CN111939109A - Preparation method of cosmetic raw material peony flower extract with high oxidation resistance - Google Patents
Preparation method of cosmetic raw material peony flower extract with high oxidation resistance Download PDFInfo
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- CN111939109A CN111939109A CN202010845991.9A CN202010845991A CN111939109A CN 111939109 A CN111939109 A CN 111939109A CN 202010845991 A CN202010845991 A CN 202010845991A CN 111939109 A CN111939109 A CN 111939109A
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- peony
- peony flower
- petals
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- 241000736199 Paeonia Species 0.000 title claims abstract description 135
- 235000006484 Paeonia officinalis Nutrition 0.000 title claims abstract description 135
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 239000002537 cosmetic Substances 0.000 title claims abstract description 15
- 239000002994 raw material Substances 0.000 title claims abstract description 15
- 230000003647 oxidation Effects 0.000 title claims abstract description 8
- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 47
- 239000003755 preservative agent Substances 0.000 claims abstract description 20
- 230000002335 preservative effect Effects 0.000 claims abstract description 18
- 230000008569 process Effects 0.000 claims abstract description 18
- 238000001914 filtration Methods 0.000 claims abstract description 15
- 239000000463 material Substances 0.000 claims abstract description 10
- 238000007710 freezing Methods 0.000 claims abstract description 9
- 230000008014 freezing Effects 0.000 claims abstract description 9
- 102000004190 Enzymes Human genes 0.000 claims abstract description 7
- 108090000790 Enzymes Proteins 0.000 claims abstract description 7
- 238000004519 manufacturing process Methods 0.000 claims abstract description 5
- 239000007788 liquid Substances 0.000 claims description 24
- 239000000243 solution Substances 0.000 claims description 24
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 21
- 239000011550 stock solution Substances 0.000 claims description 21
- 239000000047 product Substances 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000000706 filtrate Substances 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 15
- TXFPEBPIARQUIG-UHFFFAOYSA-N 4'-hydroxyacetophenone Chemical compound CC(=O)C1=CC=C(O)C=C1 TXFPEBPIARQUIG-UHFFFAOYSA-N 0.000 claims description 14
- 239000011344 liquid material Substances 0.000 claims description 14
- 239000012153 distilled water Substances 0.000 claims description 11
- 230000001954 sterilising effect Effects 0.000 claims description 11
- 238000004659 sterilization and disinfection Methods 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 10
- ACCCMOQWYVYDOT-UHFFFAOYSA-N hexane-1,1-diol Chemical compound CCCCCC(O)O ACCCMOQWYVYDOT-UHFFFAOYSA-N 0.000 claims description 8
- 238000003825 pressing Methods 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 6
- AYVIBZJMXLCJPV-UHFFFAOYSA-N 2-hydroxy-3-oxo-2-propyldecanoic acid Chemical compound C(CCCCCCC)(=O)C(C(=O)O)(CCC)O AYVIBZJMXLCJPV-UHFFFAOYSA-N 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- 230000000274 adsorptive effect Effects 0.000 claims description 5
- 238000007789 sealing Methods 0.000 claims description 5
- 238000003860 storage Methods 0.000 claims description 5
- LXAHHHIGZXPRKQ-UHFFFAOYSA-N 5-fluoro-2-methylpyridine Chemical compound CC1=CC=C(F)C=N1 LXAHHHIGZXPRKQ-UHFFFAOYSA-N 0.000 claims description 4
- 238000007599 discharging Methods 0.000 claims description 4
- 239000004927 clay Substances 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 230000017260 vegetative to reproductive phase transition of meristem Effects 0.000 claims description 3
- 239000006004 Quartz sand Substances 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 2
- 239000011347 resin Substances 0.000 claims description 2
- 229920005989 resin Polymers 0.000 claims description 2
- 230000002421 anti-septic effect Effects 0.000 claims 2
- 238000004042 decolorization Methods 0.000 claims 1
- 238000003306 harvesting Methods 0.000 claims 1
- 238000002156 mixing Methods 0.000 claims 1
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 abstract description 6
- 229910002092 carbon dioxide Inorganic materials 0.000 abstract description 6
- 238000004821 distillation Methods 0.000 abstract description 6
- 230000008901 benefit Effects 0.000 abstract description 3
- 239000001569 carbon dioxide Substances 0.000 abstract description 3
- 238000000855 fermentation Methods 0.000 abstract description 3
- 230000004151 fermentation Effects 0.000 abstract description 3
- 238000012545 processing Methods 0.000 abstract description 2
- 239000002912 waste gas Substances 0.000 abstract description 2
- 239000002351 wastewater Substances 0.000 abstract description 2
- 241000847925 Paeonia ostii Species 0.000 abstract 1
- 235000013305 food Nutrition 0.000 abstract 1
- 230000002779 inactivation Effects 0.000 abstract 1
- 238000000605 extraction Methods 0.000 description 9
- 230000002292 Radical scavenging effect Effects 0.000 description 7
- 230000007547 defect Effects 0.000 description 6
- 230000001105 regulatory effect Effects 0.000 description 6
- 230000002000 scavenging effect Effects 0.000 description 5
- 238000005054 agglomeration Methods 0.000 description 4
- 230000002776 aggregation Effects 0.000 description 4
- 238000001704 evaporation Methods 0.000 description 4
- 230000008020 evaporation Effects 0.000 description 4
- 239000012530 fluid Substances 0.000 description 4
- 238000001556 precipitation Methods 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 230000002225 anti-radical effect Effects 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000002390 rotary evaporation Methods 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- 239000013543 active substance Substances 0.000 description 2
- 150000001413 amino acids Chemical class 0.000 description 2
- 235000010208 anthocyanin Nutrition 0.000 description 2
- 229930002877 anthocyanin Natural products 0.000 description 2
- 239000004410 anthocyanin Substances 0.000 description 2
- 150000004636 anthocyanins Chemical class 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 230000009849 deactivation Effects 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- 230000000415 inactivating effect Effects 0.000 description 2
- 150000003254 radicals Chemical class 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 239000012085 test solution Substances 0.000 description 2
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 description 1
- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- MGJZITXUQXWAKY-UHFFFAOYSA-N diphenyl-(2,4,6-trinitrophenyl)iminoazanium Chemical compound [O-][N+](=O)C1=CC([N+](=O)[O-])=CC([N+]([O-])=O)=C1N=[N+](C=1C=CC=CC=1)C1=CC=CC=C1 MGJZITXUQXWAKY-UHFFFAOYSA-N 0.000 description 1
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 235000019198 oils Nutrition 0.000 description 1
- 150000008442 polyphenolic compounds Chemical class 0.000 description 1
- 235000013824 polyphenols Nutrition 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- -1 procyanidine Chemical class 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 235000015112 vegetable and seed oil Nutrition 0.000 description 1
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]
- A61K8/9789—Magnoliopsida [dicotyledons]
-
- 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
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
- A61K2800/805—Corresponding aspects not provided for by any of codes A61K2800/81 - A61K2800/95
Abstract
The invention relates to a preparation method of a cosmetic raw material peony flower extracting solution with high oxidation resistance, and belongs to the technical field of functional cosmetic raw material processing. The functional cosmetic raw material is a high oxidation resistance peony flower extract which is prepared by using a specific variety and a new food raw material of Paeonia ostii as a main material through freezing, enzyme inactivation, squeezing, filtering, decoloring and preservative treatment. The invention is characterized in that the peony flower extract with higher inoxidizability and product stability than the disclosed production processes such as distillation, supercritical carbon dioxide, subcritical and biological fermentation can be obtained; meanwhile, raw material resources are fully utilized, the process is simple and convenient, economic benefits are high, investment cost is low, residues are low, no waste water or waste gas is generated, and high-efficiency industrialization is realized.
Description
Technical Field
The invention belongs to the technical field of functional cosmetic raw material processing. In particular to a preparation method of a cosmetic raw material peony flower extract with high oxidation resistance.
Background
The peony essence is a name of 'king in flowers and very beautiful in the national color', peony is not only an ornamental plant with extremely high ornamental value, but also the flowers and root barks (cortex moutan) of the peony have extremely high medicinal value, and with the research and development of peony seed oil products, the peony industry is rapidly developed, the peony planting is also increased in a large area, and the number of the peony is also greatly increased. In order to prevent the resource from being wasted after the peony florescence, a plurality of experts can obtain effective utilization, and whether the peony petals have greater use value is researched. The result shows that the peony water squeezed from the peony petals has great use value.
Several methods for preparing peony fresh flower water are disclosed, and some of the methods are summarized as follows:
firstly, supercritical CO is adopted2Fluid extraction method
(1) Selecting fresh peony petals and selecting impurities;
(2) putting the peony fresh petals in the step (1) into an extraction tank, and using CO2Repeatedly flushing equipment to discharge air, when it is operated, firstly opening valve and cylinder valve to make air intake, then starting high-pressure valve to raise pressure, when the pressure is raised to preset pressure, regulating pressure-reducing valve to regulate separation pressure in the separator, then opening air-releasing valve, receiving rotor flowmeter to measure flow rate, regulating all valves to make extraction pressure, separation pressure and CO pass through in the course of extraction process2The flow is stabilized at the required operation condition, the valve is semi-closed, the valve is opened to carry out the full circulation flow operation, and the extraction liquid is extracted from the oil drain valve in the extraction process.
The equipment method has the defects of large equipment investment and complicated operation.
Secondly, adopting a rotary evaporation method
(1) Firstly, squeezing petals to obtain a squeezed liquid; roughly filtering the squeezed solution, and taking 1L of filtered peony flower stock solution;
(2) placing the peony flower stock solution in a rotary evaporator for rotary dry distillation to form steam, and condensing to obtain condensate, wherein the preparation process comprises the following steps:
the vacuum hose is connected with a vacuum pump, and then distilled water is injected into the heating tank. Adjusting the angle of the main machine to be inclined at will within 0-45 ℃, switching on the condensed water, switching on the power supply and connecting the main machine with an upper evaporation bottle (without releasing hands), and switching on a vacuum pump to achieve a certain vacuum degree to release hands. Adjusting the height of the host: the pressing rod at the bottom of the heating tank is pressed down, and the radian is adjusted left and right to enable the pressing rod to be in a proper position and manually separated from the pressing rod, so that the required height can be achieved. The speed regulating switch is turned on, the green light is turned on, the temperature regulating button is turned on, the heating groove starts to automatically heat, the instrument starts to operate, and the solvent can be evaporated to the receiving bottle when the temperature and the vacuum degree reach the required range. And after the evaporation is finished, firstly closing the speed regulating switch and the temperature regulating switch, pressing the pressing rod to enable the main machine to ascend, then closing the vacuum pump, opening the emptying valve above the condenser to enable the emptying valve to be communicated with the atmosphere, taking off the evaporation bottle, and finishing the evaporation process to obtain the peony flower water.
The equipment method has the disadvantages of complex process and higher requirement on operation conditions.
Thirdly, adopting a distillation method
(1) Collecting 1 kg of peony fresh flower petals;
(2) directly placing the petal into stainless steel pot with heating function, adding distilled water, boiling, condensing steam via condensing tube above the stainless steel pot to obtain distillate, and placing into sterilized container.
The equipment method has the defects of large energy consumption and low product grade of the process method.
In conclusion, the disclosed methods for preparing the peony flower extract have some defects more or less, and all of them have a common defect that the prepared peony flower extract has low antioxidant activity, short storage time and is not suitable for long-distance transportation and storage. At present, a new preparation method of a peony flower extract needs to be invented to make up for the defects of the existing preparation method.
Disclosure of Invention
The invention aims to provide a novel preparation method of a cosmetic raw material peony flower extracting solution, which can obtain the peony flower extracting solution with higher inoxidizability and product stability than the disclosed production processes such as distillation, supercritical carbon dioxide, subcritical and biological fermentation.
The preparation method is realized by the following technical scheme.
A preparation method of a cosmetic raw material peony flower extract with high oxidation resistance comprises the following preparation steps:
(1) collecting the red-phoenix peony petals at the initial stage of the flowering phase;
(2) freezing and storing the petals;
(3) carrying out high-temperature enzyme deactivation on the fresh peony petals by utilizing the frozen petals and microwave combined ultrasonic equipment; simultaneously, the function of physical sterilization is achieved;
(4) squeezing the material obtained in the step (3) in a spiral squeezing mode to obtain peony petal squeezing liquid;
(5) standing the peony petal squeezed liquid, and taking the upper layer liquid to obtain a peony petal liquid material;
(6) adding the peony petal liquid material prepared in the step (5) into an adsorptive substance, and performing high-temperature sterilization and decoloration treatment;
(7) performing two-stage filtration on the peony petal liquid material prepared in the step (6);
(8) and (3) adding the preservative system optimized for the process of the invention into the filtered solution of the peony flowers obtained after filtering in the step (7), and stirring to finally obtain the extract of the peony flowers.
The preparation method of the peony flower extracting solution is characterized by comprising the following steps:
1. the peony flower extracting solution prepared by the method has stronger anti-free radical capability. Compared with the prior preparation methods such as distillation, supercritical carbon dioxide, subcritical and biological fermentation, the peony flower extract obtained by the method has higher inoxidizability and product stability.
2. The preparation method of the peony flower stock solution can utilize peony petal raw materials to the maximum extent, has the advantages of high extraction rate, simple process, high economic benefit, low investment cost, low residue and no waste water and gas, belongs to an energy-saving and environment-friendly green preparation process, and can maintain the anti-free radical activity of the extracting solution.
3. Compared with the peony flower liquid produced by the existing preparation process, the peony flower extracting solution prepared by the method has very high corrosion resistance and longer quality guarantee period. The peony flower liquid produced by the existing preparation process is not easy to store at normal temperature, and is easy to deteriorate and rot in a short time, so that the application in the field of cosmetics is difficult, and great economic loss is caused. The peony flower extracting solution prepared by the invention overcomes the defect that the stock solution is easy to deteriorate, has long preservation time, does not deteriorate in the transportation process or before the cosmetics are prepared, greatly reduces the cost of transportation equipment, improves the product quality of the cosmetics and saves the production cost.
Detailed Description
The invention relates to a preparation method of a cosmetic raw material peony flower extract with high oxidation resistance, which comprises the following specific preparation steps:
(1) collecting the red-phoenix peony petals at the initial stage of the flowering phase, wherein the collecting time is 4-5 months, preferably 4 months 10-30, 6-10 am is selected, and the collected red-phoenix peony petals are petals which are opened for 1-10 days, preferably 1-3 days;
(2) freezing and storing the petals; the freezing temperature is-5 to-18 ℃, and the freezing temperature is preferably-10 ℃;
(3) heating the frozen petals to inactivate enzymes of the fresh peony petals by using microwave combined ultrasonic equipment; simultaneously, the function of physical sterilization is achieved; the ultrasonic frequency is 10-100 kHz, preferably 20-50kHz, and most preferably 30 kHz; the microwave condition is that the temperature of the materials is heated to 40-80 ℃, and the optimal temperature is 58-60 ℃; the time from feeding to discharging is controlled to be 5 min;
(4) squeezing the material obtained in the step (3) in a spiral squeezing mode, wherein the diameter of a spiral is phi 300mm, and obtaining peony petal squeezing liquid;
(5) standing the peony petal squeezed liquid for 5-24h, and taking the upper layer liquid to obtain a peony petal liquid material;
(6) adding adsorptive substances into the peony petal liquid material prepared in the step (5), and performing high-temperature sterilization and decoloration at 65-90 ℃, preferably 85 ℃, for 15-30 min; the adsorptive substance is one or any combination of more of white clay, quartz sand, resin and active carbon, and accounts for 1-20% of the weight of the peony petal liquid material, preferably 1-5%;
(7) performing two-stage filtration on the peony petal liquid material prepared in the step (6), wherein the filter screen is 200-800 meshes in the first-stage filtration and 1600-3500 meshes in the second-stage filtration to obtain peony flower filtrate (also called peony flower stock solution);
(8) and (4) adding the preservative optimized according to the process of the invention into the peony flower filtrate obtained in the step (7). Preparing 1 10L white plastic barrel, washing the white plastic barrel with medical alcohol for 2-3 times, and drying the white barrel; adding 30% distilled water into a treated 10L white plastic barrel, and adding peony flower filtrate (stock solution) to 1/2 barrels; adding the prepared preservative rapidly, and then adding the peony fresh flower filtrate successively until the total weight is 10 kg. Then sealing and storing to obtain the peony flower extract product. The preservative is one or any combination of more of caprylyl hydroxypentanoic acid, p-hydroxyacetophenone, propylene glycol, hexanediol and EDTA disodium, and the addition amount of the preservative is 0.01-30%, preferably 0.02-10% of the filtrate of the fresh peony flowers.
Example 1:
the peony flower extracting solution comprises the following specific steps:
(1) collecting 500Kg of red-phoenix peony petals which are opened for 1-3 days at 6-10 am of No. 4 month and No. 15;
(2) freezing and storing collected peony petals at-10 deg.C for 5 days;
(3) adding the frozen petals into microwave combined ultrasonic equipment, setting the ultrasonic frequency to be 30kHz, heating the material to 58-60 ℃, and controlling the feeding-discharging time to be within 5 minutes; heating and inactivating enzymes of fresh peony petals, and simultaneously playing a role in physical sterilization;
(4) adding the peony fresh petals subjected to enzyme deactivation and sterilization in the step (3) into a screw press, wherein the diameter of a screw is phi 300mm, and obtaining peony petal pressing liquid;
(5) standing the peony petal squeezing liquid obtained in the step (4) for 10 hours, and taking the upper layer liquid to obtain peony petal feed liquid;
(6) adding 3% of activated clay into the upper layer peony petal material liquid barrel in the step (5), stirring, heating to 80-85 ℃ in a water bath, and keeping for 30 minutes;
(7) performing two-stage filtration on the peony petal liquid material in the step (6), wherein the filter screen is 200-800 meshes in the first-stage filtration and 1600-3500 meshes in the second-stage filtration to obtain peony flower filtrate (also called peony flower stock solution);
(8) preparing 1 10L white plastic barrel, washing the white plastic barrel with medical alcohol for 2-3 times, and drying the white barrel.
(9) Preparation of preservatives
5g of caprylyl hydroxypentanoic acid, 50g of p-hydroxyacetophenone, 50g of propylene glycol and 500ml of distilled water are sequentially added into a 1L beaker, stirred and heated to 60-70 ℃, 60g of hexanediol is added, the mixture is stirred uniformly until the mixture is completely dissolved, and the mixture is cooled to the normal temperature for later use.
(10) Adding 3.0kg of distilled water into a treated 10L white plastic barrel (8), and pouring 2.0kg of the filtered peony flower filtrate (stock solution) obtained in the step (7) into the white plastic barrel; to 1/2 bucket position.
(11) Adding prepared preservative (9) rapidly, and then adding the peony fresh flower filtrate to the total weight of 10 kg. Then sealing and storing to obtain the peony flower extract product.
Example 2:
(1) collecting 500Kg of red-phoenix peony petals which are opened for 5-8 days at 6-10 am in No. 4 month and No. 18;
(2) freezing and storing collected peony petals at-10 deg.C for 5 days;
(3) adding the frozen petals into microwave combined ultrasonic equipment, setting the ultrasonic frequency as 50kHz, heating the material to 55-60 ℃, and controlling the feeding-discharging time within 5 minutes; heating and inactivating enzymes of fresh peony petals, and simultaneously playing a role in physical sterilization;
(4) adding the fresh peony petals subjected to plum killing and sterilization treatment in the step (3) into a screw press, wherein the diameter of a screw is phi 300mm, and thus obtaining peony petal pressing liquid;
(5) standing the peony petal squeezing liquid obtained in the step (4) for 15h, and taking the upper layer liquid to obtain a peony petal liquid material;
(6) adding 3% of activated carbon into the upper layer peony petal material liquid barrel in the step (5), heating to 75-80 ℃ in a water bath under stirring, and keeping for 30 minutes;
(7) performing two-stage filtration on the peony petal liquid material in the step (6), wherein the filter screen is 200-800 meshes in the first-stage filtration and 1600-3500 meshes in the second-stage filtration to obtain peony flower filtrate (also called peony flower stock solution);
(8) preparing 1 10L white plastic barrel, washing the white plastic barrel with medical alcohol for 2-3 times, and drying the white barrel.
(9) Preparation of preservatives
60g of p-hydroxyacetophenone, 50g of propylene glycol, 1.5g of disodium EDTA and 500ml of distilled water are added in sequence into a 1L beaker. Stirring and heating to 60-70 ℃, then adding 80g of hexanediol, stirring uniformly, and cooling to normal temperature for later use.
(10) Adding 3.0kg of distilled water into a treated 10L white plastic barrel (8), and putting 2.0kg of the filtered peony flower filtrate (stock solution) in the step (7) into the white plastic barrel; to 1/2 bucket position.
(11) Adding prepared preservative (9) rapidly, and then adding the peony fresh flower filtrate to the total weight of 10 kg. Then sealing and storing to obtain the peony flower extract product.
The peony flower extracting solution obtained by the invention and the stock solution prepared by the existing preparation method are used for carrying out the following experiments:
1. analysis of components of peony flower stock solution prepared by different processes
The component analysis of the peony flower extract liquid prepared by different processes is carried out by a gas chromatography, an amino acid analyzer, a spectrophotometry and a Fulin phenol method (see table 1), and the content of active substances such as amino acid, procyanidine, anthocyanin and total phenol in the peony flower stock solution prepared by the method is obviously higher than that of supercritical CO2Extracting with fluid, rotary evaporation, and distillation.
TABLE 1 analysis and comparison of ingredients of peony flower extract (example 1) and other preparation methods
2. Determination of DPPH radical scavenging Capacity
Sequentially measuring the anti-free radical scavenging capacity of the peony flower extracting solution prepared by different processes at the same time point (measuring method); and (3) detecting by using a spectrophotometer:
TABLE 2 product anti-radical scavenging ability of stock solutions prepared by different processes measured at the same time
| Item | Scavenging ability against free radicals |
| Supercritical CO2Fluid extraction method | 72.6％ |
| Rotary evaporation method | 17.8％ |
| Distillation process | 58.4％ |
| Example 1 | 94.3％ |
The data show that the anti-free radical scavenging capacity of the extracting solution of the fresh peony flowers in 4 different processes is measured in sequence at the same time point, and the measurement result proves that the anti-free radical scavenging capacity of the extracting solution of the fresh peony flowers prepared by the method is obviously higher than that of other processes.
3. Determination of anti-radical scavenging ability
The anti-radical scavenging ability of the fresh flower extract (example 1) prepared by the method of the invention was measured at different dilution times:
TABLE 3 determination of anti-free radical scavenging ability of fresh flower extract prepared according to the present invention under different dilution times
| Concentration of test solution | Scavenging ability against free radicals |
| 1％ | 16.8％ |
| 5％ | 25.6％ |
| 10％ | 33.5％ |
| 20％ | 46.5％ |
| 30％ | 55.7％ |
| 50％ | 72.6％ |
| 75％ | 87.2％ |
| 100％ | 94.3％ |
The result shows that the anti-free radical scavenging capacity of the flower extracting solution prepared by the invention is gradually enhanced along with the increase of the concentration of the flower water along with the increase of the concentration of the test solution, and the anti-free radical scavenging capacity reaches the maximum value when the concentration of the flower extracting solution is 100 percent of the original solution.
4. Stability test
Mainly investigates whether the color of the solution has obvious change and whether the phenomena of layering, turbidity, precipitation and agglomeration exist under the conditions of the same temperature, humidity and light along with the increase of the standing time of the product;
about 8mL of the peony flower stock solution prepared by the method is taken and placed in a constant-temperature constant-humidity incubator at the same time, the shelf life test of the product is carried out, the temperature is 40 ℃, the relative humidity is 75%, the light illumination is 4500Lux +/-500 Lux, the product is placed for 10 days and 30 days, the time for layering, turbidity, precipitation and agglomeration is recorded, and the stability of the product is examined.
TABLE 4 phenomena observed after 10 days of storage of the peony flower extract prepared by different processes
TABLE 5 phenomena observed after 30 days of storage of the peony flower extract prepared by different processes
As can be seen from tables 4 and 5, the products prepared by the 4 methods had only supercritical CO after standing for 10 days2The peony flower stock solution prepared by the fluid extraction method and the method has good stability and unchanged color. The phenomena of layering, turbidity, precipitation, agglomeration and the like do not occur. After being placed for 30 days, only the peony flower extracting solution (stock solution) prepared by the invention has no phenomena of layering, turbidity, precipitation, agglomeration and the like, and the product has longer shelf life.
Table 6 shows that after 30 days of standing, the main active ingredients of the peony flower extract prepared by different processes are compared
The experimental results show that the peony flower stock solution prepared by the invention contains rich active substances such as anthocyanin, procyanidine and polyphenol, and the substances which are easy to cause product instability keep better stability under the optimized preservative of the invention, and the invention is another innovation point on the basis of innovation of the preparation method; the high-oxidation-resistance peony flower stock solution prepared by the method can be used as a stable raw material for high-end cosmetic production.
Claims (10)
1. A preparation method of a cosmetic raw material peony flower extract with high oxidation resistance comprises the following preparation steps:
(1) collecting the red-phoenix peony petals at the initial stage of the flowering phase;
(2) freezing and storing the petals;
(3) heating the frozen petals to inactivate enzymes of the fresh peony petals by using microwave combined ultrasonic equipment; simultaneously, the function of physical sterilization is achieved;
(4) squeezing the material obtained in the step (3) in a spiral squeezing mode to obtain peony petal squeezing liquid;
(5) standing the peony petal squeezed liquid, and then taking the upper layer liquid to obtain a peony petal liquid material;
(6) adding the peony petal liquid material obtained in the step (5) into an adsorptive substance, and performing high-temperature sterilization and decoloration treatment;
(7) performing two-stage filtration on the peony petal liquid material prepared in the step (6) for later use;
(8) adding an anticorrosive system optimized for the process of the invention into the filtered peony flower solution obtained in the step (7); the preservative in the preservative system is one or any combination of any one of caprylyl hydroxypentanoic acid, p-hydroxyacetophenone, propylene glycol, hexanediol and EDTA disodium, and the peony flower extract is finally obtained by stirring.
2. The method of claim 1, wherein: in the step (1), the peony petals are harvested for 4-5 months, 6-10 am and 1-10 days of initial opening; preferably, the harvesting time of the peony petals is 4 months and 10 to 30, and the harvested petals are 1 to 3 days.
3. The method of claim 1, wherein: in the step (2), the freezing temperature of the petals is-5 to-18 ℃, and is preferably-10 ℃.
4. The method of claim 1, wherein: in the step (3), the ultrasonic frequency is 10-100 kHz, preferably 20-50kHz, and most preferably 30 kHz; the microwave condition is that the temperature of the materials is heated to 40-80 ℃, and the optimal temperature is 58-60 ℃; the time from feeding to discharging is controlled at 5 min.
5. The method of claim 1, wherein: in the step (5), the peony petal pressing liquid is kept still for 5-24 h.
6. The method of claim 1, wherein: in step (6), the temperature for high temperature sterilization and decolorization is set at 65-90 deg.C, preferably 85 deg.C, and the treatment time is 15-30 min.
7. The production method according to claim 1 or 6, characterized in that: in the step (6), the adsorptive substance is one or any combination of more of white clay, quartz sand, resin and activated carbon, and accounts for 1% -20% of the weight of the peony petal liquid material, preferably 1% -5%.
8. The method of claim 1, wherein: in the step (7), the filter screen for the first stage filtration is 800 meshes in size 200-.
9. The method of claim 1, wherein: in the step (8), the addition amount of the preservative is 0.01-30%, preferably 0.02-10% of the peony flower filtrate;
(1) one preparation method of the flower extracting solution comprises the following steps:
sequentially adding 5g of preservative octanoyl hydroxypentanoic acid, 50g of p-hydroxyacetophenone, 50g of propylene glycol and 500ml of distilled water into a beaker, stirring and heating to 60-70 ℃, then adding 60g of hexanediol, stirring uniformly until the hexanediol is completely dissolved to prepare a preservative system, and cooling to normal temperature for later use;
adding 3.0kg of distilled water into a 10L container, and pouring 2.0kg of the filtered peony flower filtrate obtained in the step (7) into the container; to the location of container 1/2;
rapidly adding a prepared antiseptic system, sequentially adding the peony flower filtrate until the total weight is 10kg, and sealing for storage to obtain a peony flower extract product;
(2) the second preparation method of the flower extracting solution comprises the following steps:
sequentially adding 60g of p-hydroxyacetophenone, 50g of propylene glycol, 1.5g of EDTA disodium and 500ml of distilled water into a beaker, stirring and heating to 60-70 ℃, then adding 80g of hexanediol, uniformly stirring to prepare an anticorrosive system, and cooling to normal temperature for later use;
adding 3.0kg of distilled water into a 10L container, and pouring 2.0kg of the filtered peony flower filtrate obtained in the step (7) into the container; to the location of container 1/2;
and (3) rapidly adding a prepared preservative system, then sequentially adding the peony flower filtrate until the total weight is 10kg, and then sealing and storing to obtain a peony flower extract product.
10. A peony flower extracting solution is characterized in that: the peony flower extracting solution is formed by mixing a peony flower stock solution and an antiseptic system; the preservative in the preservative system is one or any combination of more of caprylyl hydroxypentanoic acid, p-hydroxyacetophenone, propylene glycol, hexanediol and EDTA disodium, and the addition amount of the preservative is 0.01-30% of the peony flower stock solution, preferably 0.02-10%.
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| CN112111324A (en) * | 2020-09-29 | 2020-12-22 | 天宝牡丹生物科技有限公司 | Extraction method of peony flower stock solution with low cost and high extraction efficiency |
| CN113456555A (en) * | 2021-08-11 | 2021-10-01 | 云南白药集团上海科技有限公司 | Peony extract, skin external preparation containing peony extract, and preparation method and application of peony extract |
| CN115067516A (en) * | 2022-08-23 | 2022-09-20 | 山东凤凰生物科技股份有限公司 | Application of lactobacillus plantarum BLCC2-0015, peony fermentation broth and application thereof |
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