CN108653133A - A kind of preparation method of the anti-oxidant gelling agent of Maize silk flavones - Google Patents

A kind of preparation method of the anti-oxidant gelling agent of Maize silk flavones Download PDF

Info

Publication number
CN108653133A
CN108653133A CN201810618264.1A CN201810618264A CN108653133A CN 108653133 A CN108653133 A CN 108653133A CN 201810618264 A CN201810618264 A CN 201810618264A CN 108653133 A CN108653133 A CN 108653133A
Authority
CN
China
Prior art keywords
flavones
maize silk
solution
gelling agent
oxidant
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.)
Pending
Application number
CN201810618264.1A
Other languages
Chinese (zh)
Inventor
周鸿立
田海苹
崔浩
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.)
Jilin Institute of Chemical Technology
Original Assignee
Jilin Institute of Chemical Technology
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 Jilin Institute of Chemical Technology filed Critical Jilin Institute of Chemical Technology
Priority to CN201810618264.1A priority Critical patent/CN108653133A/en
Publication of CN108653133A publication Critical patent/CN108653133A/en
Pending legal-status Critical Current

Links

Classifications

    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97—Cosmetics 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
    • A61K8/9783—Angiosperms [Magnoliophyta]
    • A61K8/9794—Liliopsida [monocotyledons]
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K31/00—Medicinal preparations containing organic active ingredients
    • A61K31/60—Salicylic acid; Derivatives thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18—Magnoliophyta (angiosperms)
    • A61K36/88—Liliopsida (monocotyledons)
    • A61K36/899—Poaceae or Gramineae (Grass family), e.g. bamboo, corn or sugar cane
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/04—Dispersions; Emulsions
    • A61K8/042—Gels
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/36—Carboxylic acids; Salts or anhydrides thereof
    • A61K8/368—Carboxylic acids; Salts or anhydrides thereof with carboxyl groups directly bound to carbon atoms of aromatic rings
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00—Medicinal preparations characterised by special physical form
    • A61K9/06—Ointments; Bases therefor; Other semi-solid forms, e.g. creams, sticks, gels
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P17/00—Drugs for dermatological disorders
    • A61P17/10—Anti-acne agents
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P17/00—Drugs for dermatological disorders
    • A61P17/18—Antioxidants, e.g. antiradicals
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00—Preparations for care of the skin
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00—Preparations for care of the skin
    • A61Q19/005—Preparations for sensitive skin
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00—Preparations for care of the skin
    • A61Q19/007—Preparations for dry skin
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00—Preparations for care of the skin
    • A61Q19/08—Anti-ageing preparations
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/30—Extraction of the material
    • A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/30—Extraction of the material
    • A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/50—Methods involving additional extraction steps
    • A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying

Abstract

The invention discloses the Maize silk flavones gelling agents with antioxidant activity, including following parts by weight of component：Acritamer 940, glycerine, propylene glycol, appropriate triethanolamine, main ingredient Maize silk flavones powder and salicylic acid.Maize silk flavones have effects that anti-oxidant, anti-inflammatory, whitening, restraining and sterilizing bacteria in the present invention；According to 2015 editions《Chinese Pharmacopoeia》With 2007 editions《China cosmetic hygienic practice》, comprehensive research and evaluation have been carried out to Maize silk flavones cosmetics crude drug quality, extraction process, moulding process, quality standard, release in vitro and transdermal, stability and flavones antioxidant activity；Preparation process of the present invention is simple, and property is stablized, quality controllable, and the nonirritant daily chemical products that are suitable for are develop and useedd.

Description

A kind of preparation method of the anti-oxidant gelling agent of Maize silk flavones
Technical field
The present invention relates to cosmetics, and in particular to a kind of preparation method of the anti-oxidant gelling agent of Maize silk flavones.
Background technology
Medicine adornment with active skull cap components is with the spies such as, good penetrability small to skin irritation, safety index height, efficient Point, is increasingly favored by consumers in general, so the medicine adornment with active skull cap components is incited somebody to action with larger market potential It is the mainstream of world's cosmetics industry development.
Maize silk flavones are one of active constituents important in corn stigma column cap, have antibacterial, anti-inflammatory, reducing blood lipid, removing The functions such as free radical, Maize silk flavones have the function of anti-oxidant, radioresistance, whitening, moisturizing etc. to skin；As people are to natural Cosmetics research deepens continuously, and the function of Maize silk flavones is also more and more recognized and applied by people；This patent is being studied It is middle that Maize silk flavones are applied in gelling agent, the anti-oxidant gelling agent cosmetics of Maize silk flavones have been made, there is anti-acne, resist The functional medicine adornment product of oxidation, the effect of the brilliant white colour of skin.Suitable for slight and moderate acne patient treatment, safety is used for a long time Effectively, the generation of skin problem is reduced, keeps skin health moist.
Salicylic local action is cutin dissolving, is used as keratolytic, can due to formulation concentrations are different pharmacology It acts on different；1%~3% has angling to facilitate and itching-relieving action；5%~10% has cutin dissolution, can also generate antimycotic work With (because removal cuticula inhibits fungi growth, this product can help penetrating for other antifungal drugs, and inhibit bacterial growth)；Water Poplar acid acts on hair follicle parietal cell, can help to remove the hair follicle for being blocked and clogging, and restores the normal of cell and falls off, most to blackhead Effectively, it can also change follicular wall abnormal the phenomenon that falling off, and prevent the generation of new lesion.
Body generates various free radicals in metabolic process, as hydroxy radical, ultra-oxygen anion free radical and aliphatic radical are free Base etc.；The major reason of skin aging is that free radical increases in skin, damage biological film, also results in some hydrolases from cell Middle release makes collagenous fibres in epidermis, elastic fibers be crosslinked, become fragile, be denaturalized and follow the string so that and keratoderma thickens, It is final to make pachylosis, relaxation, form wrinkle.Maize silk flavones can capture and neutralize free radical, to dispel free radical to people Body damages, can delay skin aging, keep skin elasticity and smooth, be eventually exhibited as oxidation resistant effect.
The present invention is to the anti-oxidant gelling agent cosmetics crude drug quality of Maize silk flavones, extraction process, moulding process, quality Standard, release in vitro and transdermal, stability and flavones antioxidant activity have carried out comprehensive research and evaluation.
The present invention using Maize silk flavones powder, salicylic acid, Carbomer-940, glycerine, propylene glycol, triethanolamine as raw material, On the basis of base-material, the production technology of the anti-oxidant gelling agent of Maize silk flavones is determined by orthogonal experiment, has oxidation resistant Effect, and with sterilization, anti-inflammatory, whitening effect, do not have about anti-oxidant gelling agent of Maize silk flavones and preparation method thereof Report, this patent have certain meaning to meeting the needs of Cosmetic Market.
Invention content
It is an object of the invention in place of overcome the deficiencies in the prior art, provide a kind of anti-oxidant gel of Maize silk flavones Agent；The product has functional medicine adornment product that is anti-oxidant, going acne effect；Suitable for thering is sensitive, dryness and neutral skin to ask Safe and effective, the generation of reduction skin problem, guarantor is used for a long time in the damaged skin of topic, and the treatment to mild acne patient It is moist to hold skin health.
Another object of the present invention is to provide a kind of preparation method of above-mentioned gelling agent.
The technical solution adopted by the present invention：
A kind of anti-oxidant gelling agent of Maize silk flavones, by forming Carbomer-940, glycerine, propylene glycol L, triethanolamine, main ingredient Salicylic acid, Maize silk flavones powder and deionized water are prepared；Wherein each component content is Carbomer-940 in percentage terms 1 ~ 5%, glycerine 10 ~ 40%, propylene glycol 10 ~ 40%, appropriate triethanolamine, main ingredient Maize silk flavones powder 3 ~ 6%, salicylic acid 1 ~ 4% With deionized water 40 ~ 60%.
A kind of preparation method of above-mentioned gelling agent：
(1) extraction of Maize silk flavones：Take 50 g of Corn Stigma in beaker；Add the ethanol solution (corn of 600 mL75% Palpus：Ethyl alcohol=1:6, V/ V), it is ultrasonically treated 30 min；By the corn stigma ethanol solution vacuum filtration after supersound process, storage Filtrate, residue and 75% ethyl alcohol with 1:5 volume ratio, 30 min of twice ultrasonic；Vacuum filtration, merging filtrate, residue again with 75% ethanol solution is with 1:4 volume ratio, 30 min of ultrasound, gained filtrate will merge in Rotary Evaporators 45 three times three times At DEG C, concentrated with the rotating speed of 40 rpm；Solution to be concentrated stops concentration after there is wall built-up phenomenon, and gained concentrate is transferred to In beaker, be placed in 45 DEG C of water-baths, after 2 ~ 3 days, be dried in vacuo up to extractive of general flavone, be stored in 4 DEG C of refrigerators with Anti-metamorphic.Precision weighs 2.5 g of Stigma Maydis total flavones powder, and 20mL purified water ultrasonic dissolutions, filtering, filtrate volume concentration is added To 1/5 volume, filtrate is decolourized with diatomite, is separately added into petroleum ether and chloroform carries out extraction overnight, to remove alkaloid and do The interference effect of lipid is disturbed, then upper gained filtrate is extracted with ethyl acetate, purer flavonoids solution is obtained, is dried to powder；
(2) preparation of the anti-oxidant gelling agent of Maize silk flavones：10 g of glycerine is weighed, it is abundant that 1 g carbomers are uniformly spread on surface After infiltration, add the appropriate purified waters of 10 ~ 15mL, stir evenly and stand overnight, it is made fully to be swollen, 1.35g triethanolamines are added dropwise at transparent Gel-type vehicle, it is spare；Precision weighs 2.5 g of Maize silk flavones powder after purification, and 20mL purified water ultrasonic dissolutions are added, and filters, It is spare to obtain corn stigma preparation solution；The another 1.5 g salicylic acids for taking 60 mesh to sieve, which are added in the mixed liquor of propylene glycol and ethyl alcohol, to be dissolved Salicylic acid preparation solution, by two kinds of liquids under 40 DEG C of water bath conditions（Corn stigma preparation solution and salicylic acid preparation solution）It is slowly added to It is stirring while adding in gel-type vehicle, triethanolamine tune pH to 6.0~7.0 is added dropwise, adds water to enough, stirs evenly to obtain the final product.Above-mentioned A kind of anti-oxidant gelling agent of Maize silk flavones and preparation method thereof, reasonable design, preparation process thereof is simple, and property is stablized, matter Amount is controllable, and the nonirritant daily chemical products that are suitable for are develop and useedd.
Specific implementation mode:
Below in conjunction with specific example, the present invention is further described.
Embodiment 1:Extraction, purifying and the assay of Maize silk flavones
The extraction purification of Maize silk flavones：Take 50 g of Corn Stigma in beaker；The ethanol solution for adding 600 mL75% is (beautiful Rice palpus：Ethyl alcohol=1:6, V/ V), it is ultrasonically treated 30 min in being cleaned by ultrasonic in instrument；Corn stigma ethyl alcohol after supersound process is molten Liquid be filtered by vacuum, store filtrate, residue and 75% ethyl alcohol with 1:5 volume ratio, 30 min of twice ultrasonic；Vacuum filtration merges Filtrate, residue again the ethanol solution with 75% with 1:4 volume ratio, 30 min of ultrasound, gained filtrate will be stored in burning three times three times In bottle.Gained extracting solution is placed in 45 DEG C of water-baths, after 2 ~ 3 days, is dried in vacuo up to extractive of general flavone, is stored in 4 DEG C With anti-metamorphic in refrigerator.Precision weighs 2.5 g of Stigma Maydis total flavones powder, and 20mL purified water ultrasonic dissolutions, filtering, filtrate is added Volume concentration to 1/5 volume, filtrate is decolourized with diatomite, is separately added into petroleum ether and chloroform carries out extraction overnight, to remove life The interference effect of alkaloids and interference lipid, then upper gained filtrate is extracted with ethyl acetate, purer flavonoids solution is obtained, it is dry At powder.
Flavones qualitative experiment：This experiment using HCl- Zn powder reaction and alchlor reaction to the flavones in corn stigma into Row identification, hydrochloric acid-zinc powder reaction：The ethanol solution for taking 1mL samples, add a little zinc powder (magnesium powder) shake, then be added dropwise it is a few drop it is dense Hydrochloric acid (heats) colour developing in 1~2 min when necessary；Alchlor reacts：The ethanol solution for taking 1 mL samples, adds 1% trichlorine Change aluminium methanol solution, colour generation；
Maize silk flavones assay：According to consulting literatures general flavone wavelength be 510 nm locate absorption value maximum.Flavones is taken to carry Liquid is taken, is taken and is settled to graduation mark with 60% ethyl alcohol in the colorimetric cylinder of 2 mL of extract to 10 mL and then dilutes 5 times.Take diluted it is molten 4 part of 1 mL of liquid is placed in the colorimetric cylinder of 10 mL, a copy of it with 60% ethyl alcohol constant volume, as reference solution.Remaining each part is each Add 5% sodium nitrite solution, 0.3 mL to shake up, place 6 min, 10% aluminum nitrate solution, 0.3 mL is added to shake up, places 6 min, add 1 mol sodium hydroxide solutions, 4 mL, then it is diluted to scale with 60% ethanol solution, after placing 15 min, respectively at 510 nm Measure its absorbance.Standard curve regression equation can obtain concentration data（Using rutin as reference）, results are averaged three times 0.01 mg/mL.It is 4 ~ 6mg/g that flavones content in sample is obtained after conversion.
Embodiment 2:The preparation of gelling agent
Gel-type vehicle factor and horizontal determination:According to trial test situation, determine that investigation factor is carbomer dosage (A), glycerine Dosage (B), propylene glycol dosage (C), each factor arrange 3 horizontal progress preferred, and experimental factor is shown in Table 1 with horizontal arrangement；
1 gel-type vehicle of table prepares single factor test level design table
Factor Carbomer A（g/g） Glycerine B (g/g) Propylene glycol C (mL/g)
1 1 5 5
2 1.5 10 10
3 2 15 15
(1) gel-type vehicle recipe determination:It is horizontal with determining 3 factor 3, according to L9（3^3）9 parts of samples are prepared in the design of orthogonal arrage Product are loaded in closed plastic casing respectively, in room temperature, 55 DEG C and -15 DEG C of 1 d of placement.Observe the color of sample, clarity, Stretchability, stability, viscosity etc., and using it as investigation standard carry out comprehensive score, the equal satisfactory value of indices be 10 points ( Full marks are 10 points), other between 0~10/, the results are shown in Table 2；
2 gel-type vehicle orthogonal test scheme of table and result
Tested number A B C Room temperature 55℃ -15℃ Total score
1 1 1 1 5 4 4 13.5
2 1 2 2 8.5 8 7 2.5
3 1 3 3 6 4 4 4
4 2 1 2 7 8 9 24
5 2 2 3 4 4 4 12
6 2 3 1 4 4 3 11
7 3 1 3 5 4 3.5 12.5
8 3 2 1 8 7 6 21
9 3 3 2 4 4 3.5 11.5
K1 50.5 49.5 45
K2 47 56.5 58.5
K3 15 12.2 12.5
R 1.8 3.4 7
As seen from the results in Table 2, factor C influences matrix prescription most notable, and factor B takes second place, factor A third (Rc> Rb > Ra), determine that optimum substrate condition is A by K average values3B3C2, i.e. 1 g of carbomer, 10 g of glycerine, 10 mL of propylene glycol；
(2) determination of penetration enhancer dosage:Since Maize silk flavones are major ingredient, different according to the concentration of menthol, design is more Group of formula
Formula one
Maize silk flavones 2.5g；Salicylic acid 1.5g；Carbomer 1g；Glycerine 10g；Propylene glycol 10mL；Ethyl alcohol 10mL；Menthol 0.75g；Triethanolamine 1.35g；Deionized water adds to 50g；
Formula two
Maize silk flavones 2.5g；Salicylic acid 1.5g；Carbomer 1g；Glycerine 10g；Propylene glycol 10mL；Ethyl alcohol 10mL；Menthol 1.0g；Triethanolamine 1.35g；Deionized water adds to 50g；
Formula three
Maize silk flavones 2.5g；Salicylic acid 1.5g；Carbomer 1g；Glycerine 10g；Propylene glycol 10mL；Ethyl alcohol 10mL；Menthol 1.25g；Triethanolamine 1.35g；Deionized water adds to 50 g.
The preparation of the anti-oxidant gelling agent of Maize silk flavones
Glycerine is weighed, carbomer is uniformly spread on after surface fully infiltrates, is added appropriate purified water, stir evenly and stand overnight, it is made to fill Divide swelling, dropwise addition triethanolamine spare at clear gel matrix.Precision weighs Maize silk flavones powder after purification, is added appropriate Purified water ultrasonic dissolution, filtering, obtains corn stigma preparation solution, spare；Propylene glycol and second is added in the another salicylic acid for taking 60 mesh to sieve It is dissolved in the mixed liquor of alcohol, obtains salicylic acid preparation solution；By two kinds of liquids under 40 DEG C of water bath conditions（Corn stigma preparation solution and water Poplar acid preparation solution）It is slowly added in gel-type vehicle, it is stirring while adding, it adjusts pH to 6.0~7.0, adds water to enough, stir evenly to obtain the final product Finished product.
Embodiment 3：The quality control of the anti-oxidant gelling agent primary raw material of Maize silk flavones
Salicylic physics and chemistry differentiates：FeCl3Development process：The weak solution for taking test sample adds ferric trichloride test solution 1 to drip, i.e., aobvious purple；
Assay：Determine that a length of 298 nm of salicylic acid maximum absorption wave, precision weigh the salicylic acid pair for setting 24 h in drier It according to 100 mg of product, sets in 100 mL volumetric flasks, after being dissolved with ethanol in proper amount plus purified water is to scale, shakes up.It is accurate respectively to draw 0.3,0.6,0.9,1.2,1.5,1.8,2.1,2.4,2.7 mL of above-mentioned solution, sets in 100mL volumetric flasks, adds purified water extremely successively Scale shakes up.Using purified water as blank, trap is measured at 298nm, carrying out linear regression to concentration C with trap A obtains water Poplar acid equation of linear regression：The .9999 of Y=0.2537C+0.024, r=0 (n=9), the results showed that salicylic acid is in 3-21 Within the scope of mg/L, trap A has good linear relationship with concentration C；
Flavones is identified and containing survey with [0016], [0017]；
Acid-base value inspection：Take three parts of detections respectively from Maize silk flavones three batches of lab scale samples of anti-oxidant gelling agent finished product, every part 1.0 g gels are about taken, sets and adds a small amount of distilled water in 10 mL beakers, be transferred to after stirring in 10 mL volumetric flasks, add distilled water suitable Amount, 20 min of ultrasound let cool rear constant volume, are filtered after centrifugation, take filtrate measurement pH value, the pH value of three batches of lab scale samples 6.75 ~ In 6.97 ranges, therefore tentative this product pH value is 6.8 ± 0.2；
Limit test of microbe：The anti-oxidant gelling agent finished product sample of three batches of Maize silk flavones respectively about 1.0 g is taken, is pressed《China's makeup Product hygienic practice》Method, which check, under 2007 editions limit test of microbe items is shown in Table 3, as a result meets regulation；
3 microorganism checking of table
Project Index
Protein type Plain edition Roasting-type
Total plate count, a/g ≤30000 ≤1000 ≤1000
Coliform, a/100g ≤90 ≤40 ≤40
Pathogenic bacteria, a/g ≤50
Pathogenic bacteria It must not detect
Viscosity inspection：In the measuring bottle for taking anti-oxidant 10.0 g of gelling agent to 50 mL of Maize silk flavones, it is dissolved in water, shakes up, add water To scale, ultrasound degassing is shone with the Ping Shi viscosmeters that capillary inner diameter is 1.0 mm《Chinese Pharmacopoeia》Two annex of version in 2015 The first methods of VIG measure in accordance with the law, and at 20 DEG C, the dynamic viscosity of actual measurement 3 batches, the results are shown in Table 4.According to 3 batches of inspection results and The dynamic viscosity of the general requirement of gelling agent, this product should be 10-100 mm2/s；
4 viscosity inspection of table
Lot number 20140510 20140511 20140512
Viscosity（mm2/s） 39.8 40.1 40.3
Centrefuge experiment：Anti-oxidant 1.0 g of gelling agent of Maize silk flavones is taken to be placed in centrifuge tube, revolution centrifuges for 4000 r/min 15 min.As a result, all samples are all uniform and smooth, lamination there are no.Prove prepared Maize silk flavones antioxygen Change gelling agent to stablize；
Stability test：According to test result, by the prescription of screening and the gelling agent of technique productions, under the conditions of commercially available back, Through strong illumination experiment, high temperature, high humidity and low-temperature test, character, content, the related substance nothing of gelling agent are substantially change, high The related substance of temperature experiment gelling agent is increased slightly, and prompts gelling agent that should avoid storing under the high temperature conditions.The above test result Illustrate, the prescription, production technology and package materials selection of this gelling agent are reasonable, and gelling agent is packed with listing requirement, product Stablize.
Transdermal experiment
The preparation of rat skin in vitro
The small white mouse of (20 ± 5) g or so is divided into 6 groups, every group 4.Small white mouse skin of abdomen is lost hair or feathers with depilatory agent, is put to death, stripping From skin of abdomen, remove subcutaneous fat, cleaned repeatedly with purified water, set refrigerated in physiological saline it is spare；
Transdermal experiment method
It is receiving chamber with pharmacopeia stripping rotor, supply chamber is connected with swingle, and diffusing opening is in supply chamber using rotation membrane diffusion device Bottom；The anti-oxidant gelling agent of the Maize silk flavones of 1 g is uniformly applied in spin basket, isolated mouse skin is fixed under spin basket End, stratum corneum side are in close contact to supply chamber and test liquid, permeate 3.15 cm2.The built-in 50 mL physiological saline of acceptance pool, includes 10 % PEG 400 and 2 d oil drippings acid, constant temperature stirs in (37 ± 1) DEG C, 100 rmin- 1.Interval 1,3,5, 7,9 h take 2 mL of acceptable solution (while supplementing dielectric fluid 2mL) that 6 mL absolute ethyl alcohols are added respectively, shake up, at 284 nm It measures and absorbs angle value；It is operated with method with blank control product, acquired results carry out blank correction, and with formula 1, calculate accumulative infiltration Measure Q and enhancing rate Er；It the results are shown in Table 5；
Q=[2 × ∑ Ci+V × Cn]/SEr=K/K0 formula 1
Q :Accumulative infiltration capacity；S:Infiltrating area；V:Acceptance pool volume；Er:Enhancing rate；K:Infiltration rate after anatonosis；K0: The infiltration rate of non-anatonosis；Ci:1st time to acceptance pool drug concentration when previous sample；Cn:When the sub-sampling in acceptance pool Drug concentration；
Influence (mg cm- 2, n=3) of the 5 salicylate compound gelling agent of Maize silk flavones containing various concentration of table to transdermal accumulation infiltration capacity
Flavones content 1 h 3 h 5h 7h 9h Er
0.0% 0.0501 0.7106 0.4302 1.0763 1.2795
1.5% 0.0254 1.1623 1.4877 1.9320 2.0832 1.63
2.0% 0.1198 1.1419 1.6136 2.3937 2.1593 1.69
2.5% 0.2278 1.4859 2.0789 2.7650 3.1123 2.43
Through statistical test, the anti-oxidant gelling agent of Maize silk flavones of the Maize silk flavones containing various concentration has stronger rush to ooze work With (P<0.05), wherein 2.5 % Maize silk flavones have pole conspicuousness (P to salicylic acid difference< 0.01 ).
Embodiment 5：The anti-oxidant gelling agent skin irritation/corrosion test of Maize silk flavones
Acute skin irritation test procedure
About 24 h cut experimental animal back backbone diamond wool before experiment, can not damage epidermis, unhairing range left and right each about 3 cm×3 cm.Take about 0.5 mL of tested material（g）It is coated directly on skin, then with two layers of gauze（2.5 cm×2.5 cm）With one Layer glassine paper or the like covering, then fixed with nonirritant adhesive plaster and bandage.Other side skin is as a contrast.Using envelope Experiment is closed, the application time is 4 h.Actual use that can be according to people for cosmetic product and product type extend or shorten The application time.To the cosmetic product with rear flushing, tested only with 2 h application.Warm water or nonirritant is used after the test Solvent cleaning remains tested material.Such as suspect that tested material may cause seriously stimulation or corrosiveness, Sectional Test can be taken, by three Application is on family's rabbit back hair removal section skin simultaneously or successively for the gauze piece of a coating tested material, 3 after coating Min, 60 min and 4h remove one piece of gauze, and corrosiveness occurs at any point in time in cutaneous application position, you can stop experiment. After removing tested material 1,24,48 and 72 h observation smear position dermoreaction, by table 6 progress dermoreaction scoring, with by The average value of examination animal integral carries out overall merit and is sentenced by table 3 according to each observing time top mean values of 24,48 and 72 h Determine skin irritatin intensity.The determination of observing time should be enough to observe the overall process of reversible or irreversible stimulation, generally not More than 14d；
Multiple skin irritation test step
Experimental animal back backbone both sides hair is cut before experiment, unhairing range is respectively 3 cm × 3 cm, application area 2.5cm ×2.5 cm.Take about 0.5 mL of tested material（g）It is applied on the skin of side, when tested material is prepared using nonirritant solvent, The other side applies solvent as a contrast, smears 1 time daily, continuously smears 14d.Since second day, cropping is answered before smearing every time, is used Water or nonirritant solvent cleaning remain tested material.Observation after one hour by table 6 as a result, score, check plot and trial zone are same Processing
Daily every animal average integral is calculated according to the following formula, skin irritatin intensity is judged with table 7
Daily every animal average integral=erythema and oedema integral/animal subject number/14
6 irritation of table scores
Dermoreaction Integral
Erythema and eschar are formed
Without erythema 0
Slight erythema（It is visible reluctantly） 1
Apparent erythema 2
Moderate ~ severe erythema 3
Severe erythema（Aubergine）It is formed to slight eschar 4
Oedema is formed
Without oedema 0
Slight oedema（It is visible reluctantly） 1
Mild edema（Cutaneous protuberance is clearly outlined） 2
Intermediate edema（Cutaneous protuberance about 1mm） 3
Severe edema（Cutaneous protuberance is more than 1mm, and range expands） 4
7 irritation grade of table
Integral mean value Intensity
0 ~ ＜ 0.5 It is nonirritant
0.5 ~ ＜ 2.0 Subexcite
2.0 ~ ＜ 6.0 Moderate stimulation
6.0~8.0 Strong stimulation type
Table 8 stimulates rank
Number of animals 1h 24h 48h 72h
Erythema Oedema Total score Erythema Oedema Total score Erythema Oedema Total score Erythema Oedema
1 0 0 0 0.5 0.1 0.6 0.5 0 0.5 0.3 0
2 0 0 0 0.5 0.1 0.6 0.5 0 0.5 0.3 0
3 0 0 0 0.5 0 0.5 0.5 0.1 0.6 0.2 0.1
4 0.5 0.5 1 0.5 0.1 0.6 0.5 0.1 0.6 0.1 0.1
Total mark mean value 0.11
Stimulus intensity classification is nonirritant
The anti-oxidant gelling agent of Maize silk flavones is the cosmetics of a gel type, uses Carbomer-940 for the matrix of gel, Using Maize silk flavones and salicylic acid as main component, there is anti-oxidant, anti-acne effect functional medicine adornment product.Suitable for light The treatment of degree and moderate acne patient is used for a long time safely and effectively, reduces the generation of skin problem, keeps skin health moist.
Embodiment 4：The anti-oxidant gelling agent antioxidation activity in vitro experiment of Maize silk flavones
Sample pre-treatments：Precision weighs the anti-oxidant gelling agent of Maize silk flavones of different quality, and methanol dissolves and is settled to difference Concentration, ultrasonic mixing, centrifugation take supernatant that sample liquid is made.
Total reduction force method：Take phosphate buffer solution（pH6.6 0.2 mol/L）2.5 mL are separately added into test tube The sample liquid of 0.3 mL various concentrations（0.07,0.14,0.21,0.28,0.35mg/mL）The potassium ferricyanide of 1ml is added after mixing, 50 DEG C of 20 min of water-bath are placed in, 10% trichloroacetic acid, 1 mL, mixing is added after cooling.2.5 mL supernatants are taken, are added 2.5 0.1% ferric trichloride of mL distilled water and 0.5 mL, react 5 min after in 700 nm survey absorbance.As a contrast with VC.
Remove DPPH free radical methods：
The sample liquid 2ml for taking 0.5mg/ml, 1.0mg/ml, 1.5mg/ml, 2.0mg/ml, 2.5mg/ml different quality concentration, adds Enter the DPPH solution (being prepared with absolute ethyl alcohol) of isometric a concentration of 0.1mmol/l, is protected from light at room temperature after mixing 30min.Absorbance A i is measured at 517nm, and using 4ml absolute ethyl alcohols and distilled water (the two is respectively 2ml) as blank tune Zero.Blank control group is that 2ml sample liquids add 2ml absolute ethyl alcohols, and the light absorption value at 517nm is Aj, and blank control is arranged Group purpose is to remove the light absorption value of flavones sample itself.Model control group is that 2mlDPPH solution adds 2ml absolute ethyl alcohols, Its light absorption value at 517nm is Ao.Parallel determination is averaged for 3 times, and clearance rate is calculated according to formula：Clearance rate（%）=[1- (Ai-Aj)/Ao] × 100%.
Remove ABTS free radical methods：
The ABTS of 7 mmol/L is mixed in equal volume with the K2S2O8 solution of 2.45 mmol/L, 12 h of room temperature avoid light place is obtained ABTS reserve liquids.It is diluted with absolute ethyl alcohol, makes its range of absorbency 2.000 ± 0.100, obtain ABTS+ detection liquid.Take 11 Colorimetric cylinder is divided into be measured group：3.00 m L ABTS+ detection liquid and 0.05mg/ml, 0.10mg/ml, 0.25mg/ml, 0.5mg/ The sample liquid of ml, 1mg/ml different quality concentration, control group：ABTS+ is replaced to detect liquid, blank group with 95% ethyl alcohol：95% second Alcohol replaces Maize silk flavones prepare liquid, after each group mixing, be stored at room temperature 6 min, return to zero with absolute ethyl alcohol, rapidly in wave 3 absorbances of parallel determination, are averaged at a length of 734 nm.According to following formula：Clearance rate=［ 1-（A-A to be measured Control）/ A blank ］ × 100% calculated.
As a result：As shown in Figure of description 1,2,3, the anti-oxidant gelling agent of Maize silk flavones has the energy of reduction iron ion Power can inhibit radical transfer electronics so that radical conversion is that relatively stable product terminates free radical serial reaction, and its Reducing power enhances with the increase of concentration.Light absorption value with the anti-oxidant gelling agent of Maize silk flavones under concentration is slightly below VC, The result shows that the anti-oxidant gelling agent of Maize silk flavones has stronger oxidation resistance, but it is less than VC.
Description of the drawings：For the anti-oxidant gelling agent of Fig. 1 Maize silk flavones to the reducing power of Fe3+, Fig. 2 Maize silk flavones are anti-oxidant Gelling agent is to the Scavenging activity of DPPH free radicals, removing energy of the anti-oxidant gelling agent of Fig. 3 Maize silk flavones to ABTS free radicals Power.

Claims (5)

1. a kind of anti-oxidant gelling agent of Maize silk flavones, by weight percentage, raw material group becomes：It is filtered out by orthogonal test Gel-type vehicle prescription is Carbomer-940 1 ~ 4%, glycerine 10 ~ 40%, propylene glycol 10 ~ 40%, appropriate triethanolamine；Main ingredient is after purification Maize silk flavones powder 3 ~ 6%, salicylic acid 1 ~ 4%；
The preparation method comprises the following steps：
（1）Extraction, decoloration and the purifying of Maize silk flavones：Take 50 g of Corn Stigma in beaker；Add the second of 600 mL75% Alcoholic solution (corn stigma：Ethyl alcohol=1:6, V/ V), it is ultrasonically treated 30 min；Corn stigma ethanol solution after supersound process is true Sky filter, store filtrate, residue and 75% ethyl alcohol with 1:5 volume ratio, 30 min of twice ultrasonic；Vacuum filtration merges filter Liquid, residue again the ethanol solution with 75% with 1:4 volume ratio, 30 min of ultrasound, gained filtrate will merge rotation three times three times In evaporimeter at 45 DEG C, concentrated with the rotating speed of 40 rpm；Solution to be concentrated stops after there is wall built-up phenomenon, and gained is dense Contracting liquid is transferred in evaporating dish, is placed in 45 DEG C of water-baths, after 2 ~ 3 days, is dried in vacuo up to extractive of general flavone, is stored in 4 With anti-metamorphic in DEG C refrigerator；Precision weighs 2.5 g of Stigma Maydis total flavones powder, and 20mL purified water ultrasonic dissolutions are added, and filters, filter Liquid product is concentrated into 1/5 volume, and filtrate is decolourized with diatomite, is separately added into petroleum ether and chloroform carries out extraction overnight, to remove The interference effect of alkaloid and interference lipid, then upper gained filtrate is extracted with ethyl acetate, purer flavonoids solution is obtained, is done It is dry to powder；
（2）The preparation of the anti-oxidant gelling agent of Maize silk flavones：10 g of glycerine is weighed, it is abundant that 1 g carbomers are uniformly spread on surface After infiltration, add the appropriate purified waters of 10 ~ 15mL, stir evenly and stand overnight, it is made fully to be swollen, 1.35g triethanolamines are added dropwise at transparent Gel-type vehicle, it is spare；Precision weighs Maize silk flavones powder after purification, and appropriate purified water ultrasonic dissolution is added, and filtering obtains corn Palpus preparation solution, it is spare；
The another 1.5 g salicylic acids for taking 60 mesh to sieve, which are added in the mixed liquor of propylene glycol and ethyl alcohol, dissolves to obtain salicylic acid preparation solution, By two kinds of liquids under 40 DEG C of water bath conditions（Corn stigma preparation solution and salicylic acid preparation solution）It is slowly added in gel-type vehicle, Bian Jia Side is stirred, and triethanolamine tune pH to 6.0~7.0 is added dropwise, adds water to enough, stirs evenly to obtain the final product.
2. the preparation of Maize silk flavones according to claim 1, decoloration and purifying：Corn stigma is selected using ultrasonic extracting method With 75% ethanol solution respectively according to corn stigma：Ethyl alcohol=1:6、1:5、1:4 solid-liquid ratio is ultrasonically treated in being cleaned by ultrasonic in instrument Each 30min three times；Will gained filtrate gained extracting solution be stored in flask respectively at 45 DEG C, in Rotary Evaporators three times It is concentrated with the rotating speed of 40rpm, solution to be concentrated stops concentration after there is wall built-up phenomenon, and gained concentrate is transferred to beaker In, it is placed in 45 DEG C of water-baths, after 2 ~ 3 days, is dried in vacuo up to extractive of general flavone, is stored in 4 DEG C of refrigerators to preapre for an unfavorable turn of events Matter；Precision weighs Stigma Maydis total flavones powder, and purified water ultrasonic dissolution, filtering is added, and filtrate volume is concentrated into 1/5 volume, filters Liquid is decolourized with diatomite, is separately added into petroleum ether and chloroform carries out extraction overnight, to remove alkaloid and interfere the interference of lipid Effect, then upper gained filtrate is extracted with ethyl acetate, purer flavonoids solution is obtained, it is dry to powder.
3. the anti-oxidant gelling agent of Maize silk flavones according to claim 1, it is characterised in that the every 100 g salicylic acid models of this product Enclose 1 ~ 4g, 3 ~ 6g of Maize silk flavones after purification；1 g carbomers about need 1.35 g of triethanolamine under normal circumstances, match skin care item When carbomer final mass score should control≤0.8%.
4. the anti-oxidant gelling agent of Maize silk flavones according to claim 1, it is characterised in that this product pH value is 6~8, this product Dynamic viscosity should be 10-100 mm2/s, skin irritatin rank total mark mean value 0.11.
5. the anti-oxidant gelling agent of Maize silk flavones according to claim 1, this preparation antioxidation biology activity is high, stretchability Good, preparation process is simple, and property is stablized, quality controllable, the characteristics of meeting gelling agent with require.
CN201810618264.1A 2018-06-15 2018-06-15 A kind of preparation method of the anti-oxidant gelling agent of Maize silk flavones Pending CN108653133A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201810618264.1A CN108653133A (en) 2018-06-15 2018-06-15 A kind of preparation method of the anti-oxidant gelling agent of Maize silk flavones

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201810618264.1A CN108653133A (en) 2018-06-15 2018-06-15 A kind of preparation method of the anti-oxidant gelling agent of Maize silk flavones

Publications (1)

Publication Number Publication Date
CN108653133A true CN108653133A (en) 2018-10-16

Family

ID=63776029

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201810618264.1A Pending CN108653133A (en) 2018-06-15 2018-06-15 A kind of preparation method of the anti-oxidant gelling agent of Maize silk flavones

Country Status (1)

Country Link
CN (1) CN108653133A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108785213A (en) * 2018-09-18 2018-11-13 安徽荷本化妆品有限公司 A kind of preparation method of face mask cream that treating acne
CN113425643A (en) * 2021-07-12 2021-09-24 青岛科技大学 Preparation method and application of disinfection and bacteriostasis compound lotion

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103948822A (en) * 2014-04-29 2014-07-30 陶建壮 Method for extracting flavone from corn stigma
CN105497050A (en) * 2015-12-08 2016-04-20 吉林化工学院 Preparation method of corn silk flavonoid, and product and application thereof
CN107693484A (en) * 2017-09-06 2018-02-16 遵义医学院附属医院 A kind of rifampin gel and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103948822A (en) * 2014-04-29 2014-07-30 陶建壮 Method for extracting flavone from corn stigma
CN105497050A (en) * 2015-12-08 2016-04-20 吉林化工学院 Preparation method of corn silk flavonoid, and product and application thereof
CN107693484A (en) * 2017-09-06 2018-02-16 遵义医学院附属医院 A kind of rifampin gel and preparation method thereof

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
梅全喜: "《现代中药药理与临床应用手册》", 31 October 2016, 中国中医药出版社 *
茅伟安: "《皮肤病用药速查手册》", 30 April 2014, 金盾出版社 *
薄南南等: ""玉米须中总黄酮的提取及含量测定"", 《首都师范大学学报（自然科学版）》 *
鄢海燕等: "《药剂学》", 31 January 2018, 江苏科学技术出版社 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108785213A (en) * 2018-09-18 2018-11-13 安徽荷本化妆品有限公司 A kind of preparation method of face mask cream that treating acne
CN113425643A (en) * 2021-07-12 2021-09-24 青岛科技大学 Preparation method and application of disinfection and bacteriostasis compound lotion

Similar Documents

Publication Publication Date Title
CN102018661B (en) External preparation for resisting funguses and preparation method of external preparation
CN104306358B (en) Antipruritic scar liniment of dispelling
Singh et al. Design, development and characterization of liposomal neem gel
CN108653133A (en) A kind of preparation method of the anti-oxidant gelling agent of Maize silk flavones
CN110787070A (en) Preparation method of hemp flower and leaf extract, preparation method of hemp flower and leaf extract and microcapsule, microcapsule and cosmetic
CN105477341A (en) Liquid adhesive bandage and preparation method thereof
CN102228479A (en) Medicine for treating oral diseases and preparation method thereof
CN101889973B (en) Itraconazole gel for dogs and preparation method thereof
CN104856978A (en) Chitosan spraying film agent and preparation method thereof
CN101584715B (en) Spray for preventing and treating skin damnification and resisting infection
CN101439083B (en) Detection method of Chinese medicine soft capsules for clearing wind heat and clearing nasal passage
CN1321655C (en) Gel of Chinese traditional medicine for treating cervicitis, colpitis and preparing method
CN106943341B (en) External preparation for improving transdermal absorption of usnic acid and application of external preparation in promoting healing of skin wound
CN108354951A (en) A kind of oxygen-enriched gelling agent, preparation method and application promoting Wound healing
CN104274494B (en) A kind of American cockroach external preparation and preparation method thereof
Paul et al. Preparation of nanogel incorporated with silver nanoparticles synthesized from pongamiapinnata. L root
CN101632725A (en) Liquid for relieving itching and eliminating swelling
RU2005485C1 (en) Method for production of medicine against animal skin diseases
CN107252431A (en) A kind of compound Aescinate A liposome hydrogel patch
CN101259162A (en) Plaster containing lamioplomis rotata extract and preparation thereof
CN105726516B (en) A kind of plastics and preparation method thereof promoting animal wound healing
RU2432958C1 (en) Method of obtaining medication from agrimonia eupator, possessing diuretic, antimicrobial, antioxidant action
Rahmadianti et al. Antioxidant Gel from Brown Algae (Ascophyllum nodosum) and Binahong Leaves for Diabetic Wound Healing
CN108606985A (en) It is a kind of to be used to treat compound salicylic acid lotion of Keratotic tinea hand or pedis and preparation method thereof
CN105998232B (en) Application of paliurus ramosissimus or extract thereof in preparation of medicine for treating acne

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
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20181016