CN108186456A - A kind of preparation method of freckle removing and whitening emblic extract - Google Patents

A kind of preparation method of freckle removing and whitening emblic extract Download PDF

Info

Publication number
CN108186456A
CN108186456A CN201810191017.8A CN201810191017A CN108186456A CN 108186456 A CN108186456 A CN 108186456A CN 201810191017 A CN201810191017 A CN 201810191017A CN 108186456 A CN108186456 A CN 108186456A
Authority
CN
China
Prior art keywords
emblic
whitening
concentration
preparation
freckle removing
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201810191017.8A
Other languages
Chinese (zh)
Other versions
CN108186456B (en
Inventor
崔涛
梅双喜
苏梅
周林
查雨锋
杨和金
李学琴
王大元
高英
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Yunnan Pharmaceutical Institute
Original Assignee
Yunnan Pharmaceutical Institute
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Yunnan Pharmaceutical Institute filed Critical Yunnan Pharmaceutical Institute
Priority to CN201810191017.8A priority Critical patent/CN108186456B/en
Publication of CN108186456A publication Critical patent/CN108186456A/en
Application granted granted Critical
Publication of CN108186456B publication Critical patent/CN108186456B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • A61Q19/02Preparations for care of the skin for chemically bleaching or whitening the skin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/80Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
    • A61K2800/805Corresponding aspects not provided for by any of codes A61K2800/81 - A61K2800/95
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/80Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
    • A61K2800/82Preparation or application process involves sonication or ultrasonication
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/80Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
    • A61K2800/84Products or compounds obtained by lyophilisation, freeze-drying

Abstract

The present invention provides a kind of preparation methods of the emblic extract with freckle removing and whitening activity.Using emblic fruit as raw material, extracted, filtered by low temperature, the concentration of extracting solution low temperature, separation of solid and liquid, purification with macroreticular resin, eluent concentration, low temperature drying, obtain emblic extract.After testing, for the extraction chemical constituent based on total tannin, impurity component general flavone content is less than 5%.Through melanin inhibit test evaluation, the extract freckle removing and whitening activity significantly, without skin irritation.

Description

A kind of preparation method of freckle removing and whitening emblic extract
Technical field
The invention belongs to cosmetic fields, are related to the preparation method of emblic extract and with the remaining of freckle removing and whitening activity The preparation method of sweet seed extract.
Background technology
Emblic (Phyllanthus emblica L.) is Euphorbiaceae (Euphorbiaceae) Leafflower (Phyllanthus) fruit, alias Yunnan olive, Phyllanthus embical fruit, mountain oil are sweet, emblic leafflower fruit, Niuganguo, pyhllanth usemhlica L., poplar are sweet, Hui Ganzi Deng.Emblic originates in India, Thailand, Philippine, Malaysia, Pakistan etc., maximum with the yield of India and China.It is remaining Sweet son is distributed mainly on the provinces and regions such as Yunnan, Guangxi, Guangdong, Fujian, Guizhou, Sichuan, Taiwan, Hainan in China, with Yunnan, Fujian Yield is maximum.Emblic light is shone, can be drought-resistant well, therefore, is had very well to the torrid zone, subtropical zone dry-hot valley ecological environment Adaptability.Column condition, natural community's large area of emblic are preferably met in China adaptability ofgrowth area It is distributed in this.The root system of plant is flourishing, and sand prevention is solid native well for energy, and to preventing erosion, improving the ecological environment, there have to be positive Effect.Therefore, emblic is resourceful, and growth or cultivation are conducive to ecological environment, suitable for developing and using.
Emblic Clinical practice is with a long history and safety is good.Record in《Chinese Pharmacopoeia》, belong to Tibetan and commonly use medicine, have The effect of " clearing heat and cooling blood, food digesting stomach fortifying, cough-relieving of promoting the production of body fluid ", " removes, indigestion, abdominal distension , gai cough, laryngalgia, mouth for blood-head blood It is dry " etc. illnesss.Emblic medicine-food two-purpose records what is announced within 2002 in the Ministry of Public Health《It is both food and the item name of drug It is single》, in the civil custom for having and eating fresh fruit of fructus phyllanthi raw.
Modern plants chemical research shows that emblic mainly contains following chemical composition:Polyphenols, organic acid, carbohydrate, The substances such as vitamin, amino acid and trace elements zn, Mn, Fe, Ca and Se etc., wherein, it is noteworthy characterized by containing a large amount of Polyphenol and abundant vitamin C.Polyphenols mainly has:Glucose alkaloid (glucogallin), gallic acid (gallic acid), benzoaric acid (e11agic acid), corilagin (corlagin), terchebin (terchebin), chebulinic acid (chebulinc acid), 3,6- digalloylglucose glycosides (3,6- Digalloylglucose), 3- ethyls gallic acid (3-ethoxy-4,5-dihydroxy-bezoic acid), glactaric acid (mucic acid) and phyllemblic acid (phyllemblic acid) etc..It is anti-that modern pharmacology research shows that emblic mainly has The effects that oxidation, resisting pathogenic microbes, anti-mutagenesis, teratogenesis, antitumor, lipid-loweringing, blood pressure lowering.
At present, having foreign patent report phyllemblic tannin constituents has preferable freckle removing and whitening activity.China's emblic It is resourceful, and the plant medicine-food two-purpose, it is safe and non-toxic, provide good condition for freckle removing and whitening class product development.
Invention content
The object of the present invention is to provide it is a kind of can industrialized production, there is the emblic extract of freckle removing and whitening activity Preparation method, emblic extract active ingredient total tannin content height, the impurity component general flavone content of gained are low, appearance color It is shallow, it is safe and non-toxic, it is well positioned to meet the market demand of freckle removing and whitening.
To achieve the above object, the present invention provides a kind of preparation sides of the emblic extraction with freckle removing and whitening activity Method, the step of progress including order below:
A kind of preparation method of freckle removing and whitening emblic extract, which is characterized in that the system of the emblic extract Preparation Method includes the following steps:
Emblic fruit, low temperature extraction, filtering, the concentration of filtrate low temperature, concentrate are dissolved in water, and separation of solid and liquid clarifies aqueous Upper purification with macroreticular resin, elutes through different concentration ethanol, collects the ethanol eluate of specific alcoholic degree, concentrates, dry, detection Qualification, packaging, obtains emblic extract.
The preparation method of a kind of freckle removing and whitening emblic extract, which is characterized in that low temperature extraction process includes: 1. extracting mode is emblic fruit, crushes or do not crush, low temperature extraction, especially with cold soaking, temperature leaching, ultrasonic one kind or number The combination of kind method extracts;2. extraction solvent is acetone, the arbitrary composition of one or several kinds of solvents of methanol, ethyl alcohol, water The aqueous acetone solution of ratio, particularly 40%~70%, 40%~70% ethanol water, 40%~70% methanol are water-soluble Liquid;3. solvent dosage is 3~100 times/time of emblic weight, particularly the 5~30 of emblic weight times;4. extraction time is 0.5~for 24 hours/secondary;5. extraction time is 1~5 time, particularly 1~3 time.
The preparation method of a kind of freckle removing and whitening emblic extract, which is characterized in that low-temperature concentration process includes: 1. thickening temperature is 30~70 DEG C, particularly 40~60 DEG C;2. condensing mode is the equipment of low temperature concentration, to extract liquid dense The equipment that contracting, particularly falling film concentration, micro-filtration membrane concentration, ultrafiltration membrane concentration, NF membrane concentration, reverse osmosis membrane concentrate;3. it concentrates Terminal is be concentrated into organic solvent-free or volume about emblic weight 1~3 times.
The preparation method of a kind of freckle removing and whitening emblic extract, which is characterized in that solid-liquid separation process includes: Concentrate adds purified water, and to 2~5 times of emblic weight, mixing makes the precipitation in concentrate be completely dissolved in water, Ran Houjin Row separation of solid and liquid operate, centrifuged using centrifugation apparatus, plate-frame filtering, micro-filtration film device filtering, filter-cloth filtering mode, particularly Centrifugation apparatus centrifuges, and collects the aqueous of no precipitation.
The preparation method of a kind of freckle removing and whitening emblic extract, which is characterized in that purifying process includes:It is 1. big Macroporous adsorbent resin type:Using the macroporous absorbent resin of big polarity or medium and small polarity, as HPD826, LS305, HPD100, LX~ 68M, JKSB-1 etc.;2. macroporous absorbent resin pre-treatment:It is clean using high concentration ethanol or through processing such as alkali, acid, ethyl alcohol;On 3. Sample amount:Applied sample amount is 0.1~5 times of obtained clarification aqueous of (w/v) emblic of macroporous absorbent resin;4. it elutes:After loading Large pore resin absorption column, purified different concentration ethanol elution successively collects 10%~80% ethanol eluate, particularly 10%~40% ethanol eluate.
The preparation method of a kind of freckle removing and whitening emblic extract, which is characterized in that ethanol eluate concentrates work Skill includes:1. the ethanol eluate low temperature concentration of upper prop elution gained;2. thickening temperature:To prevent high temperature extracting solution chemical Ingredient, low temperature range are 10~70 DEG C, particularly 20~60 DEG C;3. condensing mode:The equipment concentrated using energy low temperature is carried out Extracting solution concentrates, and particularly falling film concentration, micro-filtration membrane concentration, ultrafiltration membrane concentration, NF membrane concentration, reverse osmosis membrane concentration etc. is set It is standby;4. striking point:It is concentrated into relative density 1.0~2.0, particularly 1.05~1.20.
The preparation method of a kind of freckle removing and whitening emblic extract, which is characterized in that drying process is using micro- Wave drying, the combination one or several kinds of drying modes such as vacuum freeze drying, be dried under reduced pressure, be spray-dried carry out the dry of concentrate Dry, the combination especially with one or several kinds of modes such as vacuum freeze drying, spray drying, microwave drying carries out concentrate It is dry.
The preparation method of a kind of freckle removing and whitening emblic extract, which is characterized in that emblic fruit and liquid are straight The water of contact is deionized water or purified water.
The preparation method of a kind of freckle removing and whitening emblic extract, which is characterized in that emblic extract is most End form formula is powder or dry cream.
A kind of preparation method of freckle removing and whitening emblic extract, which is characterized in that the total tan of emblic extract Matter content is more than 30%, and particularly 40~80%, general flavone content is less than 5%, especially less than 1%.
The preparation method of a kind of freckle removing and whitening emblic extract, which is characterized in that emblic extract has The effect of freckle removing and whitening and without skin irritation, skin lightening, whitening or the makeup of nti-freckle can be used in as main active In product.
The present invention has the following advantages:
(1) stable processing technique, feasible, is suitable for industrialized large-scaled production.
(2) the emblic extract freckle removing and whitening activity prepared by above-mentioned technique is notable.
(3) product is originated from the emblic fruit of medicine-food two-purpose, is not added with any exogenous components, safe to use.
(4) quality standard is scientific and reasonable, to having effective control in effect ingredient (total tannin), impurity component (general flavone) And detection.
(5) production technology is advanced, has used and has been concentrated and dried method suitable for the extraction of heat sensitive material, such as ultrasonic wave or microwave Extraction, film concentration, falling film concentration, vacuum freeze drying, microwave drying, spray drying etc..
Description of the drawings:
Fig. 1 emblic extraction production technology general flow charts
Specific embodiment
The present invention is further described with reference to example.Although above-mentioned elaborate the present invention, this hair Bright example without being limited thereto, those skilled in the art can be modified with principle according to the present invention, therefore, all according to this The various modifications that the principle of invention carries out all should be understood to fall into protection scope of the present invention.
Embodiment 1
Fresh fruit of fructus phyllanthi 100kg, drinking water are cleaned, coarse crushing, add extraction 1 time in 40% EtOH Sonicate extraction equipment, extraction Time 120min, 40% ethanol consumption are 30 times of amounts (V/W), and the filtration of 100 mesh filter cloth of extracting solution, filtrate is in falling film concentration plants In, 60 DEG C are concentrated under reduced pressure into no alcohol, and concentrate adds purified water to be dissolved to 3 times of amounts of emblic weight, tube centrifuge centrifugation, from Heart liquid is added on the LX-68M macroporous absorption columns balanced through soda acid, 95% alcohol treatment and purified water that (emblic weight is big Hole absorption 2 times of column volume), upper column flow rate is 1BV/h, then purified water, 10% ethyl alcohol, each 3BV of 80% ethanol elution with 1BV/h flow velocitys elute, and collect 80% ethanol eluate, and 60 DEG C of decompressions, which are protected from light, in falling film condenser is concentrated into 1.10 (40 DEG C), Concentrate is spray-dried (inlet air temperature:170 DEG C, it is atomized frequency:300Hz, leaving air temp:100~110 DEG C), it obtains emblic and carries Object dried cream powder is taken, density polyethylene bag is set low and is packaged into 500g/ bags, then puts shady and cool, dry, ventilation and preserves.The total tan of dried cream powder Matter content 75.3%, general flavone content 4.5%.
Embodiment 2
Emblic dry fruit 800kg, coarse crushing add 70% acetone to take 2 times in 50 DEG C of temperature extractions in refluxing extraction tank, every time 60min, every time 15 times of amounts (V/W), the filtration of 100 mesh filter cloth of extracting solution, in falling film concentration plants, 40 DEG C are concentrated under reduced pressure into filtrate Acetone, concentrate add purified water to be dissolved to 2 times of emblic weight amounts, and 200 mesh filter-cloth filterings, filtrate is added in through at 95% ethyl alcohol (emblic weight is 1 times of macroporous absorption column volume), upper column flow rate on the LS305 macroporous absorption columns that reason and purified water have balanced For 1.5BV/h, then eluted through 20% ethyl alcohol, each 3BV of 70% ethanol elution with 1BV/h flow velocitys, collect 70% ethanol eluate, It is protected from light in the 60 DEG C of decompressions of economic benefits and social benefits contracting device and is concentrated into 1.20 (50 DEG C), concentrate vacuum freeze drying (pre-freezing temperature:40 DEG C, pre-freeze Time:60min;Then it is stepped up temperature to distil, obtains emblic extract dry cream, crush, sieve with 100 mesh sieve, get dry extract Powder sets low density polyethylene bag and is packaged into 5kg/ bags, then puts shady and cool, dry, ventilation and preserve.Dried cream powder total tannin content 55.9%%, general flavone content 1.5%.
Embodiment 3
Emblic dry fruit 700kg, coarse crushing, add 50% methanol in extractor cold soaking extract 3 times, every time for 24 hours, 20 times every time It measures (V/W), extracting solution filtration, for filtrate in dual-effect concentrator, 50 DEG C are concentrated under reduced pressure into no methanol (alcohol meter measure condensate liquid meter Number is 0), concentrate adds purified water to be dissolved to 5 times of amounts of emblic weight, and centrifugation, centrifugate, which is added in, to be handled and purified through soda acid On the good HPD826 macroporous absorption columns of water balance (emblic weight is 0.5 times of macroporous absorption column volume), upper column flow rate is Then 0.5BV/h is eluted with 1BV/h flow velocitys through 20%, 50% each 3BV of ethanol elution, 50% ethanol eluate is collected, in reverse osmosis 1.20 (20 DEG C) are reduced in permeable membrane, 50 DEG C of vacuum decompression dryings of concentrate obtain emblic extract dry cream, crush, cross 200 mesh Sieve, get dry extract powder, puts Brown Glass Brown glass bottles and jars only inner packing into 5kg/ bottles, then puts shady and cool, dry, ventilation and preserve.Dried cream powder total tannin Content 70.3%, general flavone content 4.1%.
Embodiment 4
Emblic dry fruit 500kg, coarse crushing add purified water ultrasonic extraction 3 times, and each 60min, every time 50 times of amounts (V/W) carry Liquid is taken to centrifuge, centrifugate is concentrated into 3 times of emblic weight amounts in nano-filtration membrane equipment, be then added in through 95% alcohol treatment and On the JKSB-1 macroporous absorption columns that purified water has balanced (emblic weight is 1 times of macroporous absorption column volume), upper column flow rate is Then 1BV/h is eluted with 1BV/h flow velocitys through 10% ethyl alcohol, each 3BV of 40% ethanol elution, collects 40% ethanol eluate, Yu Na 1.10 (25 DEG C) are reduced in filter membrane, concentrate microwave drying obtains emblic extract dry cream, crushes, and crosses 80 mesh sieve, gets dry extract Powder puts rustless steel container inner packing into 10kg/ bottles, then puts shady and cool, dry, ventilation and preserve.Dried cream powder total tannin content 40.7%, general flavone content 0.9%.
Embodiment 5
Fresh fruit of fructus phyllanthi 1000kg, coarse crushing add in 50% EtOH Sonicate extraction equipment and extract 2 times, extraction time 60min, 40% ethanol consumption is 15 times of amount/time (V/W), and the filtration of 100 mesh filter cloth of extracting solution, in falling film concentration plants, 50 DEG C subtract filtrate Pressure is concentrated into no alcohol, and concentrate adds purified water to be dissolved to 3 times of amounts of emblic weight, tube centrifuge centrifugation, and centrifugate is added in (emblic weight is macroporous absorption column on the LX-68M macroporous absorption columns balanced through soda acid, 95% alcohol treatment and purified water 2 times of volume), upper column flow rate is 1BV/h, is then eluted, received with 1BV/h flow velocitys through 10% ethyl alcohol, each 3BV of 50% ethanol elution Collecting 50% ethanol eluate, 50 DEG C of decompressions, which are protected from light, in falling film condenser is concentrated into 1.15 (40 DEG C), concentrate spray drying (into Air temperature:170 DEG C, it is atomized frequency:300Hz, leaving air temp:100~110 DEG C), emblic extract dried cream powder is obtained, is set low close Degree Polythene Bag is packaged into 500g/ bags, then puts shady and cool, dry, ventilation and preserve.Dried cream powder total tannin content 65.3%, it is total yellow Ketone content 1.2%.
6 freckle removing and whitening activity rating of embodiment (melanin inhibits experiment)
The emblic extract whitening active that this experiment prepares embodiment 5 is evaluated.Operation is as follows:1. cell is trained It supports:The B16-F10 cells of selection tradition selection secondary culture, digest through 0.25% membrane proteolytic enzyme, with containing 8% fetal calf serum DMEM high sugar culture solution passages, are placed in 37 DEG C, 5%CO2It is cultivated in the incubator of saturated humidity environment.2d is changed the liquid once, Experiment is derived from same passage cell each time.2. given the test agent tests the inhibition of melanin in B16~F10 cells:Treat B16- When F10 cell growths are to 80%~90%, cell dissociation is adjusted into cell concentration into individual cells suspension with 0.25% film enzyme For 1.0 × 105CellsmL-1.Per hole 2mL, inoculation is planted in 6 well culture plates, and culture plate is placed in 37 DEG C, 5%CO2Incubator Middle culture is for 24 hours.Reject cell conditioned medium culture solution after for 24 hours, experiment are divided into blank group, vehicle control group, positive controls and emblic Sub- test sample group.Blank group:3mLDMEM culture solutions are added in per hole;Positive controls and emblic test sample group:Emblic is supplied Test product and kojic acid are diluted to 1,5,20 μ gmL with DMEM culture solutions-1, emblic test sample is diluted to 0.2 with DMEM culture solutions, 1、5μg·mL-1, 3mL is added in per hole;Vehicle control group:The DMEM culture solutions of 3mL DMSO containing respective volume are added in per hole.Each Parallel 3 multiple holes of concentration.Supernatant is abandoned after effect B16-F10 cells 48h, cell is cleaned 2 times with PBS, per hole 0.5mL concentration For 1molL-1NaOH dissolve intracellular melanin, treat that melanin is completely dissolved and absorption photometric value measured after 450nm at. Melanin relative amount is calculated by following equation.Tested group of mean OD value of melanin content/%=/blank group mean OD value × 100.3. result:With blank group ratio, positive control (kojic acid) is in 1-20 μ gmL-1The table of melanin in the interior cell to B16-F10 Up to significantly inhibiting, difference has statistical significance (P < 0.01);Emblic extract is in 0.2-5 μ gmL-1It is right The expression of melanin significantly inhibits in B16-F10 cells, and difference has statistical significance (P < 0.01).
7 skin irritation test of embodiment
The emblic extract toxicity that this experiment prepares embodiment 5 is evaluated:With reference to the 2007 Nian Ban Ministry of Public Health《Makeup Product hygienic practice》In skin irritation/corrosion test specification, evaluation emblic extract to rabbit local skin whether spinosity Swash property and its stimulus intensity.Method:Emblic extract powder end is configured to suspension, is then applied to rabbit intact skin On, once a day, 14d is continuously smeared, observe the symptoms performance daily.As a result:Emblic extract multiple skin irritation to rabbit Every animal integral mean value is 0.05 daily for the dermoreaction of experiment, judges emblic extract to family's rabbit skin according to criterion It is nonirritant.Conclusion:Emblic extract sample is to rabbit no skin irritation.

Claims (11)

  1. A kind of 1. preparation method of freckle removing and whitening emblic extract, which is characterized in that the preparation of the emblic extract Method includes the following steps:Emblic fruit, low temperature extraction, filtering, the concentration of filtrate low temperature, concentrate are dissolved in water, separation of solid and liquid, Purification with macroreticular resin in aqueous is clarified, is eluted through different concentration ethanol, collects the ethanol eluate of specific alcoholic degree, is concentrated, Dry, detection is qualified, and packaging obtains emblic extract.
  2. 2. the preparation method of a kind of freckle removing and whitening emblic extract according to claim 1, which is characterized in that low temperature carries Taking technique includes:1. extracting mode is emblic fruit, crushes or do not crush, low temperature extraction especially with cold soaking, temperature leaching, surpasses The combination of one or several kinds of methods of sound extracts;2. extraction solvent is acetone, the one or several kinds of methanol, ethyl alcohol, water are molten The arbitrary composition ratio of matchmaker, particularly 40%~70% aqueous acetone solution, 40%~70% ethanol water, 40%~70% first Alcohol solution;3. solvent dosage is 3~100 times/time of emblic weight, particularly the 5~30 of emblic weight times;4. it extracts Time is 0.5~24 h/ time;5. extraction time is 1~5 time, particularly 1~3 time.
  3. 3. the preparation method of a kind of freckle removing and whitening emblic extract according to claim 1, which is characterized in that low temperature is dense Contracting technique includes:1. thickening temperature is 30~70 DEG C, particularly 40~60 DEG C;2. condensing mode is the equipment of low temperature concentration It extracts liquid to concentrate, particularly falling film concentration, micro-filtration membrane concentration, ultrafiltration membrane concentration, NF membrane concentration, reverse osmosis membrane concentrate Equipment;3. striking point is be concentrated into organic solvent-free or volume about emblic weight 1~3 times.
  4. A kind of 4. preparation method of freckle removing and whitening emblic extract according to claim 1, which is characterized in that solid-liquid point Separating process includes:Concentrate adds purified water, and to 2~5 times of emblic weight, mixing is completely dissolved in the precipitation in concentrate In water, then carry out separation of solid and liquid operation, centrifuged using centrifugation apparatus, the filtering of plate-frame filtering, micro-filtration film device, filter-cloth filtering Mode, particularly centrifugation apparatus centrifuge, and collect the aqueous of no precipitation.
  5. A kind of 5. preparation method of freckle removing and whitening emblic extract according to claim 1, which is characterized in that purifying work Skill includes:1. macroporous absorbent resin type:Using the macroporous absorbent resin of big polarity or medium and small polarity, as HPD826, LS305, HPD100, LX-68M, JKSB-1 etc.;2. macroporous absorbent resin pre-treatment:Using high concentration ethanol or through alkali, acid, ethyl alcohol etc. Reason is clean;3. applied sample amount:Applied sample amount is 0.1~5 times of macroporous absorbent resin(w/v)The obtained clarification aqueous of emblic;④ Elution:Large pore resin absorption column after loading, purified different concentration ethanol elution, collects 10%~80% ethanol elution successively The ethanol eluate of liquid, particularly 10%~40%.
  6. 6. the preparation method of a kind of freckle removing and whitening emblic extract according to claim 1, which is characterized in that ethyl alcohol is washed De- liquid concentration technique includes:1. the ethanol eluate low temperature concentration of upper prop elution gained;2. thickening temperature:To prevent high temperature from breaking Bad extracting solution chemical composition, low temperature range are 10~70 DEG C, particularly 20~60 DEG C;3. condensing mode:It is dense using energy low temperature The equipment of contracting extracts liquid and concentrates, and particularly falling film concentration, micro-filtration membrane concentration, ultrafiltration membrane concentration, NF membrane concentrate, are reverse osmosis The equipment such as film concentration;4. striking point:It is concentrated into relative density 1.0~2.0, particularly 1.05~1.20.
  7. A kind of 7. preparation method of freckle removing and whitening emblic extract according to claim 1, which is characterized in that back tender Skill is using microwave drying, the combination progress for vacuum freeze drying, being dried under reduced pressure, one or several kinds of drying modes such as be spray-dried The drying of concentrate, especially with one or several kinds of modes such as vacuum freeze drying, spray drying, microwave drying combination into The drying of row concentrate.
  8. A kind of 8. preparation method of freckle removing and whitening emblic extract according to claim 1, which is characterized in that emblic The water that fruit and liquid are in direct contact is deionized water or purified water.
  9. A kind of 9. preparation method of freckle removing and whitening emblic extract according to claim 1, which is characterized in that emblic The final form of extract is powder or dry cream.
  10. 10. the preparation method of a kind of freckle removing and whitening emblic extract according to claim 1-9, which is characterized in that remaining Sweet seed extract total tannin content is more than 30%, and particularly 40~80%, general flavone content is less than 5%, especially less than 1%.
  11. 11. the preparation method of a kind of freckle removing and whitening emblic extract according to claim 1-10, which is characterized in that remaining Sweet seed extract has effects that freckle removing and whitening and without skin irritation, main active can be used as to be used in skin lightening, U.S. In the white or cosmetics of nti-freckle.
CN201810191017.8A 2018-03-08 2018-03-08 Preparation method of phyllanthus emblica extract for removing freckles and whitening skin Active CN108186456B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201810191017.8A CN108186456B (en) 2018-03-08 2018-03-08 Preparation method of phyllanthus emblica extract for removing freckles and whitening skin

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201810191017.8A CN108186456B (en) 2018-03-08 2018-03-08 Preparation method of phyllanthus emblica extract for removing freckles and whitening skin

Publications (2)

Publication Number Publication Date
CN108186456A true CN108186456A (en) 2018-06-22
CN108186456B CN108186456B (en) 2020-10-09

Family

ID=62595349

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201810191017.8A Active CN108186456B (en) 2018-03-08 2018-03-08 Preparation method of phyllanthus emblica extract for removing freckles and whitening skin

Country Status (1)

Country Link
CN (1) CN108186456B (en)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108935904A (en) * 2018-09-26 2018-12-07 广西壮族自治区农业科学院农产品加工研究所 A kind of processing method of persimmon piece preserved fruit
CN109867704A (en) * 2019-04-21 2019-06-11 北京中医药大学 A kind of method that ethyl alcohol temperature leaching method prepares Chebulagic acid
CN109876031A (en) * 2019-04-21 2019-06-14 北京中医药大学 A kind of enrichment method at phyllemblic tannin position
CN111772227A (en) * 2020-08-10 2020-10-16 四川中烟工业有限责任公司 Phyllanthus emblica targeted refined substance, preparation method and application thereof in cigarettes
CN113940430A (en) * 2021-11-22 2022-01-18 广东青云山药业有限公司 Preparation method of emblic leafflower fruit powder

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0982590B1 (en) * 1998-07-01 2003-11-19 Nitto Denko Corporation Labeled conjugate and detection method using the same
CN1582894A (en) * 2004-06-02 2005-02-23 云南省天然药物中心 Serial cosmetic compositions with Yuganzi as primary activating component
CN101204417A (en) * 2007-12-18 2008-06-25 中国林业科学研究院林产化学工业研究所 Method of extracting natural oxidationresistant active substanceoil from orange tree bark
CN102258437A (en) * 2010-05-28 2011-11-30 旦巴颜排 Hair nourishing liquid
CN102327314A (en) * 2011-07-06 2012-01-25 南京泽朗农业发展有限公司 Preparation method of phyllemblic tannin
CN102796070A (en) * 2012-08-29 2012-11-28 西南林业大学 Preparation method of oligomeric proanthocyanidins
CN105616218A (en) * 2014-10-27 2016-06-01 武汉元通堂生物科技有限公司 Preparation method of natural skin-whitening cosmetic product composition

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0982590B1 (en) * 1998-07-01 2003-11-19 Nitto Denko Corporation Labeled conjugate and detection method using the same
CN1582894A (en) * 2004-06-02 2005-02-23 云南省天然药物中心 Serial cosmetic compositions with Yuganzi as primary activating component
CN101204417A (en) * 2007-12-18 2008-06-25 中国林业科学研究院林产化学工业研究所 Method of extracting natural oxidationresistant active substanceoil from orange tree bark
CN102258437A (en) * 2010-05-28 2011-11-30 旦巴颜排 Hair nourishing liquid
CN102327314A (en) * 2011-07-06 2012-01-25 南京泽朗农业发展有限公司 Preparation method of phyllemblic tannin
CN102796070A (en) * 2012-08-29 2012-11-28 西南林业大学 Preparation method of oligomeric proanthocyanidins
CN105616218A (en) * 2014-10-27 2016-06-01 武汉元通堂生物科技有限公司 Preparation method of natural skin-whitening cosmetic product composition

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108935904A (en) * 2018-09-26 2018-12-07 广西壮族自治区农业科学院农产品加工研究所 A kind of processing method of persimmon piece preserved fruit
CN109867704A (en) * 2019-04-21 2019-06-11 北京中医药大学 A kind of method that ethyl alcohol temperature leaching method prepares Chebulagic acid
CN109876031A (en) * 2019-04-21 2019-06-14 北京中医药大学 A kind of enrichment method at phyllemblic tannin position
CN111772227A (en) * 2020-08-10 2020-10-16 四川中烟工业有限责任公司 Phyllanthus emblica targeted refined substance, preparation method and application thereof in cigarettes
CN113940430A (en) * 2021-11-22 2022-01-18 广东青云山药业有限公司 Preparation method of emblic leafflower fruit powder

Also Published As

Publication number Publication date
CN108186456B (en) 2020-10-09

Similar Documents

Publication Publication Date Title
CN108186456A (en) A kind of preparation method of freckle removing and whitening emblic extract
CN110574927B (en) Anti-saccharification composition and preparation method thereof
CN105998109B (en) Mango seed polyphenol extract and preparation method thereof
CN105030878A (en) Method for extracting multiple active ingredients of blueberry fruits
CN110201012B (en) Preparation method and application of purslane extract
CN111821233B (en) Plant whitening natural active compound composition and preparation method and application thereof
CN101301319A (en) Preparation of granada flower polyphenol and uses thereof
CN107501365A (en) A kind of method that raspberry glycosides and anthocyanin are extracted from raspberry
CN101463027A (en) Method for extracting and separating flavone and anthocyanidin from elder fruit
CN106726889A (en) The extracting method of Camellia nitidissima active ingredient and prepare the purposes of health products
CN104983915B (en) A kind of preparation method of black fruit fructus lycii natural composite antioxidant
CN106349074A (en) Method for extracting chlorogenic acid in Chinese wolfberry via microwave-assisted ultrasonic
CN101659793A (en) Method for extracting gynura bicolor purpurin
CN111374247B (en) Fracture setting raspberry concentrated juice and preparation method thereof
CN109381389A (en) A kind of persimmon leaf fermentation extracting solution and preparation method and application
CN106749452B (en) Method for preparing anthocyanin
CN106138130B (en) Mango seed flavone extract and preparation method thereof
CN112159451A (en) Gynostemma pentaphylla saponin extract and preparation method thereof
CN108578317B (en) Method for extracting active ingredients from bamboo leaves and skin care application of active ingredients
CN115400061B (en) Ginseng callus extract and preparation method and application thereof
KR101676292B1 (en) Cosmetic composition comprising an mixed extract of tangle, okra and yam and manufacturing method thereof
CN108497246A (en) A kind of plant weight losing function beverage and preparation method thereof
WO2021082889A1 (en) Environmentally-friendly method of preparing composition containing anti-inflammatory active ingredient and application thereof
CN103141829A (en) Preparation method for concentrated dandelion juice
CN110105185B (en) Skin care compound, preparation method and application thereof, and skin care product

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant
EE01 Entry into force of recordation of patent licensing contract

Application publication date: 20180622

Assignee: Yunnan Baiyao Group Co.,Ltd.

Assignor: YUNNAN INSTITUTE OF MATERIA MEDICA

Contract record no.: X2022530000005

Denomination of invention: A preparation method of spot removing and whitening Phyllanthus emblica extract

Granted publication date: 20201009

License type: Common License

Record date: 20220624

EE01 Entry into force of recordation of patent licensing contract