CN115813829A - Preparation method and application of gardenia extract - Google Patents
Preparation method and application of gardenia extract Download PDFInfo
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- CN115813829A CN115813829A CN202211713228.6A CN202211713228A CN115813829A CN 115813829 A CN115813829 A CN 115813829A CN 202211713228 A CN202211713228 A CN 202211713228A CN 115813829 A CN115813829 A CN 115813829A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
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Abstract
The invention provides a preparation method and application of a gardenia extract, wherein the preparation method comprises the following steps: s1: extracting gardenia fruit raw materials by using an ethanol water solution to obtain a crude extract; s2: enriching the crude extract by adopting macroporous resin to obtain eluent; s3: filtering the eluate with ultrafiltration membrane to remove macromolecular suspended impurities to obtain filtrate; s4: mixing the filtrate with a flocculating agent, and removing tannin and protein substances in the filtrate to obtain a flocculation treatment liquid; s5: mixing the flocculation treatment liquid with a decolorizing agent for decolorizing treatment, and removing pigment impurities and flocculation precipitation substances in the flocculation treatment liquid to obtain a decolorized liquid; s6: filtering the decolorized solution to remove decolorizer, and drying to obtain white powdered fructus Gardeniae extract. Through the design of the whole process, the invention successfully realizes the preparation of the colorless gardenia extract, does not contain carotenoid substances in the extract, has high safety and obvious anti-inflammatory and relieving effects. The preparation method is simple, and the product quality is stable among batches.
Description
Technical Field
The invention belongs to the technical field of preparation of gardenia extract, relates to a preparation method and application of a gardenia extract, and particularly relates to a preparation method and application of a gardenia extract without pigment.
Background
Gardenia jasminoides Ellis (Gardenia jasminoides) also known as Gardenia jasminoides Ellis: gardenia jasminoides Ellis, gardenia jasminoides Ellis and Cinobufagin are fruits of Gardenia jasminoides Ellis of Rubiaceae. The fruit of gardenia is a traditional Chinese medicine, belongs to the first batch of medical and edible dual-purpose resources issued by the Ministry of health, and has the functions of protecting liver, benefiting gallbladder, reducing blood pressure, calming, stopping bleeding, reducing swelling and the like. Is used for treating icteric hepatitis, sprain, contusion, hypertension, diabetes and other diseases in traditional Chinese medicine clinic.
Gardenia jasminoides is rich in iridoid, carotenoid, flavonoid and organic acid compounds. Of these, iridoids and carotenoids are most abundant. The water-soluble carotenoids contained in gardenia mainly comprise crocin and crocetin, and are often used as natural pigments; the iridoids mainly include genipin-1-beta gentioside, jasminoidin, deacetyl asperulosidic acid, etc. Modern pharmacological research shows that gardenia has the effects of resisting inflammation, regulating immunity, protecting cardiac muscle, relieving oxidative damage of vascular endothelial cells, resisting oxidation, protecting liver, benefiting gallbladder, reducing blood sugar and the like, wherein jasminoidin can play the roles of resisting infection and regulating immunity by reducing the level of inflammatory cytokines.
In view of the biological activity of the chemical components in gardenia, research and development of gardenia mostly concentrate on the extraction of total iridoid glycoside of gardenia (second military medical university of people's liberation army of China, CN200510026144.5[ P ]. 2005-12-14.), the extraction and purification of the total iridoid glycoside of gardenia (Yanxin Luyuan agricultural science limited company, a high-efficiency extraction method of the jasmoid glycoside, CN201611128817.2[ P ]. 2018-06-29.), and the extraction and purification of gardenia yellow pigment (Han plant research institute of Chinese academy of China, CN200310111453.3[ P ]. 2004-11-10.). The extracts obtained by different extraction methods usually have obvious yellow pigment residues. However, studies have shown that: essences and fragrances and pigments are the main sources of allergens in skin care products (Lijian, shaw Tree, liyangjie, etc. essences and fragrances safety problems and detection analysis in cosmetics [ J ] J. China J. Sanitary inspection, 2021,31 (17): 2156-2159.). Although the influence of the pigment residues in the gardenia extract obtained by the prior art on the safety of the product is not evaluated for a while, the pigment residues can significantly influence the appearance of the product among different batches, and further can greatly limit the application of the extract in skin care products, health care drinks and other finished products with high requirements on the appearance, especially some finished products applied to people with sensitive skin, and the introduction of the yellow pigment can induce or aggravate allergic symptoms (Majian, li Cheng, xuyan, safflower yellow caused allergic reaction [ J ]. Chinese misdiagnosis journal, 2010,10 (31): 7798-7798.).
The gardenia is complex in chemical components, particularly large-polarity parts, rich in substances such as colloids, tannins and proteins, easy to form colloids, not beneficial to sterilization and filtration, and easy to cause carbon leakage when decolorants are used for decoloration, so that the gardenia colorless extract is difficult to prepare. In the existing preparation process of the gardenia extract, few methods for decoloring by a decoloring agent exist, not only because pigments have little influence on finished products, but also because the decoloring agent is difficult to remove after the gardenia extract is decolored, and large-scale application is difficult to realize.
Therefore, the gardenia extract which is suitable for production, has stable quality and clear effective components, does not contain carotenoid pigment impurities and has excellent biological activity is provided, and the significance is great.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a preparation method and application of a gardenia extract, and particularly relates to a preparation method and application of a gardenia extract without pigment.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a method for preparing a gardenia extract, comprising the steps of:
s1, an extraction step: extracting the gardenia fruit raw material by using an ethanol water solution to obtain a crude extract;
s2, a separation and purification step: enriching the crude extract by adopting macroporous resin to obtain eluent;
s3, ultrafiltration step: filtering the eluent by using an ultrafiltration membrane to remove macromolecular suspended impurities to obtain filtrate;
s4, flocculation step: mixing the filtrate with a flocculating agent, and removing tannin and protein substances in the filtrate to obtain a flocculation treatment liquid;
s5, decoloring: mixing the flocculation treatment liquid with a decolorizing agent for decolorizing treatment, and removing pigment impurities and flocculation precipitation substances in the flocculation treatment liquid in one step to obtain a decolorized liquid;
s6, a drying step: filtering the decolorized solution to remove decolorizer, and drying to obtain white powdered fructus Gardeniae extract.
Preferably, the gardenia extract does not contain carotenoid substances, the content of the hydroxyisoczhiside in the gardenia extract is more than 3 percent, and the content of the geniposide is not more than 25 percent of the content of the hydroxyisoczhiside.
Preferably, the ethanol in the ethanol aqueous solution in step S1 accounts for 50% to 60% by mass, such as 50%, 51%, 52%, 53%, 54%, 55%, 56%, 57%, 58%, 59%, 60% and the like.
Preferably, the weight of the ethanol aqueous solution is 3-16 times of the weight of the gardenia fruit raw material, such as 3 times, 4 times, 5 times, 6 times, 7 times, 8 times, 9 times, 10 times, 11 times, 12 times, 13 times, 14 times, 15 times, 16 times, and the like.
Preferably, the extraction is reflux extraction.
Preferably, the extraction is carried out at a temperature of 75-85 deg.C, such as 75 deg.C, 76 deg.C, 77 deg.C, 78 deg.C, 79 deg.C, 80 deg.C, 81 deg.C, 82 deg.C, 83 deg.C, 84 deg.C, 85 deg.C, etc., for a period of 1-5h, such as 1h, 1.5h, 2h, 2.5h, 3h, 3.5h, 4h, 4.5h, 5h, etc.
Preferably, the extraction also comprises filtration and concentration under reduced pressure.
Preferably, the concentration is to concentrate the crude extract to 1-3 times, for example, 1 time, 1.2 times, 1.5 times, 1.7 times, 2 times, 2.2 times, 2.5 times, 2.7 times, 3 times, etc., of the weight of the gardenia fruit raw material.
Preferably, the type of the macroporous resin in the step S2 comprises any one of AB-8 type, D101 type or HPD100 type.
Preferably, the weight of the macroporous resin is 1.5-2.5 times, such as 1.5 times, 1.6 times, 1.7 times, 1.8 times, 1.9 times, 2 times, 2.1 times, 2.2 times, 2.3 times, 2.4 times, 2.5 times, etc., of the weight of the gardenia fruit raw material.
Preferably, said enrichment comprises in particular: loading the crude extract into macroporous resin for adsorption, eluting with water to remove impurities, eluting with 10% ethanol water solution (by mass), and collecting eluate.
Preferably, the adsorption time is 12-24h, such as 12h, 14h, 16h, 18h, 20h, 22h, 24h, and the like.
Preferably, the water is used in an amount of 0.5 to 2 times, e.g., 0.5 times, 0.7 times, 1 time, 1.2 times, 1.5 times, 1.7 times, 2 times, etc., the weight of the macroporous resin.
Preferably, the 10% ethanol aqueous solution is used in an amount of 3 to 10 times, for example, 3 times, 4 times, 5 times, 6 times, 7 times, 8 times, 9 times, 10 times, etc., the weight of the macroporous resin.
Preferably, the size of the ultrafiltration membrane of step S3 is 30000-70000Da, such as 30000Da, 35000Da, 40000Da, 45000Da, 50000Da, 55000Da, 60000Da, 65000Da, 70000Da, etc.
Preferably, the flocculant of step S4 comprises any one of gelatin, chitosan or carboxymethyl chitosan or a combination of at least two thereof.
Preferably, the flocculant is used in an amount of 0.005% to 0.01% by weight of the filtrate, such as 0.005%, 0.0055%, 0.006%, 0.0065%, 0.007%, 0.0075%, 0.008%, 0.0085%, 0.009%, 0.0095%, 0.01%, etc.
Preferably, the mixing in step S4 is carried out at 50-60 deg.C, such as 50 deg.C, 51 deg.C, 52 deg.C, 53 deg.C, 54 deg.C, 55 deg.C, 56 deg.C, 57 deg.C, 58 deg.C, 59 deg.C, 60 deg.C, etc., for 10-30min, such as 10min, 15min, 20min, 25min, 30min, etc.
Preferably, the mixing in step S4 is performed under stirring at a speed of not higher than 100rpm, for example, 10rpm, 20rpm, 30rpm, 40rpm, 50rpm, 60rpm, 70rpm, 80rpm, 90rpm, 100rpm, etc.
Preferably, the decolorizing agent of step S5 comprises activated carbon.
Preferably, the decolorizing agent is used in an amount of 0.5% to 1%, e.g., 0.5%, 0.55%, 0.6%, 0.65%, 0.7%, 0.75%, 0.8%, 0.85%, 0.9%, 0.95%, 1%, etc., by weight of the filtrate of step S4.
Preferably, the mixing in step S5 is performed at 50-60 deg.C, such as 50 deg.C, 51 deg.C, 52 deg.C, 53 deg.C, 54 deg.C, 55 deg.C, 56 deg.C, 57 deg.C, 58 deg.C, 59 deg.C, 60 deg.C, etc., for 20-120min, such as 20min, 30min, 40min, 50min, 60min, 70min, 80min, 90min, 100min, 110min, 120min, etc.
Preferably, the temperature of the drying in step S6 does not exceed 40 ℃.
Preferably, the drying means comprises any one or a combination of at least two of freeze drying, oven drying or spray drying.
In a second aspect, the present invention provides use of the gardenia extract obtained by the preparation method according to the first aspect in preparing a skin care or cosmetic.
In a third aspect, the present invention provides the use of the gardenia extract obtained by the preparation method of the first aspect in the preparation of a TRPV-1 inhibitor, a TNF- α inhibitor, an IL-6 inhibitor or a NO secretion inhibitor.
In a fourth aspect, the present invention provides a method of inhibiting NO secretion, the method comprising: the gardenia extract obtained by the production method as described in the first aspect is administered to a target cell or tissue.
In a fifth aspect, the present invention provides a method of inhibiting TRPV-1 expression, the method comprising: the gardenia extract obtained by the production method as described in the first aspect is administered to a target cell or tissue.
In a sixth aspect, the present invention provides a method of inhibiting TNF- α secretion, the method comprising: administering the gardenia extract obtained by the production method as described in the first aspect to a target cell or tissue.
In a seventh aspect, the present invention provides a method of inhibiting IL-6 secretion, the method comprising: administering the gardenia extract obtained by the production method as described in the first aspect to a target cell or tissue.
The recitation of numerical ranges herein includes not only the above-recited values, but also any values between any of the above-recited numerical ranges not recited, and for brevity and clarity, is not intended to be exhaustive of the specific values encompassed within the range.
Compared with the prior art, the invention has the following beneficial effects:
(1) The preparation method of the invention can fully extract the high-polarity active ingredients in the gardenia;
(2) According to the preparation method, macromolecular impurities introduced in the gardenia extraction process can be removed to the greatest extent through an ultrafiltration process;
(3) The preparation method can remove colloid, protein, pigment and other impurities in the gardenia by one step, and the obtained extract does not contain gardenia yellow pigment.
(4) The gardenia extract prepared by the method is white powder, the main components of the gardenia extract are polyphenol, hydroxygardenia glycoside and jasminoidin, and when the gardenia extract is prepared into a solution, the solution is colorless, clear and transparent, and can be widely used in products with high requirements on color, such as skin care products and the like.
(5) The gardenia extract obtained by the preparation method disclosed by the invention has better activity shown by cell anti-inflammatory experiments and relieving experimental results, and can be used as an active substance for skin care products;
(6) The gardenia extract obtained by the preparation method of the invention is ensured not to have phototoxicity and the safety of the gardenia extract is ensured through a phototoxicity detection test; ensuring that the composition has no sensitization through sensitization experiments;
(7) The quality of the product obtained by the preparation method is controlled by two monomer compounds of the hydroxyl gardenia glycoside and the gardenia glycoside, so that the quality stability of the product in batches is ensured, and the product can be used for commercialization.
Through the design of the whole process, the invention successfully realizes the preparation of the colorless gardenia extract, the extract does not contain carotenoid substances, the content of the hydroxyisoczhiside is more than 3 percent, and the content of the geniposide does not exceed 25 percent of the content of the hydroxyisoczhiside. The extract has remarkable inhibitory effect on TRPV-1, TNF-alpha, IL-6 and NO secretion, and can be used for preparing skin care products or cosmetics with soothing and anti-inflammatory effects.
Drawings
FIG. 1 is a flow chart of the preparation of Gardenia jasminoides Ellis extract;
FIG. 2 is a graph showing the results of the main components in different elution sites of the Gardenia jasminoides Ellis extract;
FIG. 3 is a graph showing the results of an inflammatory factor inhibition experiment using different Gardenia jasminoides Ellis extracts, wherein a is a graph showing the results of inhibition of NO secretion, b is a graph showing the results of inhibition of IL-6 secretion, and c is a graph showing the results of inhibition of TNF- α secretion;
FIG. 4 is a graph showing the result of inhibition of TRPV-1 by Gardenia jasminoides Ellis extract.
Detailed Description
The technical solution of the present invention is further described below by way of specific embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitation of the present invention.
In the following examples, all reagents and consumables were purchased from conventional reagent manufacturers in the field unless otherwise specified; unless otherwise indicated, all experimental methods and technical means used are those conventional in the art.
Referring to the flow chart of FIG. 1, the solvent formulations in the following examples are all mass ratios.
The fructus Gardeniae raw material is dry fructus Gardeniae, which is obtained from Kunming city, yunnan province, active carbon is medicinal active carbon, which is obtained from Shanghai activated carbon plant, inc., and gelatin, chitosan, and carboxymethyl chitosan are obtained from Shanghai Aladdin reagent.
Research experiment
1. Selection of elution sites
S1, an extraction step: extracting 100g of gardenia fruit raw material twice with 1L of 60% ethanol/water mixed solution under reflux for 1.5 hours each time, filtering the extracting solution, and concentrating under reduced pressure to 196g to obtain a deep red crude extracting solution;
s2, a separation and purification step: loading 200g of activated AB-8 type macroporous resin into a column, adsorbing a crude extract obtained in the extraction step for 18 hours, eluting with 200g of pure water to remove insoluble substances, and sequentially eluting with 1Kg of 10% ethanol, 20% ethanol and 50% ethanol at the elution speed of 2BV/h; the 10% ethanol eluent is in an opaque orange color for standby; the 20% ethanol eluent is a clear red solution for standby; the 50% ethanol eluent is a clear deep red solution for standby;
LC-MS analysis
The chemical composition analysis is carried out on the three eluted fractions by using LC-MS, the chromatogram is shown as the attached figure 2, and the main chemical compositions of each fraction are as follows:
anti-inflammatory Activity assay
The results of inflammatory factor inhibition experiment tests on the three elution parts respectively show that the 10% ethanol elution part has stronger inhibition effect on inflammatory factors compared with 20% and 50% fractions, so that the 10% ethanol elution part is selected as a follow-up research target.
2. Selection of Ultrafiltration Process
Filtering 10% of elution part by a 800-mesh sieve, performing ultrafiltration to remove impurities, and respectively filtering by 50000Da and 100000Da filter membranes to obtain two kinds of filtrate, wherein the two kinds of filtrate are clear yellow-green solutions through comparison, but a sample obtained by filtering by the 100000Da filter membrane can generate a Tyndall phenomenon when irradiated by light, and a sample filtered by the 50000Da filter membrane is clear and transparent and has no Tyndall phenomenon. Therefore, the 50000Da filter was chosen to filter the resulting sample for the subsequent purification step.
3. Selection of decolorizing Process
The filtrate obtained by ultrafiltration was decolorized (flocculant was 1% gelatin aqueous solution) under different conditions, and the results were as follows
The greatest technical problem encountered in the decolorization process is carbon leakage, namely: when the decolored active carbon is removed by filter paper or an industrial titanium rod, the obtained filtrate is dark gray, and clear and transparent filtrate can be obtained only by filtering with a filter membrane of 0.22 mu m, so that large-scale production is difficult to realize.
When the added activated carbon content is more than or equal to 2%, the carbon leakage phenomenon disappears, but the solid content in the decolored liquid is extremely low, and the LC-MS analysis result shows that the main chromatographic peaks in the decolored liquid almost completely disappear, so that the application value is low.
Before the activated carbon is added, a certain amount of flocculant with the mass concentration of 1% is added, and after decoloration, the activated carbon can be completely removed by using filter paper, but the addition of the flocculant and the activated carbon can influence the decoloration effect. When the addition amount of flocculant is 0.5% or 1% and the addition amount of active carbon is 0.5%, the obtained fructus Gardeniae extract is colorless and transparent, and is lyophilized to obtain white fructus Gardeniae extract powder.
Example 1
S1, an extraction step: extracting 102g of gardenia fruit raw material twice with 1L of 60% ethanol-water mixed solution at 80 ℃ under reflux for 1.5 hours each time, filtering the extract (200-mesh screen), and concentrating under reduced pressure to 190g to obtain a deep red crude extract;
s2, a separation and purification step: 204g of activated AB-8 type macroporous resin is filled into a column, the crude extract obtained in the step of S1 extraction is loaded and adsorbed for 12 hours, 204g of pure water is firstly used for eluting to remove insoluble substances, then 10 percent ethanol is used for eluting for 1Kg, the elution speed is 2BV/h, and the eluent is in an opaque orange color and is the target fraction;
eluting with 20% ethanol for 1Kg until the eluate is a clear red solution for later use;
eluting with 50% ethanol to obtain 1Kg of clear dark red solution;
s3, ultrafiltration step: filtering with 800 mesh screen to remove target fraction obtained in the separation and purification step, filtering the obtained filtrate with 50000Da filter membrane to obtain ultrafiltrate, and adding 10% ethanol into the filtrate to weight of 1Kg;
s4, flocculation step: preparing 1% flocculant (namely heating and dissolving gelatin by using water, and then cooling for later use), adding 5g of the prepared flocculant into 1Kg of ultrafiltrate, heating to 50 ℃, and stirring at 80rpm for 10min;
s5, decoloring: adding 5g of activated carbon into the orange ultrafiltrate treated by the flocculation step, continuously maintaining the temperature at 50 ℃, stirring at 80rpm for 30min, and filtering by qualitative filter paper to remove the activated carbon to obtain clear and transparent filtrate;
s6, low-temperature drying: freeze drying the clear filtrate to obtain 3.1g of white powdered fructus Gardeniae extract.
Respectively processing 20% of the standby component and 50% of the standby component by the steps S3-S6 to respectively obtain gardenia extract powder for later use.
Example 2
S1, an extraction step: extracting 105g of gardenia fruit raw material twice with 1L of 60% ethanol mixed solution at 80 ℃ under reflux for 1.5 hours each time, filtering the extract, and concentrating under reduced pressure to 201g to obtain a deep red crude extract;
s2, a separation and purification step: loading 201g of activated AB-8 type macroporous resin into a column, adsorbing a crude extract obtained in the step of S1 for 12 hours, eluting with 201g of pure water to remove insoluble substances, and then eluting with 1Kg of 10% ethanol at an elution speed of 2BV/h, wherein the eluent is in an opaque orange color and is a target fraction;
s3, ultrafiltration step: filtering with 800 mesh screen to remove target fraction obtained in the separation and purification step, filtering the obtained filtrate with 50000Da filter membrane to obtain ultrafiltrate, and adding 10% ethanol into the filtrate to weight of 1Kg;
s4, flocculation step: preparing 1% flocculant, namely heating and dissolving gelatin by using water, cooling for later use, adding 2.5g of flocculant into 1Kg of ultrafiltrate, heating to 50 ℃, and stirring at 80rpm for 10min;
s5, decoloring: adding 5g of activated carbon into the orange ultrafiltrate treated by the flocculation step, continuously keeping the temperature at 50 ℃, stirring at 80rpm for 30min, filtering by qualitative filter paper to remove the activated carbon to obtain gray turbid filtrate, repeatedly filtering by the filter paper to obtain turbid filtrate, performing secondary filtration on the filtrate by using a 0.22-micron nylon membrane, wherein the filtering speed is extremely low, and macroscopic activated carbon particles appear, and carbon leakage occurs.
And (4) conclusion: in this example, the flocculant addition was insufficient, resulting in carbon leakage.
Example 3
S1, an extraction step: extracting 99g of gardenia fruit raw material twice with 1L of 60% ethanol mixed solution at 80 ℃ under reflux for 1.5 hours each time, filtering the extract, and concentrating under reduced pressure to 195g to obtain a deep red crude extract;
s2, a separation and purification step: loading 200g of activated AB-8 type macroporous resin into a column, loading the crude extract obtained in the extraction step for adsorption for 12 hours, eluting with 200g of pure water to remove insoluble substances, eluting with 10% ethanol at a speed of 2BV/h for 1Kg, wherein the eluent is in an opaque orange color and is the target fraction;
s3, ultrafiltration step: filtering with 800 mesh screen to remove target fraction obtained in the separation and purification step, filtering the obtained filtrate with 50000Da filter membrane to obtain ultrafiltrate, and adding 10% ethanol into the filtrate to weight of 1Kg;
s4, flocculation step: preparing 1% flocculant, namely heating and dissolving gelatin by using water, cooling for later use, adding 5g of the prepared flocculant into 1Kg of orange ultrafiltrate, heating to 50 ℃, and stirring at 80rpm for 10min;
s5, decoloring: adding 3g of activated carbon into the orange ultrafiltrate treated by the flocculation step, continuously keeping the temperature at 50 ℃, stirring at 80rpm for 30min, and filtering by qualitative filter paper to remove the activated carbon to obtain clear and transparent filtrate;
s6, low-temperature drying: and freeze-drying the clear and transparent filtrate to obtain 3.5g of gardenia extract in light yellow-green powder.
And (4) conclusion: in this example, the amount of activated carbon added was insufficient, resulting in incomplete decolorization.
Example 4
S1, an extraction step: extracting 103g of gardenia fruit raw material twice with 1L of 50% ethanol-water mixed solution at 75 ℃ under reflux for 1 hour each time, filtering the extracting solution, and concentrating under reduced pressure to 197g to obtain a deep red crude extracting solution;
s2, separation and purification: loading 201g of activated HPD100 type macroporous resin into a column, loading the crude extract obtained in the extraction step for adsorption for 12 hours, eluting with 201g of pure water to remove insoluble substances, eluting with 10% ethanol at a speed of 2BV/h for 1Kg, wherein the eluent is opaque orange, and is the target fraction;
s3, ultrafiltration step: filtering with 800 mesh screen to remove target fraction obtained in the separation and purification step, filtering the obtained filtrate with 50000Da filter membrane to obtain ultrafiltrate, and adding 10% ethanol into the filtrate to weight of 1Kg;
s4, flocculation step: preparing 1% flocculant, namely heating and dissolving chitosan with water, cooling for later use, adding 7.5g of the prepared flocculant into 1Kg of orange ultrafiltrate, heating to 50 ℃, and stirring at 80rpm for 10min;
s5, decoloring: adding 8g of activated carbon into the orange ultrafiltrate treated by the flocculation step, continuously maintaining the temperature at 50 ℃, stirring at 80rpm for 30min, and filtering by qualitative filter paper to remove the activated carbon to obtain clear and transparent filtrate;
s6, low-temperature drying: freeze drying the clear filtrate to obtain white powdered cape jasmine fruit extract 2.3g.
Example 5
S1, an extraction step: extracting 100g of gardenia fruit raw material twice with 1L of 60% ethanol-water mixed solution at 85 ℃ under reflux for 1.5 hours each time, filtering the extracting solution, and concentrating under reduced pressure to 196g to obtain a deep red crude extracting solution;
s2, a separation and purification step: 202g of activated D101 type macroporous resin is filled into a column, crude extract obtained in the extraction step is loaded and adsorbed for 12 hours, 202g of pure water is firstly used for eluting to remove insoluble substances, then 10 percent ethanol is used for eluting 0.8Kg, the elution speed is 2BV/h, and the eluent is in an opaque orange color and is a target fraction;
s3, ultrafiltration step: filtering with 800 mesh screen to remove target fraction, filtering with 50000Da filter membrane to obtain ultrafiltrate, and adding 10% ethanol into the filtrate to weight of 0.8Kg;
s4, flocculation step: preparing 1% flocculant, namely heating and dissolving carboxymethyl chitosan with water, cooling for later use, adding 8g of prepared flocculant into 0.8Kg of orange ultrafiltrate, heating to 55 ℃, and stirring at 80rpm for 10min;
s5, decoloring: adding 8g of activated carbon into the orange ultrafiltrate treated by the flocculation step, continuously maintaining the temperature at 55 ℃, stirring at 80rpm for 30min, and filtering by qualitative filter paper to remove the activated carbon to obtain clear and transparent filtrate;
s6, low-temperature drying: freeze drying the clear filtrate to obtain white powdered fructus Gardeniae extract 2.2g.
Example 6
S1, an extraction step: reflux-extracting 20Kg of gardenia fruit raw material twice with 200Kg of 55% ethanol-water mixed solution for 1.5 hours each time, filtering the extract, and concentrating under reduced pressure to 38.6Kg to obtain a deep red crude extract;
s2, a separation and purification step: loading 40Kg of activated AB-8 type macroporous resin into a column, loading the crude extract obtained in the extraction step for adsorption for 16 hours, eluting with 40Kg of pure water to remove insoluble substances, then eluting with 10% ethanol at a rate of 2BV/h to obtain 200Kg of eluate in the shape of an opaque orange, which is the target fraction;
s3, ultrafiltration step: filtering with 800 mesh screen to remove target fraction obtained in the separation and purification step, filtering the obtained filtrate with 50000Da filter membrane to obtain ultrafiltrate, and adding 10% ethanol into the filtrate to weight of 200Kg;
s4, flocculation step: preparing 1% flocculant, namely heating and dissolving the flocculant by using water, cooling for later use, adding 1.0Kg of flocculant into 200Kg of orange ultrafiltrate, heating to 50 ℃, and stirring at 80rpm for 20min;
s5, decoloring: adding 1.0Kg of activated carbon into the orange ultrafiltrate treated by the flocculation step, keeping the temperature at 50 ℃, stirring at 80rpm for 30min, and filtering to remove the activated carbon to obtain clear and transparent filtrate;
s6, low-temperature drying: concentrating the clear transparent filtrate under reduced pressure, and freeze drying to obtain 0.62Kg of fructus Gardeniae extract in the form of white powder.
Test example
(1) The gardenia extract obtained in the above example was subjected to component detection (LC-MS), and the mass content results of each component were as follows, wherein the method in example 6 was subjected to 3 repeated tests to verify batch stability:
the results show that: the gardenia extract obtained by the extraction of each embodiment is mostly polyphenols and saccharides, wherein the content of the hydroxygeniposide is more than 3%, only a small amount of the gardenia glycoside is contained, the content of the gardenia glycoside is not more than 25% of the content of the hydroxygeniposide, and carotenoid pigment substances are not contained. The component contents of different batches have no obvious difference, which shows that the extraction method has high stability and is suitable for batch production.
(2) The three gardenia extracts obtained in example 1 were subjected to an inflammatory factor inhibition test by the following method: selecting mouse macrophage RAW264.7, spreading cells on 96-well plate, inoculating initial cell number 1 × 10 4 ～1×10 5 After the cells grow to the number required by the experiment, the gardenia extract and the positive medicine intervene for 1h, and after the medicine intervenes for 1h, LPS lipopolysaccharide is added, and the culture is continued for 24h. Collecting the supernatant, and determining the content thereofAmount of inflammatory factor NO/IL-6/TNF-alpha.
The results are shown in figure 3, (a is a result graph of inhibiting NO secretion, B is a result graph of inhibiting IL-6 secretion, C is a result graph of inhibiting TNF-alpha secretion, CTRL is a blank group, LPS is a model group, DEX is a positive dexamethasone group, A is a gardenia extract prepared by eluting with 10% ethanol, B is a gardenia extract prepared by eluting with 20% ethanol, C is a gardenia extract prepared by eluting with 50% ethanol, and the detection concentration of A/B/C is 0.5 mg/mL): similar to the results of the previous research experiments, the gardenia extract obtained by eluting with 10% ethanol has significantly stronger inhibitory effect on three inflammatory factors than the gardenia extract obtained by eluting with 20% and 50%.
(3) The gardenia extract obtained in example 6 was evaluated for its soothing effect by measuring the protein content of capsaicin receptor (TRPV 1) using keratinocytes-based test method: inoculating keratinocyte to a 6-well plate, culturing overnight, then administering, fixing with 4% paraformaldehyde, fixing for 30min, performing immunofluorescence detection of capsaicin receptor (TRPV 1), taking a picture under a microscope, collecting the picture, and analyzing the TRPV-1 inhibition effect.
The results are shown in FIG. 4, BC blank; NC is a model group; PC is a positive control group (trans-4-tert-butylcyclohexanol); the use amount of the gardenia extract is 0.125%, and the gardenia extract has good TRPV-1 inhibition activity according to the expression amount of TRPV-1.
The gardenia extract obtained by the preparation method of the invention is subjected to a phototoxicity detection test according to the technical specification for cosmetic safety 2015, and the result shows that the gardenia extract has no phototoxicity at a concentration of 4 mg/mL.
The applicant states that the present invention is illustrated by the above examples to describe the preparation method and application of gardenia extract of the present invention, but the present invention is not limited to the above examples, i.e., it is not meant that the present invention must be implemented by the above examples. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition.
Claims (10)
1. The preparation method of the gardenia extract is characterized by comprising the following steps:
s1, an extraction step: extracting gardenia fruit raw materials by using an ethanol water solution to obtain a crude extract;
s2, a separation and purification step: enriching the crude extract by adopting macroporous resin to obtain eluent;
s3, ultrafiltration step: filtering the eluate with ultrafiltration membrane to remove macromolecular suspended impurities to obtain filtrate;
s4, flocculation step: mixing the filtrate with a flocculating agent, and removing tannin and protein substances in the filtrate to obtain a flocculation treatment liquid;
s5, decoloring: mixing the flocculation treatment liquid with a decolorizing agent for decolorizing treatment, and removing pigment impurities and flocculation precipitation substances in the flocculation treatment liquid in one step to obtain a decolorized liquid;
s6, a drying step: filtering the decolorized solution to remove decolorizer, and drying to obtain white powdered fructus Gardeniae extract.
2. The method of preparing gardenia extract according to claim 1, wherein the gardenia extract does not contain carotenoid, the content of the hydroxygeniposide in the gardenia extract is more than 3%, and the content of the geniposide is not more than 25% of the content of the hydroxygeniposide.
3. The method of preparing gardenia extract according to claim 1 or 2, wherein the mass ratio of ethanol in the ethanol aqueous solution of step S1 is 50% to 60%;
preferably, the weight of the ethanol water solution is 3-16 times of that of the gardenia fruit raw material;
preferably, the extraction is reflux extraction;
preferably, the extraction temperature is 75-85 ℃ and the extraction time is 1-5h;
preferably, the extraction also comprises filtration and concentration under reduced pressure;
preferably, the concentration is to concentrate the crude extract to 1-3 times of the weight of the gardenia fruit raw material.
4. The method of preparing gardenia extract according to any one of claims 1 to 3 wherein the type of macroporous resin used in the step S2 includes any one of AB-8 type, D101 type or HPD100 type;
preferably, the weight of the macroporous resin is 1.5-2.5 times of that of the gardenia fruit raw material;
preferably, said enrichment comprises in particular: loading the crude extract into macroporous resin for adsorption, eluting with water to remove impurities, eluting with 10% ethanol water solution, and collecting eluate;
preferably, the adsorption time is 12-24h;
preferably, the amount of water is 0.5-2 times of the weight of the macroporous resin;
preferably, the 10% ethanol aqueous solution is used in an amount of 3 to 10 times the weight of the macroporous resin.
5. The method of preparing gardenia extract according to any one of claims 1 to 4 wherein the size of the ultrafiltration membrane of step S3 is 30000 to 70000Da.
6. The method of preparing gardenia extract according to any one of claims 1 to 5, wherein the flocculant of step S4 comprises any one or a combination of at least two of gelatin, chitosan or carboxymethyl chitosan;
preferably, the dosage of the flocculating agent is 0.005-0.01% of the weight of the filtrate;
preferably, the mixing temperature in the step S4 is 50-60 ℃, and the mixing time is 10-30min;
preferably, the mixing in step S4 is performed under stirring, the stirring speed being not higher than 100rpm.
7. The method of preparing gardenia extract according to any one of claims 1 to 6, wherein the decolorant of step S5 comprises activated carbon;
preferably, the dosage of the decoloring agent is 0.5 to 1 percent of the weight of the filtrate obtained in the step S4;
preferably, the mixing temperature of step S5 is 50-60 deg.C, and the mixing time is 20-120min.
8. The method of preparing gardenia extract according to any one of claims 1 to 7, wherein the temperature of drying in step S6 is not more than 40 ℃;
preferably, the drying means comprises any one or a combination of at least two of freeze drying, oven drying or spray drying.
9. Use of the gardenia extract obtained by the production method as described in any one of claims 1 to 8 for the production of skin care or cosmetics.
10. Use of the gardenia extract obtained by the preparation method according to any one of claims 1 to 8 for preparing a TRPV-1 inhibitor, a TNF- α inhibitor, an IL-6 inhibitor or a NO secretion inhibitor.
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| CN116605944A (en) * | 2023-05-31 | 2023-08-18 | 宝萃生物科技有限公司 | Flocculation adsorption composition and application thereof in preparation of phyllanthus emblica fruit extract |
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