CN102191131A - Systemic preparation method of chrysanthemum rice essential oil, chrysanthemum rice polysaccharide, chrysanthemum total flavone extract and chrysanthemum rice powder - Google Patents
Systemic preparation method of chrysanthemum rice essential oil, chrysanthemum rice polysaccharide, chrysanthemum total flavone extract and chrysanthemum rice powder Download PDFInfo
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- CN102191131A CN102191131A CN2011100627616A CN201110062761A CN102191131A CN 102191131 A CN102191131 A CN 102191131A CN 2011100627616 A CN2011100627616 A CN 2011100627616A CN 201110062761 A CN201110062761 A CN 201110062761A CN 102191131 A CN102191131 A CN 102191131A
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Abstract
The invention discloses a coproduction method for extracting chrysanthemum rice essential oil from chrysanthemum rice by one-step batch feeding, obtaining chrysanthemum rice polysaccharide from residues after extracting the essence oil, obtaining chrysanthemum total flavones from the residues after obtaining the chrysanthemum rice polysaccharide, and processing the rest residues into chrysanthemum rice powder. By the method, the chrysanthemum rice essential oil can be produced from the same batch of raw materials; oil extraction ratio is up to 5 to 9 percent; the integrated fragrance outline of the chrysanthemum rice essential oil is maintained; the yield of the polysaccharide is over 10 percent; the total flavone content is 20 to 60 percent; the carotene content of the chrysanthemum rice powder is 4 mg/100g; the amino acid content of the chrysanthemum rice powder is about 15 g/100g; the chrysanthemum rice resource is utilized completely; the extracted biological active products can provide raw materials for medicaments, cosmetics and health-care food; and low-cost and high-additional-value production of the chrysanthemum rice is realized.
Description
Technical field
The invention belongs to extraction, separation and the preparation field of natural product, particularly relating to a kind of is the method for raw material combined preparation chrysanthemum rice essential oil, chrysanthemum rice polysaccharide and chrysanthemum cream colour ketone extract and chrysanthemum ground rice with chrysanthemum popped rice flower bud.
Technical background
" augmentation Compendium of Materia Medica " records: " chrysanthemum rice goes out a kind of mother chrysanthemum in the mountain, Chuzhou. and the scholar adopts its stamen (flower bud) and does it, and is big as half mung bean, very fragrant and light circle is yellow bright, cloud: relieving internal heat, loose, to treat, dispel the wind, relieve inflammation or internal heat, make eye bright be the first, produces Suichang stone white silk." Qing Dynasty's medicine scholar Zhao Xuemin points out that in supplementary Amplifications of the Compendium of Materia Medica chrysanthemum rice is (Chrysanthemum indicum) bud of plant mother chrysanthemum, relieve internal heat, loose and treats, dispel the wind, relieve inflammation or internal heat effect such as make eye bright, and point out and produce stone and practice mountain region chrysanthemum rice and be the best.
Chrysanthemum rice bright yellow color, bitter suffering, gas cold, its fragrant outclass Wild Chrysanthemum.Ancient Chinese medicine doctor is also consistent to be thought, mother chrysanthemum nature and flavor bitter cold, the effect of eliminating inflammation and expelling toxin, clearing heat and cooling blood, sterilization are arranged, dispeling the wind.Contain protein, amino acid, various trace elements in the chrysanthemum rice, and chrysanthemum rice lactones, artoglasin, flavones, the disease-resistant key element of volatilization wet goods, can strengthen that human body is disease-resistant, the ability of diseases prevention, have clearing heat and detoxicating, tomorrow of relieving inflammation or internal heat, flat liver step-down, kidney-nourishing kidney tonifying, lipopenicillinase, clear heat, sober up, effect such as preventing cold, long-term drinking can promote the production of body fluid beauty treatment, promote longevity, especially the blurring of image and hyperpietic are had splendid disease-resistant health-care effect, these effects are relevant with compositions such as the contained essential oil of chrysanthemum rice, polysaccharide, flavones invariably.
Chrysanthemum rice essential oil is one of main effective constituent of chrysanthemum rice, and the method for producing chrysanthemum rice essential oil mainly contains steam distillation, solvent-extraction process, supercritical CO
2Extraction process etc.Steam distillation or solvent extration complex procedures, loss is big, oil yield is low and usually can change whole fragrance profile, and usually the loss head is fragrant, and product loses feeling of freshness, and used raw material is difficult to realize complete utilization.The present invention adopts latter's method can obtain the integrity profile of bigger extraction yield of chrysanthemum rice volatile oil and more active chemical maintenance chrysanthemum rice essential oil; Simultaneously, the utilization by the waste residue after chrysanthemum rice essential oil is extracted improves value-added content of product, meets resource-effective industry policy.
Open (the CN200510032608.3 of all existing both at home and abroad method about Jumi extract; 200610049807.X; 200610028335.X; : 2008100609226; 101396387A), but above report mainly concentrates on the simple processing of fragmentary technology in aspect such as the flavones, essential oil extractive technique of chrysanthemum rice and single product, lacks relevant system, forms the processing technology of the comprehensive utilization with scale, cause the wasting of resources, productivity effect is not high.
Chrysanthemum rice polysaccharide contains quite high (15%-30%) content in chrysanthemum rice, and find that in recent research it has effects such as excellent antibiotic anti-inflammatory, blood fat reducing, and in research report in the past, do not see it is made full use of by technology of the present invention is integrated.
Chrysanthemum rice total flavones has shown that it has good curative effect at aspects such as treatment heart trouble, hypertension, and report in the past is that raw material extracts by chrysanthemum rice all, and the present invention will extract from the chrysanthemum rice slag after having extracted essential oil and polysaccharide, has saved cost.
Chrysanthemum ground rice is to extract total flavones chrysanthemum rice residue afterwards, and the beneficiating ingredient that it is rich in as compositions such as amino acid, VITAMIN, lactones, can be developed to foodstuff additive, fodder additives, protective foods etc., also can be prepared into the various convenient formulations of using.
Above technology integrated once feeds intake and can obtain chrysanthemum rice polysaccharide from the residue after chrysanthemum rice essential oil extracts; Can from take out chrysanthemum rice polysaccharide residue obtain chrysanthemum rice total flavones, last residue, also be utilized at last, made full use of chrysanthemum rice resource, the bioactive product that is extracted, can be medicine, makeup and protective foods and supply raw materials, the invention provides the effective cogeneration mode that can reduce production costs, reduce the wasting of resources.
Summary of the invention
The object of the present invention is to provide a kind of chrysanthemum rice essential oil that from chrysanthemum rice raw material, extracts, can extract the method for chrysanthemum rice polysaccharide, chrysanthemum extractive of general flavone and chrysanthemum ground rice multiple product simultaneously again, realized chrysanthemum rice complete utilization, reach energy-saving and emission-reduction, the purpose that reduces production costs.
Four kinds of products of combined preparation of the present invention may further comprise the steps:
The processing of A medicinal material
Get chrysanthemum rice and pulverize with pulverizer, the back of sieving is standby.
B essential oil extraction process
Weigh → feed sealing → increasing temperature and pressure to specific extraction conditions → extraction → step-down separation → chrysanthemum rice essential oil
The C supercritical CO
2Extraction conditions
Extracting pressure 15-35MPa, temperature are 35-65 ℃; Separation reactor I pressure is 4-8Mpa, and separation reactor I I pressure is made as 4-9MPa; CO
2Flow is 20L/h; 1-4 hour extraction time.
From separation reactor I I, take out chrysanthemum rice essential oil after the D extraction is finished, get chrysanthemum rice essential oil product.
Add entry (pressing material ratio 1: 5-30 adds) in the chrysanthemum rice residue of E in the D step, 80 ℃ were heated 2 hours, and left standstill, supernatant liquid filtering, can adopt finingss such as whizzer, membrane filtration or employing gelatin to filter, and the squeezing filter residue, merging filtrate obtains the Crude polysaccharides solution I;
The filter residue of F to squeezing, the preparation process of continuation E gets filtrate II, and filter residue is standby;
G merging filtrate I and II, concentrating under reduced pressure;
H adds 5 times to 95% ethanolic soln of G step concentrated solution, makes the alcohol amount reach 80%, and standing over night is filtered filtrate for later use; 60 ℃ of oven dry of filter residue promptly get chrysanthemum rice Crude polysaccharides.
I chrysanthemum cream colour ketone extract: the filtrate of getting step H is mixed (consumption that this step has reduced consumption of ethanol and produced kinetic energy) with the filter residue of step F, adjusting alcohol measures to 40-60%, 40-80 ℃ was extracted 2 hours, filter, filter residue adds ethanol again makes into 40-60%, abovementioned steps, filter, filtrate merges, and filter residue is standby, and pressurization concentrates reclaims ethanol extremely to the greatest extent, vacuum-drying, obtain chrysanthemum rice extractive of general flavone, this extract has following feature: chrysanthemum cream colour ketone content can reach 20-60%, and has tangible fungistatic effect.
The preparation of J chrysanthemum ground rice: with the standby filter residue that step I obtains, vacuum-drying is pulverized promptly.This powder has kept original amino acid (10-25g/100g) in the chrysanthemum rice, carotene (4mg-10mg/100g), vitamins nutritive ingredient.
The present invention is with respect to the advantage of prior art:
1, the characteristics of maximum of the present invention are: can produce chrysanthemum rice essential oil, chrysanthemum rice polysaccharide, chrysanthemum rice extractive of general flavone and chrysanthemum ground rice with a collection of raw material, utilize chrysanthemum rice only to produce chrysanthemum cream colour ketone (CN101095711A, CN101248870A), supercritical CO with the past
2Active substance (CN101095712A) in the extraction chrysanthemum rice extractive with organic solvent is compared, and has accomplished making full use of of resource, has increased value-added content of product, makes production process reach energy-saving and emission-reduction.
2, oil yield Gao Keda 5%-9% of the present invention has kept the complete fragrance profile of essential oil simultaneously, reclaim in the residue in polysaccharide, total flavones and chrysanthemum ground rice, reduced production cost, increased productive value.
3, high efficiency, low cost has obtained chrysanthemum ground rice, makes the chrysanthemum ground rice of making remove the peculiar smell of chrysanthemum rice essential oil, has kept nutritive ingredients such as original amino acid, carotene in the chrysanthemum rice, can be used for purposes such as feed, food interpolation, has accomplished whole utilizations of raw material.
Description of drawings
The combined preparation process signal of Fig. 1 chrysanthemum rice essential oil, chrysanthemum rice polysaccharide, chrysanthemum cream colour ketone and chrysanthemum ground rice
Specific embodiments
Embodiment 1
1.1 get chrysanthemum rice 1000g, being ground into granularity is 50 order powder, puts supercritical CO
2In the extraction kettle of abstraction instrument, feed CO
2, flow is 20L/h, rising pressure, and making extracting pressure is 20MPa, and extraction temperature is 50 ℃, and other conditions are defined as: separation reactor I pressure is made as 6.0MPa, temperature is made as 40 ℃; Separation reactor I I pressure is made as 6.0MPa, and temperature is made as 40 ℃; Dynamic extraction 1 hour after having extracted, takes out chrysanthemum rice essential oil, yield about 9% from separation reactor I I.Chrysanthemum rice slag in the extraction kettle is standby
1.2 will add 10 times of amounts of water in 1.1 the standby filter residue, 80 ℃ were heated 2 hours, leave standstill, adopt whizzer centrifugal (3000-4000rpm), filtrate I, filter residue add 8 times of water gagings and repeat above step, filtrate II, merging filtrate obtains Crude polysaccharides solution, activated carbon decolorizing, concentrating under reduced pressure gets concentrated solution and filter residue (standby); Add 5 times to 95% ethanolic soln of concentrated solution, make the alcohol amount reach 80%, standing over night is filtered, and filtrate II I is standby; 60 ℃ of oven dry of filter residue are pulverized, and promptly get the about 100g of chrysanthemum rice polysaccharide.
Place multi-function extractor 1.3 get the standby filter residue and the standby filtrate II I of step 1.2, add the about 800mL of water, make to contain alcohol amount and reach about 40%, temperature was soaked (60 ℃) 2 hours, filter, get filter residue and filtrate, filter residue is standby, behind the filtrate recycling ethanol, be concentrated into proportion 1.2, vacuum-drying is pulverized, and obtains the total flavonoid extract.After measured, the general flavone content of this extract reaches 20%.The preparation and the further separation and purification total flavones that can be used for medicine.
1.4 the preparation of chrysanthemum ground rice: the filter residue I that gets step 1.3 puts in the baking oven, and oven drying at low temperature makes into moisture less than 8% dry powder, packing, the principal character of this chrysanthemum ground rice for contain carotene 4mg/100g, amino acid is about 15g/100g etc.
Claims (7)
1. the method for combined preparation chrysanthemum rice essential oil, chrysanthemum rice polysaccharide, chrysanthemum rice extractive of general flavone and chrysanthemum ground rice from chrysanthemum rice.
2. as the chrysanthemum rice essential oil of claim 1 preparation, be to adopt supercritical CO
2Abstraction technique is a feedstock production with chrysanthemum popped rice flower bud, and I is standby gained chrysanthemum rice residue;
3. the supercritical CO as adopting in the claim 2
2Abstraction technique, main technical details are that extracting pressure 15-35MPa, temperature are 35-65 ℃; Separation reactor I pressure is 4-8Mpa, and separation reactor I I pressure is made as 4-9MPa; CO
2Flow is 20L/h; 1-4 hour extraction time.
4. as the preparation of chrysanthemum rice polysaccharide in the claim 1, be to be feedstock production to have obtained chrysanthemum rice residue behind the chrysanthemum rice essential oil in the claim 2, adopt water extraction and alcohol precipitation method to obtain chrysanthemum rice Crude polysaccharides, wherein filtrate and residue are standby.
5. as the preparation of the extractive of general flavone in the claim 1, be to be feedstock production to extract filtrate behind the Crude polysaccharides and filter residue in the claim 4;
6. as in the chrysanthemum cream colour ketone preparation method of extract in the claim 5, get filtrate with filter residue mix (consumption that this step has reduced consumption of ethanol and produced kinetic energy), adjusting alcohol measures to 40-60%, realize by thin up, the extraction temperature that adopts is 40-80 ℃, vacuum-drying obtains chrysanthemum rice extractive of general flavone, and this extract has following feature: chrysanthemum cream colour ketone content can reach 20-60%.
7. as the preparation of the chrysanthemum ground rice of claim 1 preparation, be having produced the filter residue behind the flavones general extractive in the claim 6, obtain by vacuum-drying, its principal character contains compositions such as amino acid, carotene simultaneously in this chrysanthemum ground rice.
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| CN2011100627616A CN102191131A (en) | 2011-03-08 | 2011-03-08 | Systemic preparation method of chrysanthemum rice essential oil, chrysanthemum rice polysaccharide, chrysanthemum total flavone extract and chrysanthemum rice powder |
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Cited By (3)
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| CN103710152A (en) * | 2013-10-28 | 2014-04-09 | 黄山神草生物科技有限公司 | Method for using supercritical carbon dioxide for extraction of chrysanthemum essential oil |
| CN104673497A (en) * | 2015-03-13 | 2015-06-03 | 中南林业科技大学 | Extraction technology of plant essential oil, polysaccharide and flavone |
| CN105969527A (en) * | 2016-05-23 | 2016-09-28 | 铜陵薇吉特生物科技有限公司 | Comprehensive utilization method of ginger leaves |
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Cited By (5)
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| CN104673497A (en) * | 2015-03-13 | 2015-06-03 | 中南林业科技大学 | Extraction technology of plant essential oil, polysaccharide and flavone |
| CN104673497B (en) * | 2015-03-13 | 2017-11-10 | 中南林业科技大学 | A kind of extraction process of plants essential oil, polysaccharide and flavones |
| CN105969527A (en) * | 2016-05-23 | 2016-09-28 | 铜陵薇吉特生物科技有限公司 | Comprehensive utilization method of ginger leaves |
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Application publication date: 20110921 |