CN106924117B - With the washing product composition of artemisia annua residue preparation remaining after extraction qinghaosu - Google Patents

With the washing product composition of artemisia annua residue preparation remaining after extraction qinghaosu Download PDF

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CN106924117B
CN106924117B CN201710236589.9A CN201710236589A CN106924117B CN 106924117 B CN106924117 B CN 106924117B CN 201710236589 A CN201710236589 A CN 201710236589A CN 106924117 B CN106924117 B CN 106924117B
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artemisia annua
qinghaosu
extraction
flavones
washing product
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CN106924117A (en
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林芳花
丁运华
吴松潮
方绳英
赖翎儿
林之雄
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Huizhou University
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    • 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
    • A61Q17/00Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
    • A61Q17/005Antimicrobial preparations
    • 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
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • A61Q19/08Anti-ageing preparations
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • A61Q19/10Washing or bathing preparations
    • 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

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  • Life Sciences & Earth Sciences (AREA)
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  • Cosmetics (AREA)
  • Medicines Containing Plant Substances (AREA)

Abstract

The present invention relates to technical field of plant extraction and daily technology of fine chemicals, and in particular to a kind of washing product composition containing plant extracts.It is a kind of using the washing product composition for extracting remaining artemisia annua residue preparation after qinghaosu, contain: utilizing the flavones for extracting the artemisia annua residue preparation after qinghaosu;The volatile oil that artemisia annua residue after successively extracting qinghaosu and flavones is extracted with organic solvent;And washing product auxiliary material.The present invention prepares washing product composition using the artemisia annua residue after having extracted qinghaosu, realizes the regeneration to the resource.The washing product composition uses extract qinghaosu after the flavones that extracts of remaining artemisia annua residue and volatile oil as effective component, there is significant anti-oxidant, removing free radical, whitening, fungistatic effect to user.

Description

With the washing product composition of artemisia annua residue preparation remaining after extraction qinghaosu
Technical field
The present invention relates to technical field of plant extraction and daily technology of fine chemicals, and in particular to one kind contains plant The washing product composition of object extract.
Background technique
Artemisia annua (Artemisia annua Linn) is called yellow wormwood artemisia, is the annual herb plant of composite family artemisia, extensively Distribution each province at home is Chinese tradition Chinese herbal medicine, had developed on the basis of qinghaosu a variety of derivative dihydroartemisinines, Artesunate, Artemether, arteether, have antimalarial, resist pregnant, anti-fibrosis, anti-schistosome, resisting toxoplasmosis, anti-arrhythmia and The effects of cytotoxicity.Qinghaosu is for the value of malaria control by human knowledge and receiving, world health group at present Knit the choice drug that the compound preparation of qinghaosu is classified as and prevents and treats malaria in the world.According to the statistical data of World Health Organization, certainly From 2000, about 2.4 hundred million population of Sub-Saharan Africa area benefits from qinghaosu conjoint therapy, and about 1,500,000 people are because of the therapy Avoid death caused by malaria.
The usage amount of artemisia annua is huge, and the artemisia annua residue after extracting qinghaosu is largely discarded, these artemisia annua residues How to be recycled, continue to play value, is the project for being worth further investigation.Chinese patent application 201210270400.5 disclose a kind of artemisia annua and artemisia annua industrial abstract residue as preparing caffeoyl guinic acid raw material Application, provide an outlet for the recycling of artemisia annua residue.
Summary of the invention
Based on this, technical problem to be solved by the invention is to provide remaining artemisia annuas after a kind of qinghaosu using extraction The washing product composition of residue preparation, the washing product composition are extracted using remaining artemisia annua residue after extracting qinghaosu Flavones and volatile oil as effective component, to user have it is significant it is anti-oxidant, remove free radical, whitening, fungistatic effect.
The technical solution of present invention solution above-mentioned technical problem are as follows:
It is a kind of using the washing product composition for extracting remaining artemisia annua residue preparation after qinghaosu, contain: using mentioning The flavones of artemisia annua residue preparation after taking qinghaosu;Successively extract the artemisia annua residue organic solvent after qinghaosu and flavones Extract obtained volatile oil;And washing product auxiliary material.
Preferably, the mass ratio of the flavones and volatile oil is 20 ~ 40:60 ~ 80.Inventor is the study found that single Huang Ketone or volatile oil are all unobvious to the elimination effect of hydroxy radical, but flavones and the mixed effect of volatile oil are than single component It is good, and when blending constituent ratio is in 60 ~ 80 volatile oil: when 20% ~ 40% flavones, effect is most obvious, and elimination efficiency peaks.
Preferably, the gross mass of the flavones and volatile oil accounts for the 1 ~ 1.5% of washing product composition weight.
Preferably, the extracting method of the flavones are as follows:
(1) by the artemisia annua residue after extraction qinghaosu, constant temperature dries to constant weight in 60 DEG C of baking ovens, puts powder in pulverizer into Broken, sieving is sealed spare;
(2) step (1) residue obtained powder is aided with ultrasonic wave extraction with ethanol solution, artemisia annua residue is obtained after filtering General flavone extracting solution;
(3) step (2) resulting material concentration removal ethyl alcohol, centrifugation take supernatant after removing impurity, obtain flavones crude extract;
(4) flavones crude extract obtained by step (3) is purified using macroporous adsorbent resin column chromatography method, obtains flavones.
It is further preferred that the solid-liquid ratio of step (2) residue powder and ethanol solution is the mL of 1g:10 ~ 40, ethanol solution Percent by volume be 30% ~ 60%, extraction time be 20 ~ 50min, Extracting temperature be 40 ~ 60 DEG C, ultrasonic power 300W.
Still more preferably, the solid-liquid ratio of step (2) residue powder and ethanol solution is 1g:40 mL, ethanol solution Percent by volume is 40%, extraction time 20min, and Extracting temperature is 60 DEG C, ultrasonic power 300W.It is measured through test, upper Under the conditions of stating, the recovery rate highest of general flavone can reach 7.85%.
Further, the extracting method of the volatile oil are as follows: use the chrysanthemum after the extraction qinghaosu after extraction general flavone Wormwood artemisia residue is obtained reflux and takes out immersion liquid, obtained volatile oil after volatilization concentration, purification purification with organic solvent reflux extraction.
Preferably, the extracting method of the volatile oil are as follows: use the artemisia annua after the extraction qinghaosu after extraction general flavone Residue is added n-hexane in the ratio of solid-liquid ratio 1g:10mL, is put into thermostatic mixer, connects reflux condensing tube, adjust revolving speed For 60r/s, temperature is 75 DEG C, refluxing extraction 3 hours, the immersion liquid collected by suction that flows back repeats to extract artemisia annua residue, reflux is taken out Volatilization concentration is carried out after immersion liquid mixing, and is dissolved with dehydrated alcohol, sealing is placed on -20 DEG C of refrigerator overnights, and next day suction filtration removes Precipitate is removed, ethanol extract is collected, vacuum distillation removes ethyl alcohol, obtains blackish green volatile oil.
The washing product composition is shower cream.It is also possible to skin cream, facial cleanser, face cream, toner, Essence etc. Product.Washing product composition auxiliary material used is that cosmetics lead routine techniques, therefore do not elaborate.
The invention has the following beneficial effects:
The present invention prepares washing product composition using the artemisia annua residue after having extracted qinghaosu, realizes to the money The regeneration in source.Flavones and volatilization of the washing product composition using artemisia annua residue extraction remaining after extraction qinghaosu Oil is used as effective component, has significant anti-oxidant, removing free radical, whitening, fungistatic effect to user.
Detailed description of the invention
Fig. 1 is with clearance rate line chart of the flavones to hydroxy radical for extracting the remaining artemisia annua extraction of qinghaosu.
Fig. 2 is with the peroxide value curve graph for extracting the flavones that the remaining artemisia annua of qinghaosu is extracted.
Fig. 3 is the inhibitory effect curve graph with the tyrosinase for extracting the flavones that the remaining artemisia annua of qinghaosu is extracted.
Fig. 4 is the fungistatic effect figure of present invention gained volatile oil.
Fig. 5 is the clearance rate curve graph of the shower cream for preparing to embodiment to hydroxy radical.
Fig. 6 is inhibiting rate curve graph of the shower cream to tyrosinase of embodiment preparation.
Specific embodiment
The present invention will be described in detail with reference to the accompanying drawings and examples.
Embodiment
It is a kind of using the shower cream for extracting remaining artemisia annua residue preparation after qinghaosu, after using qinghaosu is extracted The preparation of artemisia annua residue flavones, successively extract the artemisia annua residue after qinghaosu and general flavone and extract to obtain with organic solvent Volatile oil and washing product auxiliary material.
Wherein, the extracting method of flavones are as follows:
1) by the artemisia annua residue after extraction qinghaosu, constant temperature dries to constant weight in 60 DEG C of baking ovens, puts powder in pulverizer into It is broken, and 40 meshes are crossed, it is sealed spare.
2) the above-mentioned residue powder of accurate weighing is added the ethyl alcohol that volume parts are 40% by solid-liquid ratio 1g:40 mL, extracts 20min, 60 DEG C of water bath with thermostatic control, 300 W ultrasonic wave addeds repeat to extract twice, and extracting solution mixing twice, filtering obtain artemisia annua Residue general flavone extracting solution.
3) artemisia annua residue general flavone extracting solution is concentrated in 60 DEG C of constant temperature blender with magnetic force, 150r/min, until complete (referring to the volume fraction and volume that ethyl alcohol is added, or until can't smell alcohol smell) until full removing ethyl alcohol, at 3000r/min It is centrifuged 10min, takes supernatant in 50mL volumetric flask, precipitating plus appropriate distillation water washing dissolution are centrifuged, supernatant is Huang again Ketone crude extract.Through NaNO2-Al(NO3)3The measurement of-NaOH method, the recovery rate of flavones crude extract reach 7.85%.
4) flavones crude extract obtained by step 3) is purified using macroporous adsorbent resin column chromatography method, obtains flavones.
The antioxygenic property of obtained flavones purified is determined as follows:
Removing to hydroxy radical
Reaction system (Fe is established referring to the Fenton method reacted2++H2O2→Fe+OH-+ OH) model, OH is generated, But since OH has very high reactivity, the time-to-live is short, if salicylic acid is added in the reaction system, can effectively catch OH is caught, and generates color products, which has strong absorption at 510nm, removes if being added to have in this reaction system The measured object of OH function will compete OH with salicylic acid, to make color products production quantity reduce, using fixation response time A series of prepare liquid of concentration gradients is added in the reaction system of same volume in method, with prepare liquid blank group, surveys at 510nm Measure different light absorption values.
Several 10mL centrifuge tubes are taken, 0.3mL 9mmol/L FeSO is sequentially added4Solution, 0.3mL 9mmol/L salicylic acid- Ethanol solution, the sample liquid of various concentration mix, and 0.3mL8.8mmol/L H is added2O2Solution.Centrifuge tube is placed in 37 DEG C of perseverances 30min is reacted in warm water bath cabinet, flowing water is cooling, and each pipe is separately added into distilled water, makes system final volume 5mL, 3000r/min It is centrifuged 10min, supernatant is taken to measure light absorption value A at lower 510nm0、AxAnd Ax0, it is repeated 3 times measurement.It is to hydroxyl free The clearance rate of base calculates as follows:
Clearance rate=[1-(Ax-A x0)/A0]×100%
In clearance rate formula: A0For blank sample liquid light absorption value (not sample adding liquid);AxFor analyte sample fluid light absorption value;A x0For Background light absorption value (sample adding liquid).
Experimental record table
Clearance rate=[1-(Ax-Ax0)/A0]×100%
In clearance rate formula: A0For blank sample liquid light absorption value (not sample adding liquid);AxFor analyte sample fluid light absorption value;Ax0For Background light absorption value (sample adding liquid).
By the line chart of Fig. 1 it is found that artemisia annua residue general flavone purified has removing to hydroxyl radical free radical (OH) Ability, but overall elimination effect is lower than citric acid and ascorbic acid, when artemisia annua residue general flavone purified mass concentration is by 0. 2 g/L are increased to 1 g/L, and the elimination efficiency of hydroxyl radical free radical improves very fast;When mass concentration is greater than 1g/L, elimination efficiency Without significant change.
To the inoxidizability of grease
Under anhydrous acidic conditions, the peroxide in grease makes I-Quantitatively it is oxidized to I2, I2With I-It is soluble in conjunction with generation The I of water3-, utilize I3-Color be compared with standard iodine solution it is quantitative.Under 353 nm wavelength, I2Content (ρ) is 0~100 There is good linear relationship with absorbance (A) in mg/L, extractive of general flavone is general in the world to the inoxidizability use of grease Baking oven strengthen storage method: be added in liquid grease, be sufficiently stirred, in insulating box with the flavones refined solution of appropriate mass concentration Storage compares group so that any antioxidant is not added, and the peroxide value of grease is measured by sampling in different time.And Vitamin C is used respectively Acid and citric acid solution measure peroxide value, the oxidation resistance of more various antioxidants according to the above method.
The production of content of iodine standard curve
In a series of 10 mL colorimetric cylinders of drying, it is separately added into chloroform-glacial acetic acid solution of 4 mL, 0.12mL potassium iodide Then plus 3mL distilled water be saturated lye, a pipe added to mix a pipe, then divide be added iodine titer 0.0,0.1,0.2,0.4,0.6, 0.8,1.0 mL.Then plus distilled water is to scale, jumps a queue and shakes up, stands about 5-10 min and take supernatant to move into after being layered In the quartz colorimetric utensil of 1cm, reference is made with zero pipe, its absorbance is surveyed under 353 nm wavelength, is marked according to corresponding concentration Directrix curve.
Calibration curve equation: y=234x+0.6609, R2=0.9886, y I2Content.
Specific experiment step is
1. 24 mL are added in 100 mL triangular flasks by V (oil): the mixed liquor of V (flavones refined solution)=5: 1 proportion. It is reacted in 40 DEG C of baking ovens, 60 min of interval take sample to be tested 0.1mL in dry 15 mL colorimetric cylinders, and chloroform-ice vinegar is added 4 mL of acid solution, mixing stir evenly, and KI is added and is saturated 0.12 mL of lye, 30 s of jog sets 3 min of dark place.
2. then plus distilled water is to scale, jumps a queue, overturns, mix 2~3 times, stand about 5~10 min, clarified to water phase Afterwards, it takes supernatant in 1 cm quartz colorimetric utensil, reference is made with blank at 353 nm, read the absorbance A and meter of each pipe Iodine production quantity is calculated, peroxide value (POV/%) is calculated by formula.
POV/%=(I2Content (μ g)/sample size 0.086g)) × 100
As a result record sheet
Peroxide value curve graph is referring to fig. 2.As can be seen from Figure 2, add flavones after, peroxide value have it is different degrees of under Drop, illustrates that flavones has different degrees of inhibiting effect to the oxidation of grease.And the flavones of 1g/L is to the anti-oxidant of animal fat Property is significantly higher than citric acid and ascorbic acid.
To the inhibitory effect (i.e. whitening function) of tyrosinase vigor
Melanin (melanin) is mainly generated by the melanocyte (melanocyte) of human skin basal layer of epidermis, It can be reduced injury of the ultraviolet light to skin.Draw however, melanin will cause hyperpigmentation in the abnormal accumulation of basal layer Black spot, freckle, senile plaque etc. are played, people's lives quality is influenced.As that studies melanin biosynthesis deepens continuously, Researcher has found that tyrosinase is played an important role in melanin biosynthesis, it is that tyrosine and DOPA change to melanin The main reason for major rate-limiting enzyme in the process, its overexpression is hyperpigmentation due to amiodarone.Therefore, inhibit tyrosinase Activity can block the biosynthesis reaction chain of melanin, reduce the generation of melanin, realize the effect of whitening.This experiment is logical Cross the DOPA quinone (having characteristic absorption peak at 475 nm) that measurement tyrosinase (MT) catalysis L-3,4 dihydroxyphenylalanine (L-DOPA) generates Content, come evaluate artemisia annua residue flavones crude extract and other antioxidants to the inhibiting effect of tyrosinase.
Laboratory apparatus: ultraviolet specrophotometer
Experiment reagent
The mother liquor of 10.0 mg/mL: taking flavones refined solution, citric acid and the VC of 100.0 mg, fixed with distilled water respectively Hold into 10 mL volumetric flasks, is configured to the mother liquor of 10.0 mg/mL.Used time is diluted to 0.2 with phosphate buffer solution, 0.4, 0.6、0.8、1.0mg/mL。
0.2 mol/L phosphate buffer (PBS), pH6.8: taking 2.84g disodium hydrogen phosphate in small beaker, adds a small amount of Distilled water dissolution, with constant volume in 100mL volumetric flask, is made the disodium phosphate soln of 0.2moL/L.Similarly take 2.6g di(2-ethylhexyl)phosphate Hydrogen sodium is made into the sodium dihydrogen phosphate of 0.2moL/L.Take the disodium phosphate soln and 51mL0.2moL/L of 49mL0.2moL/L Sodium dihydrogen phosphate mixing, adjust pH6.8.
1.0 mg/mL L-3,4 dihydroxyphenylalanine solution: 10mg L-3,4 dihydroxyphenylalanine is weighed, is settled to 0.2 mol/L phosphate buffer In 10 mL volumetric flasks, it is configured to the L-3,4 dihydroxyphenylalanine solution of 1.0 mg/mL.
186 U/mL tyrosinases: weighing appropriate enzyme preparation, with 0.2 mol/L phosphate buffered saline at 186 U/ mL。
Experimental implementation table
In 10mL dry colorimetric cylinder, by various reagents are sequentially added in table, 4 in each time are measured at 475nm Group extinction Value Data, respectively A1、A2、A3、A4
Increase by 0.001 with A475 per minute as 1 enzyme activity unit, the speed of enzymatic reaction is increased with A475 per minute It is value added to indicate.It being measured since being uniformly mixed, measurement in every 30 seconds is primary, 7 min are measured, when A475 tends towards stability, number Value is exactly the A475 of the group.Enzyme activity and enzyme inhibition rate are calculated by following two formula.
Enzyme activity r=[(A3- A4)/(A1- A2)] × 100%
Enzyme inhibition rate R=(1-r) × 100%
Fig. 3 is the inhibitory effect curve graph of TYR enzyme, from the figure 3, it may be seen that artemisia annua flavones has tyrosinase activity Certain inhibitory effect, when its concentration is in 0.2 ~ 0.4mg/mL, with the increase of concentration, inhibitory effect is more obvious, and is greater than Citric acid and ascorbic acid, when concentration is greater than 0.4mg/mL, inhibitory effect constantly declines, but is consistently higher than citric acid.
The extracting method of volatile oil are as follows:
By above-mentioned steps 2) extract general flavone after artemisia annua residue powder by 1g:10mL solid-liquid ratio be added n-hexane, put Enter in thermostatic mixer, connect reflux condensing tube, adjusting revolving speed is 60r/s, and temperature is 75 DEG C, refluxing extraction 3 hours.It will reflux Immersion liquid collected by suction repeats to extract artemisia annua residue, and reflux carries out volatilization concentration after taking out immersion liquid mixing.N-hexane is evaporated completely to obtain Volatile oil crude product contain more impurity, such as grease, wax, chlorophyll are extracted are dissolved in volatile oil together, Purification need to be further refined, oily crude product is will volatilize and is dissolved with dehydrated alcohol, sealing is placed on -20 DEG C of refrigerator overnights, and next day takes out Precipitate is filtered out, ethanol extract is collected, vacuum distillation removes ethyl alcohol, obtains blackish green volatile oil (not removing chlorophyll).
The fungistatic effect of gained volatile oil is tested:
(1) the corresponding liquid and solid medium for pressing recipe configuration strain draw 5 mL/ branch with liquid-transfering gun and are packed into examination Pipe is put constant incubator into, 37 DEG C of bacterium, 28 DEG C of fungi, is cultivated in 121 DEG C of high-pressure steam sterilizing pans sterilizing 20min after cooling Two to three days sees whether complete sterilizing.
(2) it is inoculated with: a small amount of staphylococcus aureus, Escherichia coli, streptococcus is aseptically seeded to equipped with ox The test tube of meat extract peptone culture solution, Candida albicans are inoculated in potato culture medium, and Penicillium notatum is inoculated in czapek's medium.Every kind 2 test tubes of microbionation, slight oscillatory test tube shake up.It is placed in suitable constant incubator culture, is proliferated it sufficiently, it is standby With.
(3) clean filter paper is made the roundlet scraps of paper that diameter is 0.5cm with punch, after hot air sterilization, is dipped in difference In the volatile oil extracting liquid of concentration, fully absorb it, it is spare.
(4) well-grown bacteria suspension after 0.5 mL transfers is drawn with liquid-transfering gun in super-clean bench, it is flat injects corresponding bacterium Plate, coating are uniform.The filter paper that immersion treatment is crossed drains, and is attached on above-mentioned plate containing bacterium, and each plate pastes 3 identical Huangs The filter paper of flower wormwood artemisia volatile oil mass concentration.Using acetone as blank control, experiment 2 times is repeated.It is placed in incubator, bacterium 37 DEG C culture for 24 hours, 28 DEG C of culture 48h of fungi.It takes out and measures antibacterial circle diameter.Analyze fungistatic effect.
Referring to fig. 4, as shown in Figure 4, artemisia annua residue volatile oil is to 5 kinds selected by experiment for the fungistatic effect figure of volatile oil Bacterium has certain inhibitory effect.It is wherein best to the inhibitory effect of Penicillium notatum, and with the increase of concentration, effect is better;It is right The inhibitory effect variation of other 4 kinds of bacterium is unobvious.
The preparation of shower cream:
The addition range of flavones and its volatile oil that the extraction of artemisia annua residue is arranged is 0.5% ~ 2%, takes 1%, 1.5%, 2% 3 A anti-oxidant experiment of gradient.Wherein, the flavones and its volatile oil proportion that artemisia annua residue extracts are as follows:
Volatile oil oil+flavones quality of three gradients is as follows:
It is in proportion C12: C14=2:1 weighs 7.5 g fatty acid mixeds, is placed in small beaker, and 2.3 g potassium hydroxide are molten Solution is heated to 80 DEG C after when spare preparation mixes fatty acid mixed with a certain amount of deionized water at the aqueous solution of 50 %, 50 % potassium hydroxide solutions are added and carry out saponification.The effective component of above three gradient is added after sufficiently reacting, is added Distilled water mixes well rear spare to 50mL.Detection to its stability, inoxidizability and its active effect, is washed one's hair to determine The optimum formula and whitening effect of bath lotion are measured, and determine its optimum formula.
Stability Determination
The sealing of above-mentioned shower cream preservative film is placed in 0 DEG C and 50 DEG C of insulating boxs, observe its precipitating every three days and is divided Layer situation determines its stability according to the time that precipitating and delamination occur, is observed continuously 10 days.
Stability record sheet
The elimination effect of hydroxy radical
Record sheet (control group has returned to zero)
Each experimental group to the clearance rate curve graph of hydroxy radical referring to Fig. 5, as shown in Figure 5, single effective component flavones or Volatile oil is all unobvious to the elimination effect of hydroxy radical, but the effect of blending constituent is generally got well than single component.And when mixed Component ratio is closed in 60% ~ 80% volatile oil, 20% ~ 40% flavones, effect is most obvious, and elimination efficiency peaks.
Whitening effect
Experimental implementation table
In 10mL dry colorimetric cylinder, by various reagents are sequentially added in table, 4 in each time are measured at 475nm Group extinction Value Data, respectively A1, A2, A3, A4.
Increase by 0.001 with A475 per minute as 1 enzyme activity unit, the speed of enzymatic reaction is increased with A475 per minute It is value added to indicate.It being measured since being uniformly mixed, measurement in every 30 seconds is primary, 7 min are measured, when A475 tends towards stability, number Value is exactly the A475 of the group.Enzyme activity and enzyme inhibition rate are calculated by following two formula.
Enzyme activity r=[(A3-A4)/(A1-A2)] × 100%
Enzyme inhibition rate R=(1-r) × 100%
Record sheet (A4 control has been returned to zero)
Each experimental group to the inhibiting rate curve graph of tyrosinase referring to Fig. 6, as shown in fig. 6, single effective component flavones or Volatile oil is all unobvious to the inhibitory effect of tyrosinase, but the effect of blending constituent is obviously got well than single component.And when mixed Component ratio is closed at 40% ~ 60%, effect is most obvious, and elimination efficiency peaks.
A specific embodiment of the invention above described embodiment only expresses, the description thereof is more specific and detailed, but simultaneously It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection of the invention Range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.

Claims (5)

1. the washing product composition of remaining artemisia annua residue preparation after a kind of qinghaosu using extraction, which is characterized in that contain Have: utilizing the flavones of the artemisia annua residue preparation after extraction qinghaosu;Successively extract the artemisia annua residue after qinghaosu and flavones The volatile oil extracted with organic solvent;And washing product auxiliary material;
The mass ratio of the flavones and volatile oil is 20 ~ 40:60 ~ 80;
The gross mass of the flavones and volatile oil accounts for the 1% ~ 1.5% of washing product composition weight;
The extracting method of the flavones are as follows:
(1) by the artemisia annua residue after extraction qinghaosu, constant temperature dries to constant weight in 60 DEG C of baking ovens, puts into pulverizer and crushes, mistake Sieve, is sealed spare;
(2) step (1) residue obtained powder is aided with ultrasonic wave extraction with ethanol solution, it is always yellow that artemisia annua residue is obtained after filtering Ketone extracting solution;
(3) step (2) resulting material concentration removal ethyl alcohol, centrifugation take supernatant after removing impurity, obtain flavones crude extract;
(4) flavones crude extract obtained by step (3) is purified using macroporous adsorbent resin column chromatography method, obtains flavones;
The extracting method of the volatile oil are as follows: using the artemisia annua residue after the extraction qinghaosu after extraction general flavone, use is organic Solvent refluxing extraction method obtains reflux and takes out immersion liquid, obtains volatile oil after volatilization concentration, purification purification.
2. the washing product of remaining artemisia annua residue preparation combines after the qinghaosu according to claim 1 using extraction Object, it is characterised in that: the solid-liquid ratio of step (2) residue powder and ethanol solution is the mL of 1g:10 ~ 40, the volume hundred of ethanol solution Divide than being 30% ~ 60%, extraction time is 20 ~ 50min, and Extracting temperature is 40 ~ 60 DEG C, ultrasonic power 300W.
3. the washing product of remaining artemisia annua residue preparation combines after the qinghaosu according to claim 2 using extraction Object, it is characterised in that: the solid-liquid ratio of step (2) residue powder and ethanol solution is 1g:40 mL, the volume basis of ethanol solution Than being 40%, extraction time 20min, Extracting temperature is 60 DEG C, ultrasonic power 300W.
4. the washing product of remaining artemisia annua residue preparation combines after the qinghaosu according to claim 1 using extraction Object, which is characterized in that the extracting method of the volatile oil are as follows: residual using the artemisia annua after the extraction qinghaosu after extraction general flavone Slag is added n-hexane in the ratio of solid-liquid ratio 1g:10mL, is put into thermostatic mixer, connects reflux condensing tube, adjust revolving speed For 60r/s, temperature is 75 DEG C, refluxing extraction 3 hours, the immersion liquid collected by suction that flows back repeats to extract artemisia annua residue, reflux is taken out Volatilization concentration is carried out after immersion liquid mixing, and is dissolved with dehydrated alcohol, sealing is placed on -20 DEG C of refrigerator overnights, and next day suction filtration removes Precipitate is removed, ethanol extract is collected, vacuum distillation removes ethyl alcohol, obtains blackish green volatile oil.
5. the washing product of remaining artemisia annua residue preparation combines after the qinghaosu according to claim 1 using extraction Object, it is characterised in that: the washing product composition is shower cream.
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