CN102058634B - Method for extracting and purifying total flavonoids of sea buckthorn - Google Patents
Method for extracting and purifying total flavonoids of sea buckthorn Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 30
- 235000003145 Hippophae rhamnoides Nutrition 0.000 title claims abstract description 15
- 229930003935 flavonoid Natural products 0.000 title description 11
- 235000017173 flavonoids Nutrition 0.000 title description 11
- 150000002215 flavonoids Chemical class 0.000 title description 8
- 240000000950 Hippophae rhamnoides Species 0.000 title 1
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Abstract
The invention discloses a method for extracting and purifying seabuckthorn flavone, which comprises the following steps: providing raw materials, degreasing, dilute alkali extraction, filtering, regulating pH of filtrate, centrifugal separation, carrying out alcohol-soluble ultrasonic extraction on precipitates, carrying out centrifugal separation, recovering ethanol, diluting by adding pure water and adding a clarifying agent for treatment, carrying out centrifugal separation, carrying out resin adsorption on clear liquid, washing by water, carrying out ethanol elution, concentrating eluent, and drying to obtain a product. Optimizing the conditions of each step, and finally forming a complete set of seabuckthorn leaf flavone extraction and purification engineering; the process is not an alcohol or water extraction process, and is not a simple alkali extraction process, because the process comprises the steps of ultrasonic alcohol dissolving and the like, and the complete process is not recorded in the prior art.
Description
Technical field:
The present invention relates to the flavones chemical substance and extract the purifying field, especially relate to the method that a kind of Fructus Hippophae total flavones extracts purifying.
Background technology:
Flavones: its full name should be " a Vitamin P complex material ", extensively is present in nature, and its kind has been found about 3000 kinds; Its molecular structure all has the polyphenol compound of C6C3C6, between two aromatic nucleus (A, B ring), links to each other with three carbochains, and above common structure adds that different side-chain radicals forms the glucoside unit of different types of glucoside kind; As: Quercetin, Isorhamnetol, kaempferol, myricetin; Apigenin or the like; These different glucoside units connect with different carbohydrate molecules again, as: glucose, rhamnosyl, Chinese scholartree disaccharides, vicianose or the like, so formed thousands of kinds of flavonoid compounds.Past is referred to as vitamin P to them, and plant polyphenol kind is included into these compounds in scientific circles now, so flavonoid compound is big family members in the plant polyphenol kind.Flavonoid substances is in close relations to HUMAN HEALTH, is one type of good antioxidant, has now found that in seabuckthorn plant, to contain 32 kinds of flavonoid compounds (flavonoid glycoside), and a lot of medium-height grass the effective elements of the medicines also are flavonoid substances.
Production technique for Fructus Hippophae flavone in the prior art is mainly alcohol extracting-water precipitating shallow lake method (hereinafter to be referred as alcohol extracting), and its process step comprises: degreasing, alcohol reflux; Filter; Concentrate, again with ethyl acetate to lixiviate liquid concentrator dissolution filter, purifying, concentrate, dried finished.And the shortcoming of this method is, because the price of edible ethanol is per ton greater than 7000 yuan now, causes the Fructus Hippophae flavone of producing with pure extracting method, and its cost has surpassed 1200 yuan/KG, and cost can be in any more, makes Fructus Hippophae flavone produce difficulty greatly.
Also have in the prior art and make raw material, carried out the technical study of flooding (putting forward) Folium Hippophae total flavones hereinafter to be referred as water with Folium Hippophae.Its technology comprises: with the Folium Hippophae cleaning and removing impurities, drying and crushing is then used petroleum ether degreasing then, and the hot water lixiviate is filtered, and filtrating is transferred PH, and deposition is washed to neutral, ethanol drip washing then, and will filtrate concentrates, deposition, filtration, drying obtains product at last.A this method object lesson in the prior art is following:
A. the degreasing of Folium Hippophae: get the Folium Hippophae of 190 gram impurity elimination drying and crushing, after 1 hour, 75 ℃ were refluxed 1 hour with 400 milliliters of sherwood oils (boiling range 60-90 ℃) immersion, filtered the posterior lobe slag and refluxed 1 hour with 200 milliliters of sherwood oils, refiltered.
B. water extraction: the volatilization of degreasing posterior lobe slag adds 1500 ml waters behind the sherwood oil to the greatest extent soaked 30 minutes, refluxed 30 minutes, filtered, and filter residue is used 900 milliliters more respectively, and 600 ml waters respectively refluxed 30 minutes, and filtrating is cooled to room temperature after merging, and gets aqueous extract.
C. transfer pH value to isolate the crude flavonoid powder glycosides, regulate the pH value of aqueous extract with 1: 1 hydrochloric acid, because of flavonoid glycoside solubleness under acidic conditions little; The usable acid deposition is separated out it; But acidity should not be strong excessively, in order to avoid generate melt salt and hydrolysis takes place, the flavonoid glycoside (TFH) of separating out dissolved again.Experiment learns that when the extracting solution pH value was 3, TFH yield value was the highest, and the flavones yield reaches 1.05%.
D.30% ethanol drip washing gets product: contain protein in the crude flavonoid powder glycosides, Polyphenols impurity such as polysaccharide and cyanidin(e) with 30% ethanol drip washing, can reduce the interference impurity that is dissolved in high density alcohol like this, and little to the dissolving influence of flavonoid glycoside.
Yet be merely 8.4% with " water is carried " method products obtained therefrom content flavones, clutch lattice product (18%) is too far away, and yield (1.05%) also on the low side, no production meaning.
Summary of the invention:
The objective of the invention is to overcome the defective that above-mentioned technology exists, a kind of inexpensive extracting and purifying method of Fructus Hippophae total flavones efficiently is provided.
Because 4 kinds of contained Flavone aglycones in the leaf of Fructus Hippophae flavone: Quercetin, kaempferol, Isorhamnetol and myricetin (also claiming ampelopsin); All contain abundant phenolic hydroxyls in its molecular structure, can with the alkali salify after water-soluble, be that these aglycons all become glycoside to exist in the natural hippophae leaf; They all are connected with several different glycan molecules, have increased so more that it is water-soluble, and the contriver finds after a large amount of experiments and repeated validation; Extract with diluted alkaline water, can improve yield greatly.Extremely rare alkali lye replaces ethanol, and its cost is higher slightly little by little than water, and ethanol (95% concentration) present price is wanted more than 7000 yuan/ton; If use 70% extraction using alcohol, per ton also wanting more than 5000 yuan, and the valency of water per ton be several units; The difference of cost has more than 1000 times, thereby greatly reduces extraction cost.
A kind of method of Fructus Hippophae total flavones extraction purifying comprises the step of next coming in order: supply raw materials, degreasing is extracted, and filters, and filtrating is regulated pH; Spinning, throw out are carried out alcohol and are dissolved ultrasonic extraction, and ethanol is reclaimed in spinning, add pure water and finings and handle; Spinning, clear liquid resin absorption, washing, ethanol elution; Elutriant concentrates, and drying obtains product, and the wherein said diluted alkaline that is extracted as extracts; Said diluted alkaline extraction step is: add 1: 15-30 (W/V) mass percent concentration is that the dilute alkaline soln of 0.3%-0.5% extracts, and wherein said diluted alkaline is based on the weight of the dry blade of sea-buckthorn and calculates, and extracting temperature is 70-95 ℃, extraction time 15-25 minute.The processing condition of this extraction are avoided the hydrolysis of flavonoid glycoside.
Extremely rare alkaline solution can promote flavones to extract; And confirmed corresponding extraction conditions; Because some technology is also on the books in the prior art except that alkali is carried heavy pure the dissolving of acid, some technology is record not, and the contriver studies other each process steps; And improve and optimized each step or its processing condition, thereby further improved the output and the quality of product.
(1) in defatting step, add 1: 12-30 (W/V) butane, wherein said butane are based on the weight of the dry blade of sea-buckthorn and calculate, 45-70 ℃ reflux 0.5-1.5 hour.Emit extraction liquid, reclaim butane, get leaf oil.This defatting step carries out 3 times altogether.
(2) since borax can with contain adjacent two phenolic hydroxyl groups and combine (as just containing adjacent two phenolic hydroxyl groups in the Quercetin molecule); Play adjacent two phenolic hydroxyl groups of protection, not oxidized destructive effect, therefore after degreasing, in leaching process, add 1: 10-20 (W/V) mass percent concentration is the borax soln (being sodium tetraborate) of 0.3%-0.5%; Wherein said borax soln is based on the weight of the dry blade of sea-buckthorn and calculates; After being heated with stirring to little boiling, add dilute alkaline soln again, can further improve the quality of products.
(3) a Folium Hippophae extracts 3 times altogether, and only add 1 during the 2nd, the 3rd extraction: 15-30 (W/V) mass percent concentration is the sig water of 0.35-0.45%, and wherein said diluted alkaline is based on the weight of the dry blade of sea-buckthorn and calculates.
(4) wherein said filtrating is under 60-80 ℃, regulates in the pH step filtrating, and PH is adjusted to 4.0-5.0, and the flavonoid glycoside deposition, can be avoided flavonoid glycoside to form melt salt fully and dissolve again extremely under the mild conditions at this this moment, reduced yield.
(5) wherein carry out alcohol at said throw out and dissolve the ultrasonic extraction step for to add 1: the ethanol of 5-10 (W/V) mass percent concentration 60%-80%, wherein said ethanol are based on the weight calculating of the dry blade of sea-buckthorn, 50 ℃-80 ℃ supersound extraction 20-30 minute.This extraction step carries out 2-4 time altogether.In this step, during with dissolve with ethanol deposition (alcohol dissolves), flavonoid glycoside dissolves in the ethanol, and a large amount of impurity such as protein, and pectin class MS insoluble separating in 60% above ethanol precipitated and separated removing when centrifugal.Though also to go to dissolve extract deposition with small amount of ethanol, this moment consumption seldom, the phenomenon of a large amount of lyosorptions in the time of front end can not occurring and extract dried leaf.The small amount of ethanol of using in the technology rear end also is convenient to reclaim.
(6) wherein in said recovery ethanol step, at 50-80 ℃ of vacuum decompression recovery ethanol, when steaming to the 1/2-1/3 volume; The 1/4-1/2 that adds the about original volume of pure water; Treat that distillate alcoholic acid mass percent concentration≤10% o'clock ends, add 34 times (W/V) of pure water to Folium Hippophae consumption again, routine 1kg Folium Hippophae adds the 3-4L pure water; Add finings again and be heated to 50-70 ℃, be stirred well to natural subsidence.After being cooled to normal temperature through cold water jacket, high speed centrifugation discards throw out.
(7) in the resin absorption step, use macroporous resin.
(8) in the ethanol elution step, use 50% ethanol and 70% ethanol to carry out wash-out respectively, merge elutriant then.This compares and uses 25% ethanol and 75% pure wash-out to have better elute effect in the prior art.
(9) in drying step, use spraying drying.
Above-mentioned each concrete step can be separately or a plurality of being incorporated into together in the described process for extracting, and the technical scheme of its formation all belongs to protection content of the present invention.
The present invention uses the diluted alkaline flooding, Acid precipitation, and alcohol dissolves the macroporous resin adsorption method.The flavones content that can make product is more than 20%, and the flavonoid extracts yield is at 3-4%.Quality difference with Folium Hippophae fluctuates to some extent, owing to do not adopt extraction using alcohol, uses diluted alkaline water instead, and cost falls greatly naturally.The alcohol extracting of back is only removed the dissolution precipitation thing with ethanol seldom, and thereafter this small amount of ethanol major part is all reclaimed use, and the production safety aspect also is better than alcohol extraction process.
Following the present invention will make in more detail through specific specific embodiments and enumerating.
Specific embodiments
Get the dry blade of sea-buckthorn, add 1: 12 (W/V) butane and carry out the butane degreasing, promptly the 1kg cured leaf adds the 12L butane and then adds the 3000ml butane if get 250 gram Folium Hippophae; 60 ℃ of reflux are 1 hour in the special pressure container, emit extraction liquid, reclaim butane; Get leaf oil; Repetitive operation is totally 3 de-oilings, and reduced vacuum is taken out butane in the most leaf, and system is heated to 60 ℃;
(W/V) mass percent 0.4% borax soln that adds 1: 10 in the leaf slag after degreasing, promptly the 1kg cured leaf adds the 10L borax soln and then adds the 2500ml borax soln if get 250 gram Folium Hippophae, fully stirs; After being heated to little boiling, under agitation condition, add 1: 10 (W/V) 0.8% dilute alkaline soln; Be that the 1kg cured leaf adds the 10L dilute alkaline soln, do not stop to be heated with stirring to 80-90 ℃, kept 15 minutes; Extract extraction liquid out; Add 1: 15 (W/V) mass percent 0.4% sig water, promptly the 1kg cured leaf adds the above operation of 15L dilute alkaline soln repetition, extracts altogether 3 times;
Extract extraction liquid out and merge 3 filtratings under 60-70 ℃, transfer PH-4.2-4.3, the static high speed centrifugation that spends the night separates abandoning supernatant.
Throw out adds 1: 5 (W/V) mass percent 80% ethanol, is 1kg cured leaf added-time 5L ethanol; Stir extraction, 20 minutes, spinning at 50-60 ℃ with the ultrasonic extraction device; Repeat above operation and extract altogether 3 times, discard throw out;
50-60 ℃ of vacuum decompression of clear liquid (alcoholic solution) reclaims ethanol, when steaming to the 1/2-1/3 volume, adds 1/4 of the about original volume of pure water, treats that distillate ethanol≤10% o'clock only; Add 3-4 times (W/V) of pure water to Folium Hippophae consumption, add finings again and be heated to 60-70 ℃, stir after 30 minutes; Cooling fast; (tubular-bowl centrifuge 15000r/min), discards throw out in spinning.
Supernatant is used the AB-8 macroporous resin adsorption;
Use a large amount of pure water drip washing resin columns then, until flowing out water liquid water white transparency;
Then, merge elutriant, and reclaim ethanol at 50 ℃ of vacuum decompressions with 50% ethanol and 70% ethanol elution;
The liquid concentrator spraying drying;
Obtain finished product.
Get 250 gram prepared from defatted seabuckthorn leaves and accomplish a whole set of operation, obtain leaf of Fructus Hippophae flavone extract 10.0876 grams at last, this extract records its flavones content=21.6% with the flavones measuring method that Nanjing Ze Lang medical sci-tech company is provided.
According to above result, can calculate the extract (X) of 100 gram Folium Hippophae
250 grams: 10.0876 grams=100 grams: X X=4.0350 restrains (containing flavones 21.6%)
Explain that 100 gram Folium Hippophae can extract the extract that 4.035 grams contain flavones 21.6%, promptly yield is 4.03%.As previously mentioned, the yield of leaf of Fructus Hippophae flavone extract of the present invention is 3-4%; The leaf flavones purity of product is more than 20%, wherein contains true yellow ketone material=4.0350 * 21.6%=0.8715 gram, and promptly 100 gram Folium Hippophae extract 0.8715 gram flavones=871.5 milligram, and available 871.5 milligrams/100 gram leaves are represented.Flavonoid content 832mg/100 gram is a basically identical in the Folium Hippophae of putting down in writing in itself and the existing document, and it is that 800-900mg is consistent on a large scale.Above result can explain that at least the present invention can extract the flavonoid substance overwhelming majority in the Folium Hippophae.
Claims (8)
1. a Fructus Hippophae total flavones extracts the method for purifying, and it comprises the step of next coming in order: supply raw materials, degreasing is extracted; Filter, filtrating is regulated pH, spinning, and throw out carries out alcohol and dissolves ultrasonic extraction; Ethanol is reclaimed in spinning, adds pure water and finings and handles spinning; The clear liquid resin absorption, washing, ethanol elution, elutriant concentrates; Drying obtains product, it is characterized in that, the wherein said diluted alkaline that is extracted as extracts; Said diluted alkaline extraction step is for adding 1: 15-30 (W/V) mass percent concentration is that the dilute alkaline soln of 0.3%-0.5% extracts, and wherein said diluted alkaline is based on the weight of the dry blade of sea-buckthorn and calculates, and extracting temperature is 70-95 ℃, extraction time 15-25 minute.
2. the method for claim 1; Wherein after degreasing, add 1: 10-20 (W/V) mass percent concentration is the borax soln of 0.3%-0.5%; Wherein said borax soln is based on the weight of the dry blade of sea-buckthorn and calculates, be heated with stirring to little boiling after, add dilute alkaline soln again.
3. claim 1 or 2 method, a Folium Hippophae extracts 3 times altogether, and only add 1 when extracting for the 2nd, the 3rd time: 15-30 (W/V) mass percent concentration is the sig water of 0.35-0.45%, and wherein said diluted alkaline is based on the weight of the dry blade of sea-buckthorn and calculates.
4. the method for aforementioned arbitrary claim, wherein said defatting step is for adding 1: 12-30 (W/V) butane, wherein said butane are based on the weight of the dry blade of sea-buckthorn and calculate, 45-70 ℃ reflux 0.5-1.5 hour.
5. the method for aforementioned arbitrary claim, wherein said filtrating are transferred PH=4.0-5.0 under 60-80 ℃.
6. the method for aforementioned arbitrary claim; Wherein said throw out carries out alcohol and dissolves the ultrasonic extraction step for to add 1: the ethanol of 5-10 (W/V) mass percent concentration 60%-80%; Wherein said ethanol is based on the weight of the dry blade of sea-buckthorn and calculates, 50 ℃-80 ℃ supersound extraction 20-30 minute.
7. the method for aforementioned arbitrary claim, wherein said throw out are carried out alcohol and are dissolved the ultrasonic extraction step and carry out 2-4 time altogether.
8. the method for aforementioned arbitrary claim in the wherein said recovery ethanol step, reclaims ethanol at 50-80 ℃ of vacuum decompression; When steaming to the 1/2-1/3 volume, add the 1/4-1/2 of the about original volume of pure water, treat that distillate alcoholic acid mass percent concentration≤10% o'clock is only; Add 3-4 times (W/V) of pure water to Folium Hippophae consumption again, add finings again and be heated to 50-70 ℃, be stirred well to natural subsidence; After being cooled to normal temperature through cold water jacket, high speed centrifugation discards throw out.
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| CN103054915A (en) * | 2012-12-13 | 2013-04-24 | 大兴安岭林格贝有机食品有限责任公司 | Novel production process for total flavones of hippophae rhamnoides |
| CN103417588A (en) * | 2013-08-23 | 2013-12-04 | 中国科学院新疆理化技术研究所 | Preparation method of effective part of Hippophae rhamnoides |
| CN104127356B (en) * | 2014-08-07 | 2016-08-17 | 中国科学院新疆理化技术研究所 | A kind of Fructus Hippophae oropharynx anti-inflammation combination liquid and preparation method thereof |
| CN107854498A (en) * | 2017-11-22 | 2018-03-30 | 江南大学 | A kind of accurate extractive technique of leaf of Fructus Hippophae flavone using RP HPLC DAD monitorings |
Citations (3)
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| CN1308084A (en) * | 2001-02-13 | 2001-08-15 | 天津市阳成高科技天然制品有限公司 | Resin adsorption process of preparing sea-buckthorn flavone with sea-buckthorn leaf |
| CN1504467A (en) * | 2002-12-05 | 2004-06-16 | 河北神兴沙棘研究院 | Extraction technology for seabuckthorn leaf general flavone |
| CN101225080A (en) * | 2008-01-25 | 2008-07-23 | 东北农业大学 | Method for extracting flavone from sea-buckthorn leaves and feed stuff containing the same |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1308084A (en) * | 2001-02-13 | 2001-08-15 | 天津市阳成高科技天然制品有限公司 | Resin adsorption process of preparing sea-buckthorn flavone with sea-buckthorn leaf |
| CN1504467A (en) * | 2002-12-05 | 2004-06-16 | 河北神兴沙棘研究院 | Extraction technology for seabuckthorn leaf general flavone |
| CN101225080A (en) * | 2008-01-25 | 2008-07-23 | 东北农业大学 | Method for extracting flavone from sea-buckthorn leaves and feed stuff containing the same |
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