CN104921997A - Ultrahigh-pressure pressure extraction method of peony flower and whitening antioxidant essence prepared thereby - Google Patents
Ultrahigh-pressure pressure extraction method of peony flower and whitening antioxidant essence prepared thereby Download PDFInfo
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- CN104921997A CN104921997A CN201510351477.9A CN201510351477A CN104921997A CN 104921997 A CN104921997 A CN 104921997A CN 201510351477 A CN201510351477 A CN 201510351477A CN 104921997 A CN104921997 A CN 104921997A
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Abstract
The invention relates to an ultrahigh-pressure pressure extraction method of peony flower and whitening antioxidant essence prepared thereby. By weight, 55% to 98.5% of water, 0.5% to 10% of glycerine, 0.5% to 20% of 1, 2-propandiol, and 0.5% to 15% of 1, 3-butanedio are subjected to ultrahigh-pressure extraction; the process is simple, the operating time is short, active ingredients in gallic acid, cosmosiin and the like can be effectively extracted, the extract is high in anti-oxidation and whitening activity and can be prepared into cosmetics, such as essences, body lotions, milks and creams.
Description
Technical field
The present invention relates to a kind of use Flos Moutan hyperpressure extraction thing essence of cosmetic technical field, the whitening of specifically a kind of Flos Moutan ultrahigh-pressure extraction method and preparation thereof, antioxidation essence.
Background technology
Paeonia suffruticosa is a kind of special product rare flower of China, and due to its large flower and brilliant color, be again important Chinese crude drug, the successive dynasties are subject to liking of people and pay attention to.Current China Paeonia suffruticosa cultivated area is comparatively large, and only Heze Prefecture's cultivated area has reached more than 100,000 mus.Viewing and admiring except function except having, Flos Moutan or the traditional medicine of heat-clearing and toxic substances removing, having and blood, hemopoietic, removing heat from blood effect.In addition, the proanthocyanidin contained in Flos Moutan is one of material that antioxidant activity is stronger.Therefore, adopt modern extractive technique, rose extract is made the cosmetics with whitening, antioxidant effect, will greatly increase Flos Moutan economic worth, and be conducive to the in-depth development of Paeonia suffruticosa specialty industries.
Through finding the literature search of prior art, Feng Zhiwen is at " Journal of Northwest Sci Tech University of Agriculture and Forestry " (Vol.37, No.1,2009,205 ~ 210) " the antioxidant activity analyses of 6 kind peony petals " have been delivered, research finds that peony petal extracting solution obviously can suppress hydroxylation, and dark petal extracting solution is stronger to radical scavenging activity.Chen Jialing is at " daily chemical industry " (Vol.44No.12,2014,692 ~ 695) delivered " research of Flos Moutan Aqueous extracts scavenging hydroxyl and restraint of tyrosinase activity ", research finds that Flos Moutan Aqueous extracts has good hydroxy radical and tyrosinase inhibitory action.
Chinese invention patent application 99112074.4 discloses the extraction process of natural Paeonia suffruticosa liquid and natural Paeonia suffruticosa liquid, the root of Paeonia suffruticosa is got in this invention, branch, branch put into high-temperature retorting reactor, heat after condensation and distill, obtain product in the middle of Paeonia suffruticosa liquid, again leaf, flower, root are put into middle product and decocted, stir, distill, obtain Paeonia suffruticosa liquid.
Chinese invention patent application 201210359240.1 discloses a kind of eye mask applying peony root extractive and pastes essence and preparation method thereof.This essence by moisturizing component, thickening component, antiallergic component, in and component, anticorrosion component and effect active component composition, wherein effect active component is hyaluronate sodium, Herba bromi japonici glucose, hamamelis extract, peony root extractive.But do not relate to Flos Moutan in this invention raw material.
Chinese invention patent application 200980145098.7 discloses a kind of containing the antioxidation cosmetic product compositions through the Paeonia suffruticosa of processing, the extract of Rhizoma Polygonati or Bulbus Lilii.This invention using the extract containing at least one used in the Paeonia suffruticosa of medicinal herbs process technologies processing, Rhizoma Polygonati and Bulbus Lilii or with the mixture of at least one extract in crude Paeonia suffruticosa, Rhizoma Polygonati and the Bulbus Lilii antioxidation cosmetic product compositions as active component.
But these inventions just using Flos Moutan or root of Paeonia suffruticosa Ardr. as a kind of raw material, the index composition in extracting solution is indefinite, does not relate to extracting method and the whitening effect of Flos Moutan hyperpressure extraction liquid.
Summary of the invention
The object of the invention is to overcome deficiency of the prior art, provide a kind of and adopt hyperpressure extraction technology, can effectively extract the index components such as gallic acid, cosmosiin, thus improve the Flos Moutan essence preparation method of whitening, antioxidant activity.
The present invention is achieved by the following technical solutions:
A kind of Flos Moutan ultrahigh-pressure extraction method,
Get fresh Paeonia suffruticosa or the dry Flos Moutan of water content below 12% is for subsequent use;
Flos Moutan is extracted under ultra-high pressure condition with Extraction solvent;
Extraction fluid, obtains essence;
Described Extraction solvent comprises water, glycerol, 1,2-PD, 1,3 butylene glycol.
Preferably, described Extraction solvent is mixed by the solution of following percentage by volume: 55-98.5% water, 0.5-10% glycerol, 0.5-20%1,2-propylene glycol, 0.5-15%1,3-butanediol.
Preferably, described ultra-high pressure condition is: when extracting, controlled pressure scope is 100MPa ~ 500MPa, and the hyperpressure extraction time is 1-2min.
Preferably, described Extraction solvent consumption is 10-40 times of Flos Moutan consumption.
Preferably, the method for described extraction fluid adopts and filters and/or centrifugal treating.
Preferably, the rotating speed of described centrifugal treating is more than 8000r/min.
Said method prepare whitening, antioxidation essence, it is characterized in that, in described essence, the content of gallic acid is 7.21-8.55mg/g, cosmosiin content is 12.3-20.5mg/g.
Present invention also offers a kind of quality inspection standard of Flos Moutan extracting solution, get extracting solution HPLC after 0.45 μm of micro-filtrate membrane filtration and measure gallic acid and cosmosiin content.This quality inspection standard has detection fast, evaluates accurately, is easy to the advantages such as standardized and popularized.
The present invention by the following method and evaluation of estimate index test, obtain the optimum extracting method of Flos Moutan essence.
Take a certain amount of Flos Moutan sample, proceed in polyethylene plastic bag, by different solvents according to certain solid-liquid ratio (1:5,1:10,1:20,1:30,1:40,1:50g/mL) add solvent after seal, certain pressure (50 is set, 100,200,300,400,500MPa), the time (1,2,3,4,5min) carry out hyperpressure extraction, after release, filter, centrifugal 5min, obtain supernatant, extracting solution HPLC after 0.45 μm of micro-filtrate membrane filtration measures gallic acid and cosmosiin content.After extracting solution vacuum lyophilization, solid content deionized water is mixed with the aqueous solution that concentration is 0.5mg/mL, measures its DPPH free radical, superoxide anion and tyrosinase inhibition rate.All experiments all in triplicate, results averaged.
Table 1 different solvents Flos Moutan extracts experimental studies results
As shown in table 1, Extraction solvent has material impact to active component in Flos Moutan extract and antioxidation, whitening effect.Because the polarity of water is very large, in Paeonia suffruticosa, in flavone etc., the compound solubility of low polarity is poor, and therefore, take water as solvent, reference compound extraction ratio is low, poor activity.With 50% ethanol for Extraction solvent, although the extraction ratio of reference compound is higher, extract TYR enzyme inhibition rate is poor, and this solvent is poor to the low polar compound extraction ratio that TYR enzyme inhibition activity is higher, therefore, can not reach sample requirement.With water, glycerol, 1,2-propylene glycol, 1, when the mixture of 3-butanediol is as Extraction solvent, its polarity scope is very wide, is applicable to the extraction of all kinds of organic compound, to high in Flos Moutan, in even low polar compound dissolubility very high, pass through the preferred of proportioning simultaneously, ensure that target compound extraction ratio is generally the sample of solvent higher than pure water or 50% ethanol, there is higher free radical and TYR enzyme inhibition activity simultaneously, meet sample requirement.
In above-mentioned experimental basis, fixed extraction solvent, changes and extracts pressure and extraction time, found that, extracts pressure and obviously reduces lower than 50MPa with higher than extraction ratio during 500MPa, therefore, extracts pressure limit and chooses 50-500MPa.Hyperpressure extraction technology can complete the extraction of target compound within the extremely short time, and meanwhile, extraction time is little on the impact of active substance extraction ratio, and consider conventional efficient, the problem such as energy-conservation, the selective extraction time is 1-2min.
Solid-liquid ratio experiment finds, when solid-liquid ratio is lower than 1:10, extraction ratio is lower, and extracting solution activity can not reach sample requirement.And when solid-liquid ratio reaches 1:40, target compound fully extracts.Consider, Extraction solvent consumption is 10-40 times of Flos Moutan consumption.
Sample storage stability experiment finds, rotating speed, lower than the sample of 8000r/min centrifugal treating, stores and occurs a small amount of flocculent deposit after 30 days, and therefore, the rotating speed of centrifugal treating is more than 8000r/min.
Compared with prior art, the present invention has following useful effect: present invention process is simple, operating time is short, effectively can extract the gallic acid in Flos Moutan, cosmosiin isoreactivity material, this extracting solution has very high antioxidation and whitening active, can be mixed with the cosmetics such as essence, cream for skin care, emulsion, cream, but range of application of the present invention is not limited to this.
Accompanying drawing explanation
Fig. 1 Flos Moutan essence high-efficient liquid phase chromatogram
Detailed description of the invention
Following instance will the invention will be further described by reference to the accompanying drawings.The present embodiment is implemented under premised on technical solution of the present invention, gives detailed embodiment and process, but protection scope of the present invention is not limited to following embodiment.The experimental technique of unreceipted actual conditions in the following example, usually conveniently condition, or according to the condition that manufacturer advises.
Below in conjunction with specific embodiment, the invention will be further described, but the present invention is not limited to following examples.
Embodiment 1
Take 10g Flos Moutan sample in the present embodiment, proceed in polyethylene plastic bag, seal after adding 100mL solvent, certain pressure 100MPa is set, time 1min carries out hyperpressure extraction, after release, filter, the centrifugal 5min of 8000r/min, supernatant is this essence.Wherein, solvent is the percentage by volume of water is 98.5%, the percentage by volume of glycerol is 0.5%, 1, the percentage by volume of 2-propylene glycol is 0.5%, and the percentage by volume of 1,3 butylene glycol is 0.5%, gallic acid, cosmosiin content are 7.21,12.3mg/g, DPPH free radical, superoxide anion and tyrosinase inhibition rate are 51.3%, 47.6% and 68.1%.
Embodiment 2
Take 10g Flos Moutan sample in the present embodiment, proceed in polyethylene plastic bag, seal after adding 200mL solvent, certain pressure 200MPa is set, time 1min carries out hyperpressure extraction, after release, filter, the centrifugal 5min of 10000r/min, supernatant is this essence.Wherein, solvent is the percentage by volume of water is 55%, the percentage by volume of glycerol is 10%, 1, the percentage by volume of 2-propylene glycol is 20%, and the percentage by volume of 1,3 butylene glycol is 15%, gallic acid, cosmosiin content are 8.55,20.5mg/g, DPPH free radical, superoxide anion and tyrosinase inhibition rate are 85.3%, 82.7% and 94.6%.
Embodiment 3
Take 10g Flos Moutan sample in the present embodiment, proceed in polyethylene plastic bag, seal after adding 300mL solvent, certain pressure 300MPa is set, time 1min carries out hyperpressure extraction, after release, filter, the centrifugal 5min of 8000r/min, supernatant is this essence.Wherein, solvent is the percentage by volume of water is 60%, the percentage by volume of glycerol is 10%, 1, the percentage by volume of 2-propylene glycol is 15%, and the percentage by volume of 1,3 butylene glycol is 15%, gallic acid, cosmosiin content are 8.25,19.8mg/g, DPPH free radical, superoxide anion and tyrosinase inhibition rate are 81.4%, 79.6% and 90.5%.
Embodiment 4
Take 10g Flos Moutan sample in the present embodiment, proceed in polyethylene plastic bag, seal after adding 400mL solvent, certain pressure 400MPa is set, time 1min carries out hyperpressure extraction, after release, filter, the centrifugal 5min of 8000r/min, supernatant is this essence.Wherein, solvent is the percentage by volume of water is 70%, the percentage by volume of glycerol is 5%, 1, the percentage by volume of 2-propylene glycol is 10%, and the percentage by volume of 1,3 butylene glycol is 15%, gallic acid, cosmosiin content are 7.94,18.2mg/g, DPPH free radical, superoxide anion and tyrosinase inhibition rate are 80.5%, 77.8% and 91.0%.
Embodiment 5
Take 10g Flos Moutan sample in the present embodiment, proceed in polyethylene plastic bag, seal after adding 500mL solvent, certain pressure 500MPa is set, time 1min carries out hyperpressure extraction, after release, filter, the centrifugal 5min of 10000r/min, supernatant is this essence.Wherein, solvent is the percentage by volume of water is 80%, the percentage by volume of glycerol is 5%, 1, the percentage by volume of 2-propylene glycol is 5%, and the percentage by volume of 1,3 butylene glycol is 10%, gallic acid, cosmosiin content are 7.56,16.4mg/g, DPPH free radical, superoxide anion and tyrosinase inhibition rate are 75.6%, 70.5% and 82.3%.
Although above-mentioned, the specific embodiment of the present invention is described; but not limiting the scope of the invention; one of ordinary skill in the art should be understood that; on the basis of technical scheme of the present invention, those skilled in the art do not need to pay various amendment or distortion that creative work can make still within protection scope of the present invention.
Claims (9)
1. a Flos Moutan ultrahigh-pressure extraction method, is characterized in that,
Get fresh Paeonia suffruticosa or the dry Flos Moutan of water content below 12% is for subsequent use;
Flos Moutan is extracted under ultra-high pressure condition with Extraction solvent;
Extraction fluid, obtains essence; Described Extraction solvent comprises water, glycerol, 1,2-PD, 1,3 butylene glycol.
2. method according to claim 1, is characterized in that, described Extraction solvent is mixed by the solution of following percentage by volume: 55-98.5% water, 0.5-10% glycerol, 0.5-20%1,2-propylene glycol, 0.5-15%1,3-butanediol.
3. method according to claim 1, is characterized in that, described ultra-high pressure condition is: when extracting, controlled pressure scope is 50MPa ~ 500MPa, and the hyperpressure extraction time is 1-2min.
4. method according to claim 1, is characterized in that, described Extraction solvent consumption is 10-40 times of Flos Moutan consumption.
5. method according to claim 1, is characterized in that, the method for described extraction fluid adopts filters and/or centrifugal treating.
6. method according to claim 1, is characterized in that, the rotating speed of described centrifugal treating is more than 8000r/min.
7. method described in claim 1-6 prepare whitening, antioxidation essence, it is characterized in that, in described essence, the content of gallic acid is 7.21-8.55mg/g, cosmosiin content is 12.3-20.5mg/g.
8. essence according to claim 7 is applied preparing in cosmetics.
9. a quality inspection standard for Flos Moutan extracting solution, is characterized in that,
Get extracting solution HPLC after 0.45 μm of micro-filtrate membrane filtration and measure gallic acid and cosmosiin content.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106242974A (en) * | 2016-08-02 | 2016-12-21 | 重庆工商大学 | A kind of Flos Moutan is extracted method and the application of ethyl vanillate |
| CN108158861A (en) * | 2018-03-07 | 2018-06-15 | 安徽心缘康生物科技有限公司 | A kind of preparation method of the Essence containing peony essential oil |
| CN113332198A (en) * | 2021-06-02 | 2021-09-03 | 山西纳安生物科技股份有限公司 | Special peony active extract for daily use chemicals and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106242974A (en) * | 2016-08-02 | 2016-12-21 | 重庆工商大学 | A kind of Flos Moutan is extracted method and the application of ethyl vanillate |
| CN106242974B (en) * | 2016-08-02 | 2018-08-17 | 重庆工商大学 | The method of extraction ethyl vanillate and application in a kind of peony |
| CN108158861A (en) * | 2018-03-07 | 2018-06-15 | 安徽心缘康生物科技有限公司 | A kind of preparation method of the Essence containing peony essential oil |
| CN113332198A (en) * | 2021-06-02 | 2021-09-03 | 山西纳安生物科技股份有限公司 | Special peony active extract for daily use chemicals and preparation method thereof |
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Effective date of registration: 20230803 Address after: 101499 Jingwei Industrial Development Zone, Beifang Town, Huairou District, Beijing Patentee after: BEIJING DAWN AEROSPACE BIO-TECH Co.,Ltd. Address before: 250014 No. 19, ASTRI Road, Lixia District, Shandong, Ji'nan Patentee before: SHANDONG ANALYSIS AND TEST CENTER |