CN104473825B - Longan fruit stone polyphenol method for extraction and purification and its application in polyphenol skin-lightening cosmetic is prepared - Google Patents
Longan fruit stone polyphenol method for extraction and purification and its application in polyphenol skin-lightening cosmetic is prepared Download PDFInfo
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Abstract
The present invention discloses a kind of longan fruit stone polyphenol method for extraction and purification and its application in polyphenol skin-lightening cosmetic is prepared.Longan fruit stone powder is handled three times respectively with anhydrous propanone and 50~70% aqueous acetone solution, merges the filtrate of second and third time, polyphenol is obtained after reclaiming acetone；The polyphenol that macroporous absorbent resin obtains to extraction purifies, and is concentrated in vacuo to the dry polyphenol purified.The method recovery rate of the present invention is high; used easily-recovered organic solvent; water in extract solution does not have to heating evaporation; room temperature or low-temperature treatment are advantageous to protect product and save the energy; product dissolubility improves after purification; facilitate compound product, and a brand-new purposes is provided for longan fruit stone, develop the cosmetics of four kinds of great market prospects：Polyphenol whitening nourishing facial milk, polyphenol whitening nutritive water, polyphenol whitening nutritional breast, polyphenol whitening nourishing cream, also provide a kind of approach with bright prospects for the integrated application exploitation of longan fruit stone.
Description
Technical field：
The invention belongs to biomedicine field, and in particular to a kind of longan fruit stone polyphenol method for extraction and purification and its prepare
Application in polyphenol skin-lightening cosmetic.
Background technology：
Longan (Dimocarpus longan Lour.) is Sapindaceae (Sapindaceae) Euphoria (Dimocarpus
Lour.) evergreen fruit trees.There is plantation in many national such as China, Thailand, India and Vietnam as industrial crops.China point
The provinces and regions such as Fujian, Taiwan, Guangxi, Guangdong, Hainan, Sichuan, Guizhou, Yunnan are distributed in, have large area in Fujian, Guangdong, Guangxi
Plantation.Longan popular name longan, also known as imperial mesh, than mesh, lichee slave, intelligence development, sub- lichee, circle eye, river pellet, black horse pearl, swallow ovum, honey
Spleen, shark tear, wooden round, embroidery wood group etc., are the famous fruit of south China, its pulp is milky white or pale, and meat band is crisp, fresh and sweet.
Longan is as nourishing health-care food, existing more than 1,000 years history.Traditional Chinese medicine thinks that arillus longan can be used for treatment consumptive disease thin
Weak, insomnia, forgetful, palpitation with fear, palpitation, heart-spleen boosting, fill blood, calm the nerves.
China is the country of origin and producing country of longan, and cultivated area and yield account for the 70% and more than 50% of the world respectively,
It is maximum YEAST IN LONGAN PRODUCTION state.In the past 10 years, total output increases substantially, and is increased to 2006 years by 36.53 ten thousand tons in 1997
110.65 ten thousand tons, amplification is up to 202.90%, wherein 47.56 ten thousand tons of Guangdong in 2006,38.57 ten thousand tons of Guangxi, Fujian 21.28 ten thousand
Ton.Because concentration is compared in listing, storing condition is backward and storage and freshness-retaining technology is insufficient, and only part longan directly disappears as fruit
Take, substantial amounts of longan is used to process dried longan pulp, longan sweet can and longan cream etc., and remaining fruit stone is all straight as waste
Connect discarding.Longan fruit stone has the effect of hemostasis, analgesic therapy, qi-regulating, dampness elimination, controls traumatic bleeding, hernia, mange, wet sore and scrofula.Most
Nearly report stone extracts have anti-oxidant, hypoglycemic, antifatigue and suppression rectum cancer cell hyperplasia isoreactivity.Fixed dragon
Eye fruit stone composition is exactly mainly that polyphenol, Soong and Barlow are determined using HPLC-ESI-MS GC-MSs except nutritional ingredient
17 kinds of polyphenol, Wu Nini is determined using same method containing 13 kinds of polyphenol, Wang Zhiyuan such as corilagins in longan fruit stone
Therefrom get four kinds of compounds such as progallin A.Zheng G. etc. are drawn from the isolated gallic acid of longan fruit stone, curry
Capital, ellagic acid, progallin A, 1-O- galloyl-β-D- glucopyanosyls, Methy Brevifolin-carboxlate, short leaf Soviet Union
Wooden phenol and rhamnopyranosyl ellagic acid, and determine their Scavenging ability, the results showed that activity is very strong.
Document report plant polyphenol has various biological activity, such as anti-oxidant, antibacterial, antiviral, anti-inflammatory, anti-artery
Hardening, anti-mutagenesis, antitumor etc., and have inhibitory action to a variety of enzymes.Contain a variety of phenolic compounds in the fruit of plant, this
A little compounds can protected from oxidative damage, suppress yeast, fungi, virus and the growth of bacterium.For comprehensive exploitation profit
With longan fruit stone, study it more phenol extractions, purifying and polyphenol after purification suppression tyrosinase effect, and will purifying
Polyphenol compound in cosmetic product.
There is document report for the extraction conditions of longan fruit stone polyphenol.Such as optimal conditions of document report (Wang Zhi is remote)
It is：Acetone concentration 50% (v/v), solid-liquid ratio l：140 (g/mL), 50 DEG C of extraction temperature, extraction time 2h, ultrasonic 20min, extraction
Three times, longan seed polyphenol yield is 62.1mg/g (PB methods).The optimal conditions of document report (Wu Lanlan etc.) are：Extraction time
106min, volume fraction of ethanol 58%, 64 DEG C of Extracting temperature, solid-liquid ratio 1: 9, on this condition, polyphenol yield is
(42.690mg/g Forint phenol method).The method of document (Huang Ruqiang) is existed with the 80~95% of 3~10 times (volume fraction) ethanol
50~90 DEG C of 3~6h of refluxing extraction, ethyl acetate extraction extract solution, silicagel column on extract, are washed with petroleum ether-chloroform gradient
It is de-, it is concentrated in vacuo, the polyphenol powder of microwave drying.The method of document (Li Qingbiao etc.) is the phosphate buffer with pH9~11
60~80 DEG C of 10~40min of extraction, filtering concentrate filtrate, hydrochloric acid acidizing and precipitation, and vacuum drying precipitation obtains product.
The content of the invention：
First purpose of the present invention is to provide a kind of longan fruit stone polyphenol method for extraction and purification.
The longan fruit stone polyphenol method for extraction and purification of the present invention, it is characterised in that comprise the following steps：
(1), extract：It is first 1 according to mass volume ratio (g/mL) by longan fruit stone powder and anhydrous propanone:10~15 mixing
1~2h is stirred at room temperature, upper liquid is abandoned after standing, is then 1 according to longan fruit stone powder and extractant mass volume ratio:10~15
Second of aqueous acetone solution for adding 50~70%, is stirred at room temperature 4~6h, stands, pours out upper liquid and filter, according still further to longan
Fruit stone powder is 1 with extractant mass volume ratio:10~15 third times add 50~70% aqueous acetone solution, are stirred at room temperature 4
~6h, stand, pour out extract solution filtering, merge the filtrate of second and third time, polyphenol is obtained after reclaiming acetone；
(2), purify：Macroporous absorbent resin is 0.7 according to dry weight weight ratio with the longan fruit stone powder in step (1)：1,
Macroporous absorbent resin is pre-processed, then the polyphenol obtained by step (1) is diluted with water to after concentration is 4~6g/L
Post, eluted with the ethanol that volume fraction is 40~80%, be concentrated in vacuo to the dry polyphenol purified.
It is preferred that longan fruit stone powder, its preparation method are in step (1)：Longan fruit stone is dried naturally, crushed 20 mesh
Sieve obtains longan fruit core powder.
Recovery acetone described in step (1), preferably normal pressure rotary evaporation reclaim acetone.
Macroporous absorbent resin in step (2), preferably macroporous absorbent resin HPD-100 or macroporous absorbent resin NKA-
II。
Large pore resin absorption column ratio of height to diameter in step (2) is preferably 10.
Being pre-processed to macroporous absorbent resin in step (2), specific method is：Added in resin column and be higher than resin
Layer 10 centimetres volume fraction be 95% ethanol soak more than 4 hours, release immersion liquid, with volume fraction be 95% ethanol after
Continuous washing to cleaning solution is diluted with water untill not muddy and eluent uv scan must not detect absworption peak, then uses water
Washing to ethanol content is less than 1% (without obvious ethanol smell).
Upper prop in step (2), loading flow velocity preferably 1~2BV/h, loading volume is preferably 6~8BV；Described uses body
The ethanol that fraction is 40~80% is eluted, and elution flow rate is preferably 0.5~1.5BV/h, and elution volume is preferably 1.5~
2.5BV。
The present invention extracts the yield of polyphenol with Forint phenol method measure from longan fruit stone powder and passes through macroporous absorption tree
The polyphenol content of fat after purification, the polyphenol yield extracted by the method for the present invention reach more than 62mg/g dry fruit cores, purify
Polyphenol content afterwards is more than 60%.
Tyrosinase can effectively be suppressed by the polyphenol of the method extraction purification of the present invention, experiment confirms 2.0mg/mL
The longan fruit stone polyphenol of purifying is more than 51.5% to the inhibiting rate of tyrosinase, and the junket of cosmetics whitening additive ursin
The IC of propylhomoserin enzyme50Value is 5.3mmol/L (1.46mg/mL).Therefore, second object of the present invention is to provide longan fruit stone polyphenol
Application in polyphenol skin-lightening cosmetic is prepared.
Described polyphenol skin-lightening cosmetic, preferably polyphenol whitening nourishing facial milk, polyphenol whitening nutritive water, polyphenol whitening
Nutritional breast and polyphenol whitening nourishing cream.
It is preferred that dosage of the longan fruit stone polyphenol in polyphenol skin-lightening cosmetic is mass percent 0.01~10.0%.
By the method for the present invention from the polyphenol good water solubility after longan fruit stone extraction purification, this is carried to compound in cosmetics
Possibility is supplied.Longan fruit stone polyphenol, which has, preferably suppresses tyrosinase effect, very strong effect of scavenging radical and absorption
The effect of ultraviolet, while also there is crease-resistant, anti-inflammatory, antibacterial, moisture-keeping function as plant polyphenol, therefore available longan fruit stone is more
Phenol prepares the skin-lightening cosmetic of multiple efficacies.
The solution have the advantages that：Polyphenol recovery rate is high, used easily-recovered organic solvent, and the water in extract solution is not
With heating evaporation, room temperature or low-temperature treatment are advantageous to protect product and save the energy, and product dissolubility improves after purification, convenient multiple
A brand-new purposes is provided with product, and for longan fruit stone, develops the cosmetics of four kinds of great market prospects：Polyphenol
Whitening nourishing facial milk, polyphenol whitening nutritive water, polyphenol whitening nutritional breast, polyphenol whitening nourishing cream, also it is the comprehensive of longan fruit stone
Close application and development and provide a kind of approach with bright prospects.
Embodiment：
Following examples are to further explanation of the invention, rather than limitation of the present invention.
Embodiment 1：
(1), extract：The fruit stone that longan processing abandons is collected in longan fruit field, is dried naturally, be crushed 20 mesh sieves and obtain longan
Fruit stone powder.Longan fruit stone powder 100g is taken in 2000mL three-necked flasks, adds 1500mL anhydrous propanones, installation band sealing
Agitating device, remaining two mouthfuls stopper, and are stirred at room temperature 1h, stand 1h, and pouring out upper liquid as far as possible, (basic clarification, separately makees to locate
Reason), abandon upper liquid；Second of the addition acetone of 1500mL 60%, the closed stirring 6h of room temperature, static 1h, is poured out as far as possible afterwards
Layer liquid simultaneously filters；Third time adds the acetone of 1500mL 60%, room temperature closed stirring 4h, static 1h, filtering；Merge second and third time
Filtrate, normal pressure rotary evaporation recovery acetone obtain polyphenol, and it is 5g/L that gained polyphenol, which is diluted with water to polyphenol concentration, through Forint phenol method
It is 64.67mg/g dry fruit cores to determine the total recovery rate of polyphenol.The polyphenol aqueous solution is used to purify in next step.
(2), purify：70g macroporous absorbent resin HPD-100 are taken, (specification is 40 × 400mm of Φ) adds high in resin column
Soaked more than 4 hours in 10 centimetres of 95% ethanol of resin bed, release immersion liquid, continue to be washed till cleaning solution in test tube with 95% ethanol
In be diluted with water untill not muddy and eluent uv scan must not detect absworption peak, be washed with water to wash to ethanol and contain
Amount is less than 1% (without obvious ethanol smell).By HPD-100 large pore resin absorption columns on the polyphenol aqueous solution, loading flow velocity 1BV/h,
Loading volume 6BV, is eluted, elution flow rate 1BV/h, elution volume 1.5BV with the ethanol that volume fraction is 70%, and vacuum is dense
It is reduced to dry that purified polyphenol, polyphenol content are 62.37%.
The polyphenol of extraction purification suppresses tyrosinase evaluation of effect：Using 1.0mmo1/L L-DOPA as substrate.First will
1.0mL3mol/L L-DOPA (phosphate buffer solution for being dissolved in pH=6.8) is placed in cuvette, adds 0.85mL pH=
6.8 phosphate buffer solution, the constant temperature l0min in 30 DEG C of waters bath with thermostatic control, add 1.0mL purified polyphenol solution and (be dissolved in pH=
In 6.8 phosphate buffer solution) and 0.15mL 0.15g/L the tyrosinase aqueous solution, determine OD475.In this live body system,
The whole mass concentration of enzyme is 7.5mg/L.Formula can be defined as to the relative inhibition (I) of enzyme：
In formula：ODlRefer to containing substrate, tyrosinase, purified polyphenol live body system absorbance；OD2Refer to containing
Substrate, tyrosinase, but the absorbance of the live body system without purified polyphenol；OD3Refer to containing substrate, purified polyphenol, but
The absorbance of live body system without tyrosinase；OD4Refer to containing substrate, but the survey without tyrosinase, purified polyphenol
The absorbance of live body system.
Result is that the polyphenol of 2mg/mL extraction purifications is 53.97% to the inhibiting rate of tyrosinase.
Embodiment 2：
(1), extract：The fruit stone that longan processing abandons is collected in longan fruit field, is dried naturally, be crushed 20 mesh sieves and obtain longan
Fruit stone powder.Longan fruit stone powder 100g is taken in 2000mL three-necked flasks, adds 1200mL anhydrous propanones, installation band sealing
Agitating device, remaining two mouthfuls stopper, and are stirred at room temperature 2h, stand 1h, and pouring out upper liquid as far as possible, (basic clarification, separately makees to locate
Reason), abandon upper liquid；Second of the addition acetone of 1500mL 55%, the closed stirring 5h of room temperature, static 1h, is poured out as far as possible afterwards
Layer liquid simultaneously filters；Third time adds the acetone of 1000mL 55%, room temperature closed stirring 4h, static 1h, filtering；Merge second and third time
Filtrate, normal pressure rotary evaporation recovery acetone obtain polyphenol, and it is 4g/L that gained polyphenol, which is diluted with water to polyphenol concentration, through Forint phenol method
It is 63.58mg/g dry fruit cores to determine the total recovery rate of polyphenol.The polyphenol aqueous solution is used to purify in next step.
(2), purify：70g macroporous absorbent resin NKA-II are taken, (specification is 40 × 400mm of Φ) adds high in resin column
Soaked more than 4 hours in 10 centimetres of 95% ethanol of resin bed, release immersion liquid, continue to be washed till cleaning solution in test tube with 95% ethanol
In be diluted with water untill not muddy and eluent uv scan must not detect absworption peak, be washed with water to wash to ethanol and contain
Amount is less than 1% (without obvious ethanol smell).By NKA-II large pore resin absorption columns on the polyphenol aqueous solution, loading flow velocity 1.5BV/h,
Loading volume 8BV, is eluted, elution flow rate 0.6BV/h, elution volume 2BV with the ethanol that volume fraction is 80%, and vacuum is dense
It is reduced to dry that purified polyphenol, polyphenol content are 63.19%.
The polyphenol of extraction purification suppresses tyrosinase evaluation of effect：Method is the same as the method in embodiment 1.
Result is that the polyphenol of 2mg/mL extraction purifications is 55.23% to the inhibiting rate of tyrosinase.
Embodiment 3：
(1), extract：The fruit stone that longan processing abandons is collected in longan fruit field, is dried naturally, be crushed 20 mesh sieves and obtain longan
Fruit stone powder.Longan fruit stone powder 100g is taken in 2000mL three-necked flasks, adds 1000mL anhydrous propanones, installation band sealing
Agitating device, remaining two mouthfuls stopper, and are stirred at room temperature 1h, stand 1h, and pouring out upper liquid as far as possible, (basic clarification, separately makees to locate
Reason), abandon upper liquid；Second of the addition acetone of 1000mL 50%, the closed stirring 4h of room temperature, static 1h, is poured out as far as possible afterwards
Layer liquid simultaneously filters；Third time adds the acetone of 1000mL 50%, room temperature closed stirring 6h, static 1h, filtering；Merge second and third time
Filtrate, normal pressure rotary evaporation recovery acetone obtain polyphenol, and it is 6g/L that gained polyphenol, which is diluted with water to polyphenol concentration, through Forint phenol method
It is 62.23mg/g dry fruit cores to determine the total recovery rate of polyphenol.The polyphenol aqueous solution is used to purify in next step.
(2), purify：70g macroporous absorbent resin NKA-II are taken, (specification is 40 × 400mm of Φ) adds high in resin column
Soaked more than 4 hours in 10 centimetres of 95% ethanol of resin bed, release immersion liquid, continue to be washed till cleaning solution in test tube with 95% ethanol
In be diluted with water untill not muddy and eluent uv scan must not detect absworption peak, be washed with water to wash to ethanol and contain
Amount is less than 1% (without obvious ethanol smell).By NKA-II large pore resin absorption columns on the polyphenol aqueous solution, loading flow velocity 2BV/h, on
Sample volume 6BV, is eluted, elution flow rate 0.5BV/h, elution volume 2.5BV with the ethanol that volume fraction is 40%, and vacuum is dense
It is reduced to dry that purified polyphenol, polyphenol content are 60.73%.
The polyphenol of extraction purification suppresses tyrosinase evaluation of effect：Method is the same as the method in embodiment 1.
Result is that the polyphenol of 2mg/mL extraction purifications is 51.83% to the inhibiting rate of tyrosinase.
Embodiment 4：
(1), extract：The fruit stone that longan processing abandons is collected in longan fruit field, is dried naturally, be crushed 20 mesh sieves and obtain longan
Fruit stone powder.Longan fruit stone powder 100g is taken in 2000mL three-necked flasks, adds 1500mL anhydrous propanones, installation band sealing
Agitating device, remaining two mouthfuls stopper, and are stirred at room temperature 2h, stand 1h, and pouring out upper liquid as far as possible, (basic clarification, separately makees to locate
Reason), abandon upper liquid；Second of the addition acetone of 1500mL 70%, the closed stirring 4h of room temperature, static 1h, is poured out as far as possible afterwards
Layer liquid simultaneously filters；Third time adds the acetone of 1500mL 70%, room temperature closed stirring 4h, static 1h, filtering；Merge second and third time
Filtrate, normal pressure rotary evaporation recovery acetone obtain polyphenol, and it is 4g/L that gained polyphenol, which is diluted with water to polyphenol concentration, through Forint phenol method
It is 64.29mg/g dry fruit cores to determine the total recovery rate of polyphenol.The polyphenol aqueous solution is used to purify in next step.
(2), purify：70g macroporous absorbent resin HPD-100 are taken, (specification is 40 × 400mm of Φ) adds high in resin column
Soaked more than 4 hours in 10 centimetres of 95% ethanol of resin bed, release immersion liquid, continue to be washed till cleaning solution in test tube with 95% ethanol
In be diluted with water untill not muddy and eluent uv scan must not detect absworption peak, be washed with water to wash to ethanol and contain
Amount is less than 1% (without obvious ethanol smell).By HPD-100 large pore resin absorption columns on the polyphenol aqueous solution, loading flow velocity 1BV/h,
Loading volume 6BV, eluted with the ethanol that volume fraction is 50%, elution flow rate 1.5BV/h, elution volume 2.5BV, vacuum
Purified polyphenol is concentrated to dryness to obtain, polyphenol content is 61.24%.
The polyphenol of extraction purification suppresses tyrosinase evaluation of effect：Method is the same as the method in embodiment 1.
Result is that the polyphenol of 2mg/mL extraction purifications is 52.66% to the inhibiting rate of tyrosinase.
Embodiment 5：
1st, the preparation of longan fruit stone polyphenol whitening nourishing facial milk
The composition proportion of the longan fruit stone polyphenol whitening nourishing facial milk of table 1.
| Raw material | Dosage/% |
| Longan fruit stone polyphenol | 0.01~10.0 |
| Alkyl alcohol ethoxylates sulfate ammonium salt | 1.0~30.0 |
| Sodium lauroyl sarcosine | 1.0~20.0 |
| Hydroxyethyl ether cellulose | 0.1~5.0 |
| PEG7- cocounut oil acid glycerides | 0.1~10.0 |
| Glycerine | 0.1~20.0 |
| Essence | 0.01~4.0 |
| Preservative | 0.1~1.0 |
| Water | 77.6 |
Longan fruit stone polyphenol (in embodiment 1 obtained by extraction purification) 3.0%, alkyl alcohol ethoxylates sulfate ammonium salt
8%, sodium lauroyl sarcosine 8.0%, hydroxyethyl ether cellulose 1.0%, PEG7- cocounut oil acid glyceride 1.0%, glycerine 1.0%,
Essence 0.2%, preservative 0.2%, water 77.6%.
Specifically preparation method is：Hydroxyethyl ether cellulose mixes with water, stirring and dissolving, adds alkyl alcohol ethoxylates sulphur
Acid esters ammonium salt, sodium lauroyl sarcosine, PEG-7 cocounut oil acid glyceride, glycerine, are heated to 70 DEG C, stirring and dissolving, stirring is cooled to
When temperature is 45 DEG C, longan fruit stone polyphenol, essence, preservative are added, is stirred, discharging obtains longan fruit stone polyphenol whitening battalion
Support mildy wash.
2nd, longan fruit stone polyphenol whitening nutritive water
The composition proportion of the longan fruit stone polyphenol whitening nutritive water of table 2.
| Raw material | Dosage/% |
| Longan fruit stone polyphenol | 0.01~10.0 |
| Asiaticosid | 0.1~2.0 |
| Sodium Hyaluronate | 0.01~1.0 |
| Glucan | 0.05~2.0 |
| Glycerine | 0.1~20.0 |
| Water | 30~100 |
| Disodium ethylene diamine tetraacetate | 0.01~0.5 |
| Triethanolamine | 0.01~1.0 |
| Preservative | 0.1~0.6 |
| Cremophor RH40 | 0.01~2.0 |
| Essence | 0.01~1.0 |
Longan fruit stone polyphenol (in embodiment 2 obtained by extraction purification) 3.0%, asiaticosid 0.5%, Sodium Hyaluronate
0.1%, glucan 0.5%, glycerine 10.0%, disodium ethylene diamine tetraacetate 0.05%, triethanolamine 0.2%, preservative
0.2%, Cremophor RH40 2.0%, essence 0.2%, water to 100%.
Cremophor RH40, essence are mixed and are dissolved in water, then other various raw materials are added, stirring and dissolving, is discharged
To longan fruit stone polyphenol whitening nutritive water.
3rd, longan fruit stone polyphenol whitening nutritional breast
The composition proportion of the longan fruit stone polyphenol whitening nutritional breast of table 3.
| Raw material | Dosage/% |
| Longan fruit stone polyphenol | 0.01~10.0 |
| Asiaticosid | 0.1~2.0 |
| Carbomer | 0.2~1.0 |
| Propane diols | 0.05~2.0 |
| Disodium ethylene diamine tetraacetate | 0.01~0.5 |
| Water | 30~100 |
| PEG-21 tristearin alcohol ethers | 0.1~4.0 |
| PEG-2 tristearin alcohol ethers | 0.1~4.0 |
| Tristerin | 0.1~4.0 |
| Dimethyl silicone polymer | 0.1~10.0 |
| Isopropyl palmitate | 0.1~10.0 |
| Cetostearyl alcohol | 0.1~10.0 |
| Dibutyl hydroxy toluene | 0.01~0.5 |
| Triethanolamine | 0.2~1.0 |
| Preservative | 0.1~0.6 |
| Essence | 0.01~1.0 |
Longan fruit stone polyphenol (in embodiment 3 obtained by extraction purification) 3.0%, carbomer 0.4%, asiaticosid 0.5%, third
Glycol 4.0%, disodium ethylene diamine tetraacetate 0.1%, PEG-21 tristearin alcohol ether 2.0%, PEG-2 tristearin alcohol ether 1.5%, stearic acid
Glyceride 1.0%, dimethyl silicone polymer 3.0%, isopropyl palmitate 4.0%, cetostearyl alcohol 0.5%, dibutyl hydroxy
Toluene 0.1%, triethanolamine 0.4%, essence 0.1%, preservative 0.3%, add water to 100%.
Card ripple is scattered in glycerine, adds water, disodium ethylene diamine tetraacetate, PEG-21 tristearin alcohol ethers, high-speed stirred,
And 80 DEG C are heated to, obtain aqueous phase；By oil phase (PEG-2 tristearin alcohol ether, tristerin, dimethyl silicone polymer, palmitic acid
Isopropyl ester, cetostearyl alcohol, dibutyl hydroxy toluene) 80 DEG C are heated with stirring to, melt oil phase；Oil phase is added in aqueous phase,
Constant temperature high-speed stirred；Add triethanolamine homogeneous；Stirring is cooled to 45 DEG C or so, adds longan fruit stone polyphenol, asiaticosid, perfume (or spice)
Essence, preservative；Stir, discharging obtains longan fruit stone polyphenol whitening nutritional breast.
4th, longan fruit stone polyphenol whitening nourishing cream
The composition proportion of the longan fruit stone polyphenol whitening nourishing cream of table 4.
| Raw material | Dosage/% |
| Longan fruit stone polyphenol | 0.01~10.0 |
| Asiaticosid | 0.1~2.0 |
| Carbomer | 0.2~1.0 |
| Glycerine | 0.1~20.0 |
| Water | 30~100 |
| Disodium ethylene diamine tetraacetate | 0.01~0.5 |
| White Mineral Oil | 0.1~20.0 |
| Isobutyl palmitate | 0.1~10.0 |
| Cetostearyl alcohol | 0.1~10.0 |
| Polysorbate60 | 0.1~10.0 |
| Span60 | 0.1~10.0 |
| Beeswax | 0.1~10.0 |
| Dibutyl hydroxy toluene | 0.01~0.5 |
| Triethanolamine | 0.2~1.0 |
| Essence | 0.01~1.0 |
| Preservative | 0.1~0.6 |
Longan fruit stone polyphenol (in embodiment 4 obtained by extraction purification) 3.0%, carbomer 0.5%, glycerine 3.0%, centella
Glycosides 0.5%, disodium ethylene diamine tetraacetate 0.1%, White Mineral Oil 12.0%, isobutyl palmitate 7.0%, cetostearyl alcohol 2.0%,
Polysorbate60 3.0%, Span60 2.0%, beeswax 4.0%, dibutyl hydroxy toluene 0.1%, three second
Hydramine 0.5%, essence 0.1%, preservative 0.3%, add water to 100%.
Card ripple is scattered in glycerine, adds water, disodium ethylene diamine tetraacetate, high-speed stirred, and is heated to 80 DEG C, is obtained
To aqueous phase；By oil phase (White Mineral Oil, isobutyl palmitate, cetostearyl alcohol, polysorbate60, Span60,
Beeswax, dibutyl hydroxy toluene) 80 DEG C are heated with stirring to, melt oil phase；Oil phase is added in aqueous phase, constant temperature high-speed stirred；
Add triethanolamine homogeneous；Stirring is cooled to 45 DEG C or so, adds longan fruit stone polyphenol, asiaticosid, essence, preservative；Stir
Mix uniformly, discharging obtains longan fruit stone polyphenol whitening nourishing cream.
Claims (9)
1. a kind of longan fruit stone polyphenol method for extraction and purification, it is characterised in that comprise the following steps：
(1), extract：It is first 1 according to mass volume ratio by longan fruit stone powder and anhydrous propanone:10~15 mixed room temperatures stirring 1
~2h, upper liquid is abandoned after standing, be then 1 according to longan fruit stone powder and extractant mass volume ratio:10~15 second plus
Enter 50~70% aqueous acetone solution, 4~6h is stirred at room temperature, stand, pour out upper liquid and filter, according still further to longan fruit stone powder
It is 1 with extractant mass volume ratio:10~15 third times add 50~70% aqueous acetone solution, and 4~6h is stirred at room temperature, quiet
Put, pour out extract solution filtering, merge the filtrate of second and third time, polyphenol is obtained after reclaiming acetone；
(2), purify：Macroporous absorbent resin is 0.7 according to dry weight weight ratio with the longan fruit stone powder in step (1)：1, to big
Macroporous adsorbent resin is pre-processed, and the polyphenol obtained by step (1) then is diluted with water into concentration for upper prop after 4~6g/L,
Loading flow velocity is 1~2BV/h, and loading volume is 6~8BV, is eluted with the ethanol that volume fraction is 40~80%, vacuum is dense
It is reduced to the dry polyphenol purified.
2. longan fruit stone polyphenol method for extraction and purification according to claim 1, it is characterised in that longan fruit in step (1)
Core powder, its preparation method are：Longan fruit stone is dried naturally, 20 mesh sieves is crushed and obtains longan fruit core powder.
3. longan fruit stone polyphenol method for extraction and purification according to claim 1, it is characterised in that described in step (1)
Acetone is reclaimed, acetone is reclaimed for normal pressure rotary evaporation.
4. longan fruit stone polyphenol method for extraction and purification according to claim 1, it is characterised in that the macropore in step (2)
Polymeric adsorbent is macroporous absorbent resin HPD-100 or macroporous absorbent resin NKA-II.
5. longan fruit stone polyphenol method for extraction and purification according to claim 1, it is characterised in that the macropore in step (2)
Adsorption resin column ratio of height to diameter is 10.
6. longan fruit stone polyphenol method for extraction and purification according to claim 1, it is characterised in that described uses volume fraction
Eluted for 40~80% ethanol, elution flow rate is 0.5~1.5BV/h, and elution volume is 1.5~2.5BV.
7. application of the longan fruit stone polyphenol for the method extraction purification for passing through claim 1 in polyphenol skin-lightening cosmetic is prepared.
8. application of the longan fruit stone polyphenol according to claim 7 in polyphenol skin-lightening cosmetic is prepared, it is characterised in that
Described cosmetics are polyphenol whitening nourishing facial milk, polyphenol whitening nutritive water, polyphenol whitening nutritional breast and polyphenol whitening nutrition
Frost.
9. application of the longan fruit stone polyphenol according to claim 8 in polyphenol skin-lightening cosmetic is prepared, it is characterised in that
Dosage of the longan fruit stone polyphenol in polyphenol skin-lightening cosmetic is mass percent 0.01~10.0%.
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| CN105456176A (en) * | 2015-12-29 | 2016-04-06 | 广州市科能化妆品科研有限公司 | Emulsion cream and preparing method thereof |
| CN107019738A (en) * | 2017-02-28 | 2017-08-08 | 广西南岜仔科技有限公司 | A kind of hypoglycemic longan seed polyphenol extracting method |
| CN107050164A (en) * | 2017-02-28 | 2017-08-18 | 广西南岜仔科技有限公司 | A kind of antibacterial extract extracting method of longan seed |
| CN116731400B (en) * | 2023-04-04 | 2024-01-30 | 华南农业大学 | Longan seed polyphenol starch active membrane and preparation method and application thereof |
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| CN102920830A (en) * | 2012-11-28 | 2013-02-13 | 华南师范大学 | Method for effectively extracting polyphenol from Longan seed |
| CN102961486A (en) * | 2012-12-24 | 2013-03-13 | 厦门大学 | Extraction method of longan seed polyphenol |
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| CN102920830A (en) * | 2012-11-28 | 2013-02-13 | 华南师范大学 | Method for effectively extracting polyphenol from Longan seed |
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