plant extraction in the food having health-care and weight-losing functions |
-
2015
- 2015-01-13 CN CN201510015606.7A patent/CN104644702A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005154411A (en) * | 2003-11-27 | 2005-06-16 | Sarusu Biotech Corp | Composition for preventing/removing hangover |
| CN101040711A (en) * | 2006-03-24 | 2007-09-26 | 孙贻超 | The application of Suaeda plant extraction in the food having health-care and weight-losing functions |
Non-Patent Citations (1)
| Title |
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| 牟浩: ""盐地碱蓬黄酮的分离提取及抗氧化活性的研究"", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105769947A (en) * | 2016-05-26 | 2016-07-20 | 佛山科学技术学院 | Method for extracting flavone in cratoxylum cochinchinense |
| CN112939826A (en) * | 2021-02-05 | 2021-06-11 | 浙江工业大学 | Method for extracting and separating mesotrione from reaction liquid by using macroporous adsorption resin |
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