CN113975186A - Plant essential oil compound extract and preparation method and application thereof - Google Patents

Plant essential oil compound extract and preparation method and application thereof Download PDF

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CN113975186A
CN113975186A CN202111303864.7A CN202111303864A CN113975186A CN 113975186 A CN113975186 A CN 113975186A CN 202111303864 A CN202111303864 A CN 202111303864A CN 113975186 A CN113975186 A CN 113975186A
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倪柏雯
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Jiangsu Times Mingyang New Biotechnology Research Institute Co ltd
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    • 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
    • A61K8/92—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
    • A61K8/922—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof of vegetable origin
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
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    • A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
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    • 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
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    • A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/37—Esters of carboxylic acids
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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
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    • 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
    • A61Q17/00—Barrier 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
    • A61Q17/005—Antimicrobial preparations
    • 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
    • A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/52—Stabilizers
    • A61K2800/522—Antioxidants; Radical scavengers
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    • 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
    • A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/59—Mixtures
    • A61K2800/592—Mixtures of compounds complementing their respective functions
    • A61K2800/5922—At least two compounds being classified in the same subclass of A61K8/18
    • 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

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Abstract

The plant essential oil compound extract comprises a water phase, an oil phase and a natural antioxidant, wherein the water phase comprises the following components in parts by mass: 75-80 parts of ultrapure water, 4-6 parts of polyglycerol-6 stearate, 3-5 parts of glycerol, 0.3-0.5 part of sodium dehydroacetate and 0.3-0.3 part of carbomer 9400.1, wherein the oil phase comprises the following components in parts by mass: 40-50 parts of tea tree essential oil, 10-15 parts of rose essential oil, 5-10 parts of cumquat essential oil, 10-15 parts of caproic acid, 5-10 parts of capric acid and 3-5 parts of glyceryl monocaprylate. The plant essential oil composite extract, the preparation method and the application thereof have the advantages of reasonable formula arrangement, excellent antibacterial effect, aromatic smell, excellent oxidation resistance, good stability, difficult microorganism breeding, color change and odor change, good chromaticity, simple preparation method steps, improvement on the extraction methods of various plant essential oils and plant extracts, improvement on the extraction yield, reduction in cost and wide application prospect.

Description

Plant essential oil compound extract and preparation method and application thereof
Technical Field
The invention belongs to the technical field of plant essential oil compound extracts, and particularly relates to a plant essential oil compound extract and a preparation method and application thereof.
Background
In recent years, cosmetics have become an indispensable part of modern life with the development of society and the enhancement of consumption consciousness. The cosmetic industry in China is in the rapid growth stage of industrial development, but meanwhile, the application of chemical synthesis raw materials in cosmetics seriously affects the health of consumers and even causes environmental pollution, thereby causing wide social attention.
The research and the utilization of natural raw materials become a new trend of the cosmetic industry, the formulation naturalization also meets the requirement of consumption upgrade in the production and consumption of cosmetics, and the natural cosmetic formula is pursued by consumers. Therefore, the invention develops the plant essential oil composite extract and the preparation method thereof, and the natural plant essential oil and the plant extract are utilized to improve the stability and the efficacy of the formula of the cosmetic, reduce the cost and facilitate the production and the large-scale production.
Chinese patent application No. CN109381367A discloses a protein cream special for infants, which is low in applicability and does not further improve stability, antibacterial property and the like of a formula in order to solve skin problems such as dryness, speckles or "discoloration", skin allergy, neonatal jaundice, dry skin, miliaria and the like which are easily caused on the skin of infants.
Disclosure of Invention
The purpose of the invention is as follows: in order to overcome the defects, the invention aims to provide the plant essential oil composite extract, the preparation method and the application thereof, the formula is reasonable in arrangement, the antibacterial effect is excellent, the smell is fragrant, the antioxidant performance is excellent, the stability is good, microorganisms are not easy to breed, the color and the taste are not easy to change, the chromaticity is good, the steps of the preparation method are simple, the extraction yield is improved, the cost is reduced and the application prospect is wide by improving the extraction method of each plant essential oil and plant extract.
The purpose of the invention is realized by the following technical scheme:
the plant essential oil compound extract is characterized by comprising a water phase, an oil phase and a natural antioxidant, wherein the water phase comprises the following components in parts by mass: 75-80 parts of ultrapure water, 4-6 parts of polyglycerol-6 stearate, 3-5 parts of glycerol, 0.3-0.5 part of sodium dehydroacetate and 0.3-0.3 part of carbomer 9400.1, wherein the oil phase comprises the following components in parts by mass: 40-50 parts of tea tree essential oil, 10-15 parts of rose essential oil, 5-10 parts of cumquat essential oil, 10-15 parts of caproic acid, 5-10 parts of capric acid and 3-5 parts of glyceryl monocaprylate, wherein the natural antioxidant comprises the following components in parts by mass: 10-15 parts of rosemary lipid extract and 8-10 parts of green tea extract; the mass ratio of the water phase to the oil phase to the natural antioxidant is 1: 1.5-2: 0.001-0.002.
The plant essential oil composite extract is reasonable in formula design, and is prepared into cream-texture plant essential oil composite extract by compounding a water phase, an oil phase and a natural antioxidant. The plant essential oil composite extract comprises tea tree essential oil, the tea tree essential oil is a natural antibacterial substance, has a strong inhibiting effect on escherichia coli and staphylococcus aureus, is good in skin permeability, and is excellent natural skin care oil wax; the tea tree essential oil has high content of unsaturated fatty acid, is easy to oxidize, has antioxidant activity, and can improve the oil oxidation stabilization period of the tea tree essential oil; comprises cumquat essential oil which has the functions of antioxidant activity, bacteriostasis, antitoxic, anti-inflammation and analgesia and can also improve the oil oxidation stabilization period of the tea tree essential oil; the bacteriostatic agent comprises caproic acid, capric acid, caproic acid and capric acid which are used as medium-chain fatty acids, glyceryl monocaprylate which is used as medium-chain fatty acid ester, wherein the caproic acid and capric acid have strong inhibiting effect on escherichia coli, salmonella and staphylococcus aureus, and the glyceryl monocaprylate has strong inhibiting effect on staphylococcus aureus and salmonella.
At present, in order to improve the preservative capability of cosmetics, preservatives such as formaldehyde and paraben are often added, which have potential risks to skin, and some traditional preservatives such as sodium benzoate and potassium sorbate have high requirements on the pH value of products, so that the preservative capability of the cosmetics is obviously reduced in a system with a non-optimal pH value, while cason has chronic toxicity to skin.
In order to further improve the antioxidant performance of the plant essential oil composite extract, maintain the formula stability of the plant essential oil composite extract, particularly the oxidation stability of grease, avoid breeding microorganisms, discoloring and odor-changing, and mildew and odor, a natural antioxidant consisting of rosemary lipid extract and green tea extract is added, liposoluble plant extracts such as carnosic acid in the rosemary lipid extract have obvious antioxidant effect on essential oil in an oil phase, water-soluble extracts such as tea polyphenol in the green tea extract have obvious antioxidant effect on essential oil in the oil phase, particularly the liposoluble plant extract and the water-soluble extract are compounded, so that the plant essential oil composite extract has a synergistic antioxidant effect, and the expression of good chromaticity of the plant essential oil composite extract can be achieved by adjusting the content of the green tea extract.
Wherein the polyglycerol-6 stearate is from Saian Weizhen Biotech, Glycerol is from Shanghai leaf Biotech (purity: AR ≥ 99%), sodium dehydroacetate is from Sigma Aldrich trade, carbomer 940 is from Shanghai leaf Biotech (purity BR), hexanoic acid is from Sigma Aldrich trade, capric acid is from Shanghai leaf Biotech (purity: CP 98%), decanoic acid is from Shanghai leaf Biotech (purity: GC ≥ 98%), and glyceryl monocaprylate is from Shanghai leaf Biotech (purity BR).
The invention also relates to a preparation method of the plant essential oil compound extract, which comprises the following steps:
(1) preparation of the aqueous phase: dissolving carbomer 940 in ultrapure water, wherein the mass ratio of carbomer 940 to ultrapure water is 1:99-100, until carbomer 940 fully absorbs water and swells, and no agglomeration is seen, so as to obtain a component A; dissolving sodium dehydroacetate in ultrapure water, and dissolving in a vortex manner, wherein the mass ratio of the sodium dehydroacetate to the ultrapure water is 1:45-48, so as to obtain a component B; heating the ultrapure water with the residual mass to 70-75 ℃, dissolving polyglycerol-6 stearate in the ultrapure water, stirring by a stirrer at the rotation speed of 450-; placing the component A for 10-12h, then mixing the component A and the component C, stirring by a stirrer, setting the rotating speed of the stirrer to be 900-750 r/min, and the stirring time to be 10-15min to obtain a mixed solution, adding the component B into the mixed solution, continuing stirring by the stirrer, setting the rotating speed of the stirrer to be 700-750r/min, and stirring for 3-4min to obtain a water phase;
(2) preparation of oil phase: mixing tea tree essential oil, rose essential oil, cumquat essential oil, caproic acid, capric acid and glyceryl monocaprylate, heating to 70-80 ℃, continuously stirring by using a stirrer, wherein the rotating speed of the stirrer is set to be 450-year-old 500r/min, and the stirring time is 10-15min to obtain an oil phase;
(3) preparing the plant essential oil compound extract: sequentially adding the oil phase, the rosemary extract and the green tea extract into the water phase, heating to 50-60 ℃, continuously stirring by using a stirrer, setting the rotating speed of the stirrer to be 900 plus materials at 1000r/min, and the stirring time to be 20-30min, then homogenizing by using the stirrer, setting the rotating speed of the stirrer to be 1600 plus materials at 1800r/min, and the stirring time to be 10-15min to obtain the plant essential oil composite extract.
Further, the preparation method of the plant essential oil compound extract comprises the extraction of tea tree essential oil, and the extraction method of the tea tree essential oil comprises the following steps:
(1) soaking: cutting off the mutual leaf white stem layer branches and leaves, putting the mutual leaf white stem layer branches and leaves into a flask, adding ultrapure water into the flask, and soaking for 5-6h, wherein the material-liquid ratio of the mutual leaf white stem layer branches and leaves to the ultrapure water is 1: 18-20;
(2) extraction: slowly heating to boil, keeping refluxing for 4-5h until the oil amount is not increased, naturally cooling, collecting oil liquid with volatile oil extractor, adding anhydrous magnesium sulfate into the collected oil liquid, and removing water to obtain tea tree essential oil.
The branch and leaf of the interbedded white stem layer are from the area of the Yangxi province, and the anhydrous magnesium sulfate is from Guangfu scientific and technological development Limited company in Tianjin City (the purity is analytically pure).
Further, the preparation method of the plant essential oil compound extract comprises the extraction of rose essential oil, and the extraction method of rose essential oil comprises the following steps:
(1) drying and crushing: vacuum freeze drying fresh flos Rosae Rugosae for 10-12 hr, pulverizing, and sieving with 40 mesh sieve;
(2) supercritical CO2 extraction: extracting the fresh rose flowers by a supercritical CO2 extraction device, wherein the extraction pressure of the supercritical CO2 extraction device is set to be 20-25MPa, the extraction temperature is set to be 30-40 ℃, the flow rate of supercritical CO2 is set to be 1.2-1.4/h, and the extraction time is set to be 1.5-2h, so that the rose essential oil is obtained.
The fresh rose flower is from the first flower of Suhining county, Shaoyang city, Hunan province.
Further, the preparation method of the plant essential oil compound extract comprises the extraction of kumquat essential oil, and the extraction method of the kumquat essential oil comprises the following steps:
(1) drying and crushing: cleaning fresh Fortunella margarita, air drying, removing pulp, vacuum freeze drying Fortunella margarita peel for 10-12 hr, pulverizing, and sieving with 80 mesh sieve to obtain Fortunella margarita peel powder;
(2) and (3) extraction: and (2) filling the kumquat peel powder into a balance kettle, sealing the balance kettle, wrapping an electric heating belt outside the balance kettle, filling R134 a-10.0-12.0 Mpa into the balance kettle at a temperature of 45-50 ℃ at a flow rate of R134a of 1.5-2.0L/min, extracting for 1.5-2h at the temperature of the balance kettle, and after extraction is finished, discharging the liquid in the balance kettle until yellow oily liquid does not exist and collecting to obtain the kumquat essential oil.
The R134a is obtained from Oborubin technology, Inc. (purity: AR ≥ 99.9%).
Further, the preparation method of the plant essential oil compound extract comprises the following steps of:
(1) crushing: pulverizing herba Rosmarini officinalis with pulverizer, and sieving with 30 mesh sieve to obtain herba Rosmarini officinalis powder:
(2) extraction: putting rosemary powder into a flask, adding ethanol into the flask, wherein the concentration of the ethanol is 80%, the material-liquid ratio of the rosemary powder to the ethanol is 1:10-12, performing ultrasonic-assisted extraction at 50-60 ℃, filtering, the extraction time is 45-50min, the frequency of the ultrasonic-assisted extraction is 25-30kHz and the power is 200W, repeating the operation for 2-3 times, combining the filtrates obtained by the 2-3 times of extraction, and concentrating to dryness to obtain the rosemary lipid extract.
The rosemary is from Bozhou city Yingzhengtang pharmaceutical Co., Ltd, and the ethanol is from Sigma Aldrich (Shanghai) trade Co., Ltd
Further, the preparation method of the plant essential oil compound extract, the extraction of the green tea extract and the extraction method of the green tea extract comprise the following steps:
(1) crushing: pulverizing green tea leaves by a pulverizer, and sieving by a 60-mesh sieve to obtain green tea powder;
(2) leaching and suction filtration: placing green tea powder into a flask, adding ultrapure water into the flask, heating the green tea powder and the ultrapure water to 70-80 ℃, leaching at the constant temperature of 70-80 ℃ for 0.5-1h, repeating the operation for 2-3 times, and filtering and combining the leaching liquor;
(3) concentration and extraction: concentrating the leaching solution under reduced pressure, adding ethyl acetate with the same volume, stirring uniformly, standing for layering, repeating the operation for 2-3 times, and collecting a water phase; adding equal volume of ethyl acetate into the collected water phase, stirring uniformly, standing for layering, collecting an organic phase, adding equal volume of ethyl acetate into the lower layer water phase, extracting repeatedly for 2-3 times, distilling the organic phase under reduced pressure, drying to obtain an extract I, adding anhydrous ethanol into the combined water phase for 2-3 times for precipitation, standing for 10-12h, centrifuging and drying to obtain an extract II, and uniformly mixing the extract I and the extract II to obtain the green tea extract.
The green tea leaf is from Zhejiang tea Qiankun food company, Inc., and the ethyl acetate and the absolute ethyl alcohol are from Sigma Aldrich (Shanghai) trade company, Inc.
Further, the plant essential oil compound extract is used in cosmetics, including basic cosmetics, beauty cosmetics and curative cosmetics.
Compared with the prior art, the invention has the following beneficial effects:
(1) the formula of the plant essential oil composite extract disclosed by the invention is reasonable in design, and the plant essential oil composite extract with cream texture is obtained by compounding the water phase, the oil phase and the natural antioxidant; the compounding of the tea tree essential oil, the rose essential oil, the cumquat essential oil, the caproic acid, the capric acid and the glyceryl monocaprylate has excellent antibacterial property, the compounding of the rose essential oil, the cumquat essential oil, the rosemary extract and the green tea extract improves the antioxidant property of the plant essential oil composite extract, the formula stability of the plant essential oil composite extract is maintained, and the caproic acid, the capric acid and the glyceryl monocaprylate are added to play a synergistic role with the plant essential oils such as the tea tree essential oil and the rose essential oil, so that the combination of high-efficiency bacteriostasis and reduction of respective effective dosage is achieved;
(2) the preparation method of the plant essential oil composite extract, disclosed by the invention, has the advantages of reasonable arrangement of preparation steps, simplicity, controllability and high flexibility, improves the extraction yield and reduces the cost by improving the extraction method of each plant essential oil and plant extract, and has wide application prospect.
Detailed Description
In the following, the technical solutions in the embodiments of the present invention are clearly and completely described in the embodiments with reference to specific experimental data, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The following examples provide a plant essential oil compound extract and a preparation method thereof, wherein the plant essential oil compound extract comprises a water phase, an oil phase and a natural antioxidant, and the water phase comprises the following components in parts by mass: 75-80 parts of ultrapure water, 4-6 parts of polyglycerol-6 stearate, 3-5 parts of glycerol, 0.3-0.5 part of sodium dehydroacetate and 0.3-0.3 part of carbomer 9400.1, wherein the oil phase comprises the following components in parts by mass: 40-50 parts of tea tree essential oil, 10-15 parts of rose essential oil, 5-10 parts of cumquat essential oil, 10-15 parts of caproic acid, 5-10 parts of capric acid and 3-5 parts of glyceryl monocaprylate, wherein the natural antioxidant comprises the following components in parts by mass: 10-15 parts of rosemary lipid extract and 8-10 parts of green tea extract; the mass ratio of the water phase to the oil phase to the natural antioxidant is 1: 1.5-2: 0.001-0.002.
Example 1
The plant essential oil compound extract comprises a water phase, an oil phase and a natural antioxidant, wherein the water phase comprises the following components in parts by weight: 80 parts of ultrapure water, 5 parts of polyglycerol-6 stearate, 4 parts of glycerol, 0.5 part of sodium dehydroacetate and 9400.2 parts of carbomer, wherein the oil phase comprises the following components in parts by mass: 45 parts of tea tree essential oil, 15 parts of rose essential oil, 5 parts of cumquat essential oil, 15 parts of caproic acid, 8 parts of capric acid and 3 parts of glycerol monocaprylate, wherein the natural antioxidant comprises the following components in parts by mass: 15 parts of rosemary lipid extract and 8 parts of green tea extract; the mass ratio of the water phase to the oil phase to the natural antioxidant is 1: 1.5: 0.0015, the preparation method of the plant essential oil compound extract comprises the following steps:
(1) preparation of the aqueous phase: dissolving carbomer 940 in ultrapure water, wherein the mass ratio of carbomer 940 to ultrapure water is 1:99, until carbomer 940 fully absorbs water and swells, and no agglomeration is seen, so as to obtain a component A; dissolving sodium dehydroacetate in ultrapure water, and dissolving in a vortex manner, wherein the mass ratio of the sodium dehydroacetate to the ultrapure water is 1:45 to obtain a component B; heating ultrapure water with the residual mass to 75 ℃, dissolving polyglycerol-6 stearate in the ultrapure water, stirring by a stirrer at the rotating speed of 500r/min for 15min, adding glycerol, continuously stirring by the stirrer at the rotating speed of 450r/min for 5min to obtain a component C; standing the component A for 12h, mixing the component A and the component C, stirring by a stirrer, setting the rotation speed of the stirrer to be 1000r/min, and stirring for 15min to obtain a mixed solution, adding the component B into the mixed solution, continuously stirring by the stirrer, setting the rotation speed of the stirrer to be 750r/min, and stirring for 4min to obtain a water phase;
(2) preparation of oil phase: mixing tea tree essential oil, rose essential oil, cumquat essential oil, caproic acid, capric acid and glyceryl monocaprylate, heating to 80 ℃, and continuously stirring by using a stirrer, wherein the rotating speed of the stirrer is set to be 500r/min, and the stirring time is 15min, so as to obtain an oil phase;
(3) preparing the plant essential oil compound extract: sequentially adding the oil phase, the rosemary extract and the green tea extract into the water phase, heating to 55 ℃, continuously stirring by using a stirrer, wherein the rotating speed of the stirrer is set to 900r/min, the stirring time is 25min, then homogenizing by using the stirrer, the rotating speed of the stirrer is set to 1800r/min, and the stirring time is 15min, so as to obtain the plant essential oil compound extract I.
Comparative example 1
The plant essential oil compound extract comprises a water phase, an oil phase and a natural antioxidant, wherein the water phase comprises the following components in parts by weight: 80 parts of ultrapure water, 5 parts of polyglycerol-6 stearate, 4 parts of glycerol, 0.5 part of sodium dehydroacetate and 9400.2 parts of carbomer, wherein the oil phase comprises tea tree essential oil; the mass ratio of the water phase to the oil phase is 1:1.5, and the preparation method of the plant essential oil compound extract comprises the following steps:
(1) preparation of the aqueous phase: dissolving carbomer 940 in ultrapure water, wherein the mass ratio of carbomer 940 to ultrapure water is 1:99, until carbomer 940 fully absorbs water and swells, and no agglomeration is seen, so as to obtain a component A; dissolving sodium dehydroacetate in ultrapure water, and dissolving in a vortex manner, wherein the mass ratio of the sodium dehydroacetate to the ultrapure water is 1:45 to obtain a component B; heating ultrapure water with the residual mass to 75 ℃, dissolving polyglycerol-6 stearate in the ultrapure water, stirring by a stirrer at the rotating speed of 500r/min for 15min, adding glycerol, continuously stirring by the stirrer at the rotating speed of 450r/min for 5min to obtain a component C; standing the component A for 12h, mixing the component A and the component C, stirring by a stirrer, setting the rotation speed of the stirrer to be 1000r/min, and stirring for 15min to obtain a mixed solution, adding the component B into the mixed solution, continuously stirring by the stirrer, setting the rotation speed of the stirrer to be 750r/min, and stirring for 4min to obtain a water phase;
(2) preparing the plant essential oil compound extract: adding tea tree essential oil into the water phase, heating to 55 ℃, continuously stirring by a stirrer, setting the rotating speed of the stirrer to be 900r/min, stirring for 25min, homogenizing by the stirrer, setting the rotating speed of the stirrer to be 1800r/min, and stirring for 15min to obtain a second plant essential oil compound extract.
And (3) measuring the oxidation stability of the oil: the oil oxidation stability of the plant essential oil compound extract I and the plant essential oil compound extract II is measured by a 743 type edible oil oxidation stability tester; the test conditions were: the temperature is 120 ℃, and the air flow is 20L/h. And 3g of the plant essential oil compound extract I or the plant essential oil compound extract II is put into a reaction tube, 50mL of distilled water is added into a receiving pool, when the temperature of a heating tank reaches a measurement temperature, the conductivity curve of the sample in the reaction tube is measured, and the time when the second derivative of the conductivity is maximum is taken as a measurement end point, so that the oil stabilization period of the sample is evaluated.
And (3) measuring the peroxide value: the peroxide value represents an index of the degree of oxidation of fats and oils, fatty acids, and the like. Is the active oxygen content in the 1kg sample, expressed as millimoles of peroxide. Indicating whether the sample has been deteriorated by oxidation. Products made from fats and oils can be judged for quality and degree of deterioration by detecting their peroxide value. The peroxide value determination steps of the plant essential oil compound extract I and the plant essential oil compound extract II are as follows: mixing the first plant essential oil compound extract or the second plant essential oil compound extract 0.3g with 3mL of isooctane/2-propanol (3: 1, v/v), and vortexing (10s, 3 times). After centrifugation at 1000rpm for 2min, 100. mu.L of the organic solvent phase was mixed with 100. mu.L of methanol/isobutanol (2: 1, v/v), 15. mu.L of 3.94M ammonium thiocyanate and 15. mu.L of ferrous iron solution (prepared by adding equal amounts of 0.132MBaCl2 and 0.144M FeS04, as ready for use) were added and after incubation at room temperature for 20min exactly protected from light at 4minThe absorbance was measured at a wavelength of 75nm, using a mixed solvent of methanol/isobutanol (2: 1, v/v) as a blank. Determining the concentration of plant essential oil complex extract mono or plant essential oil complex extract diperoxide using a standard curve prepared with hydrogen peroxide (y ═ 0.0079x-0.0005, R ═ 0.0079x-0.000520.9994). During testing, the test piece is placed in an oven at 60 ℃ for accelerated oxidation, the peroxide value is detected every 4 days, and the observation period is set to be 16 days according to the result of a pre-experiment.
And (3) antibacterial property measurement: (1)1, culture medium and reagent preparation: beef extract peptone liquid medium: taking 3g of beef extract, 10g of peptone and 5g of sodium chloride, adding 1000mL of water, heating, adjusting the pH value to 7.0-7.2, and subpackaging in triangular flasks. Sealing, and sterilizing at 121 deg.C and 0.1mpa for 20 min. If a solid medium is prepared, 2% agar is added, and the operation is the same as above. Used for culturing escherichia coli, staphylococcus aureus and salmonella; 2. preparation of phosphate buffer solution: accurately weighing 2.83g of anhydrous disodium hydrogen phosphate and 1.36g of potassium dihydrogen phosphate, adding into 1000ml of double distilled water, adjusting the pH to 7.2-7.4 after complete dissolution, and sterilizing for later use; 3. normal saline 0.85g sodium chloride was added to a volume of 1000mL in a volumetric flask with distilled water. And (5) sterilizing for later use. (2) Preparation of bacterial suspension: inoculating the frozen and preserved Escherichia coli, Staphylococcus aureus and Salmonella into a test tube slant containing beef extract peptone solid medium, placing in a constant temperature incubator at 37 deg.C, and culturing for 24 h. Inoculating the recovered Escherichia coli Staphylococcus aureus and Salmonella to beef extract peptone liquid culture medium, activating and culturing at 37 deg.C for 120r/min in shaking table for a certain time, and separating single colony by plate-streaking method. The 1 single colony was picked up and cultured in 100mL beef extract peptone broth at 37 ℃ on a shaker at 120 r/min. The liquid culture medium without bacteria was used as a blank, and the OD was measured by sampling every 2 hours600nmValue, determined for 24 hours. Using time as abscissa, OD600nmThe values are ordinate and growth curves of the three bacteria were made, respectively. According to the growth curve of each bacterium, picking single colony to 100mL liquid culture medium, shake culturing at 37 deg.C and 120r/min to logarithmic phase, coating, counting and determining the timeThe corresponding absorbance value. And diluting the strain to a certain bacterial liquid concentration by adopting a tenfold dilution method for later use. (3) Weighing a certain amount of the plant essential oil compound extract I or the plant essential oil compound extract II, dissolving the plant essential oil compound extract I or the plant essential oil compound extract II in 0.5% (v/v) of absolute ethyl alcohol, then adding sterile liquid containing 0.5% (w/v) of Tween-80, stirring while pouring, and shaking uniformly to obtain a sample solution 1 and a sample solution 2. Wherein the ethanol content is 0.5%, and the Tween-80 content is 0.5%. Sample solution 1 and sample solution 2 were prepared to a concentration of 2.0% (w/w), respectively, and 100. mu.L of 10 was aspirated using sterile liquid containing 0.5% ethanol and 0.5% Tween-80 as a control7And (3) placing the CFU/mL bacterial suspension in a nutrient agar culture dish, uniformly coating, and standing for 4-6 hours to ensure that the thallus is stably attached to the surface of a solid culture medium. The culture dish is divided into 4 areas on average, a sterile gun head with the diameter of 8mm is used for punching at the central position of each area, the small holes are sealed by alcohol lamp flame, and then 100uL of sample solution with corresponding concentration is added into each hole. Marking, horizontally placing the culture dish in a constant temperature incubator at 37 ℃, taking out after standing and culturing for 24h, and measuring the size of the bacteriostatic zone by using a vernier caliper. The experiment was repeated 3 times and the mean was calculated. When the diameter of the inhibition zone is 8mm, no bacteriostasis is considered, and the larger the diameter of the inhibition zone is, the better the bacteriostasis effect is.
TABLE 1
Figure BDA0003339415750000141
Example 2
The extraction method of the tea tree essential oil comprises the following steps:
(1) soaking: cutting off the branches and leaves of the interbedded white stem layer, putting the branches and leaves of the interbedded white stem layer into a flask, adding ultrapure water into the flask, and soaking for 6 hours, wherein the material-liquid ratio of the branches and leaves of the interbedded white stem layer to the ultrapure water is 1: 20;
(2) extraction: slowly heating to boil, keeping refluxing for 5h until the oil amount is not increased, naturally cooling, collecting oil liquid by a volatile oil extractor, adding anhydrous magnesium sulfate into the collected oil liquid, and removing water to obtain tea tree essential oil.
The branch and leaf of the interbedded white stem layer are from the area of the Yangxi province, and the anhydrous magnesium sulfate is from Guangfu scientific and technological development Limited company in Tianjin City (the purity is analytically pure). According to the method for extracting the tea tree essential oil, the average extraction yield of the tea tree essential oil is 2.5678% (the average extraction yield is the mass of the extracted tea tree essential oil/the mass of the interfilament white dry layer branches and leaves, the tea tree essential oil is weighed by an electronic balance, the mass of the tea tree essential oil is obtained by a differential method, the yield is influenced by partial oil volatilization after the interfilament white dry layer plants are dried to dryness, the mass of the interfilament white dry layer branches and leaves is obtained by weighing after the surface moisture of the interfilament white dry layer branches and leaves is naturally dried under the condition of room temperature, and the tea tree essential oil is weighed again after being dried to constant weight and obtained by the differential method).
Example 3
The extraction method of the rose essential oil comprises the following steps:
(1) drying and crushing: vacuum freeze drying fresh flos Rosae Rugosae for 12 hr, pulverizing, and sieving with 40 mesh sieve;
(2) supercritical CO2 extraction: extracting the fresh rose flowers by a supercritical CO2 extraction device, wherein the extraction pressure of the supercritical CO2 extraction device is set to be 25MPa, the extraction temperature is set to be 35 ℃, the flow of the supercritical CO2 is set to be 1.2/h, and the extraction time is set to be 2h, so that the rose essential oil is obtained.
The fresh rose flower is from Suizhining county flower I of Shaoyang city in Hunan province, and the average extraction yield of the rose essential oil is 1.35% (the average extraction yield is the mass of the extracted rose essential oil/the mass of the fresh rose flower, the tea tree essential oil is weighed by an electronic balance, and the mass of the tea tree essential oil is obtained by differential subtraction).
Example 4
The method for extracting kumquat essential oil comprises the following steps:
(1) drying and crushing: cleaning fresh Fortunella margarita, air drying, removing pulp, vacuum freeze drying Fortunella margarita peel for 12 hr, pulverizing, and sieving with 80 mesh sieve to obtain Fortunella margarita peel powder;
(2) and (3) extraction: and (2) filling the kumquat peel powder into a balance kettle, sealing the balance kettle, wrapping an electric heating belt outside the balance kettle, filling R134 a-12.0 Mpa into the balance kettle in the balance kettle, setting the flow of R134a at 1.8L/min, setting the temperature of the balance kettle at 45 ℃, and extracting for 2h, and after extraction is finished, discharging the liquid in the balance kettle until yellow oily liquid does not exist and collecting to obtain the kumquat essential oil.
The R134a is obtained from Oborubin technology limited (purity: AR is more than or equal to 99.9%), and the average extraction yield of the cumquat essential oil is 4.56% (average extraction yield is the quality of the extracted cumquat essential oil/the quality of cumquat). In addition, the D-limonene content of the kumquat essential oil is 68.1%.
Example 5
The method for extracting the rosemary lipid extract comprises the following steps:
(1) crushing: pulverizing herba Rosmarini officinalis with pulverizer, and sieving with 30 mesh sieve to obtain herba Rosmarini officinalis powder:
(2) extraction: putting rosemary powder into a flask, adding ethanol into the flask, wherein the concentration of the ethanol is 80%, the material-liquid ratio of the rosemary powder to the ethanol is 1:12, performing ultrasonic-assisted extraction at 55 ℃, filtering, wherein the extraction time is 45min, the frequency of the ultrasonic-assisted extraction is 25-30kHz and the power is 200W, repeating the operation for 3 times, combining the filtrates obtained by the 3 times of extraction, and concentrating to dryness to obtain a rosemary lipid extract.
The rosemary was obtained from the national institute of justice pharmaceutical limited, Bozhou city, the ethanol was obtained from Sigma Aldrich (Shanghai) trade limited, and the average extraction yield of the rosemary lipid extract was 20.3% (average extraction yield ═ mass of extracted rosemary lipid extract/mass of rosemary). In addition, the rosemary lipid extract had a carnosic acid content of 8.6%, a carnosol content of 12.3%, and a rosmarinic acid content of 3.2%.
Example 6
The extraction method of the green tea extract comprises the following steps:
(1) crushing: pulverizing green tea leaves by a pulverizer, and sieving by a 60-mesh sieve to obtain green tea powder;
(2) leaching and suction filtration: placing green tea powder into a flask, adding ultrapure water into the flask, heating the green tea powder and the ultrapure water to 80 ℃ at a material-liquid ratio of 1:25, leaching at 80 ℃ for 1h at constant temperature, repeating the operation for 3 times, and filtering and combining the leaching liquor;
(3) concentration and extraction: concentrating the leaching solution under reduced pressure, adding ethyl acetate with the same volume, stirring uniformly, standing for layering, repeating the operation for 3 times, and collecting a water phase; adding equal volume of ethyl acetate into the collected water phase, stirring uniformly, standing for layering, collecting an organic phase, adding equal volume of ethyl acetate into the lower water phase, extracting repeatedly for 3 times, distilling the organic phase under reduced pressure, drying to obtain an extract I, adding anhydrous ethanol into the 3 combined water phases for precipitation, standing for 12h, centrifuging and drying to obtain an extract II, and uniformly mixing the extract I and the extract II to obtain the green tea extract.
The green tea leaves come from Qiankun food products of Zhejiang tea, and the ethyl acetate and the absolute ethyl alcohol come from Sigma Aldrich trade company, the extraction method of the green tea extract has the advantages that the first extract is tea polyphenol, the second extract is tea polysaccharide, the average extraction yield of the tea polyphenol is 14.21%, and the average extraction yield of the tea polysaccharide is 8.69% (the average extraction yield is the quality of the extracted tea polyphenol or tea polysaccharide/the quality of the green tea leaves).
The specific applications of the present invention are numerous and the above description is only of the preferred embodiment of the invention. It should be noted that the above examples are only for illustrating the present invention, and are not intended to limit the scope of the present invention. It will be apparent to those skilled in the art that various modifications can be made without departing from the principles of the invention and these modifications are to be considered within the scope of the invention.

Claims (8)

1. The plant essential oil compound extract is characterized by comprising a water phase, an oil phase and a natural antioxidant, wherein the water phase comprises the following components in parts by mass: 75-80 parts of ultrapure water, 4-6 parts of polyglycerol-6 stearate, 3-5 parts of glycerol, 0.3-0.5 part of sodium dehydroacetate and 0.3-0.3 part of carbomer 9400.1, wherein the oil phase comprises the following components in parts by mass: 40-50 parts of tea tree essential oil, 10-15 parts of rose essential oil, 5-10 parts of cumquat essential oil, 10-15 parts of caproic acid, 5-10 parts of capric acid and 3-5 parts of glyceryl monocaprylate, wherein the natural antioxidant comprises the following components in parts by mass: 10-15 parts of rosemary lipid extract and 8-10 parts of green tea extract; the mass ratio of the water phase to the oil phase to the natural antioxidant is 1: 1.5-2: 0.001-0.002.
2. The preparation method of the plant essential oil composite extract as claimed in claim 1, which comprises the following steps:
preparation of the aqueous phase: dissolving carbomer 940 in ultrapure water, wherein the mass ratio of carbomer 940 to ultrapure water is 1:99-100, until carbomer 940 fully absorbs water and swells, and no agglomeration is seen, so as to obtain a component A; dissolving sodium dehydroacetate in ultrapure water, and dissolving in a vortex manner, wherein the mass ratio of the sodium dehydroacetate to the ultrapure water is 1:45-48, so as to obtain a component B; heating the ultrapure water with the residual mass to 70-75 ℃, dissolving polyglycerol-6 stearate in the ultrapure water, stirring by a stirrer at the rotation speed of 450-charge 500r/min for 10-15min, adding glycerol, continuously stirring by the stirrer at the rotation speed of 450-charge 500r/min for 5-10min to obtain a component C, standing the component A for 10-12h, mixing the component A and the component C, stirring by the stirrer at the rotation speed of 900-charge 1000r/min for 10-15min to obtain a mixed solution, adding the component B into the mixed solution, continuously stirring by the stirrer at the rotation speed of 700-charge 750r/min for 3-4min, obtaining a water phase;
preparation of oil phase: mixing tea tree essential oil, rose essential oil, cumquat essential oil, caproic acid, capric acid and glyceryl monocaprylate, heating to 70-80 ℃, continuously stirring by using a stirrer, wherein the rotating speed of the stirrer is set to be 450-year-old 500r/min, and the stirring time is 10-15min to obtain an oil phase;
preparing the plant essential oil compound extract: sequentially adding the oil phase, the rosemary extract and the green tea extract into the water phase, heating to 50-60 ℃, continuously stirring by using a stirrer, setting the rotating speed of the stirrer to be 900 plus materials at 1000r/min, and the stirring time to be 20-30min, then homogenizing by using the stirrer, setting the rotating speed of the stirrer to be 1600 plus materials at 1800r/min, and the stirring time to be 10-15min to obtain the plant essential oil composite extract.
3. The method for preparing the composite extract of essential oil of plants according to claim 2, which comprises the extraction of tea tree essential oil, wherein the method for extracting tea tree essential oil comprises the following steps:
soaking: cutting off the mutual leaf white stem layer branches and leaves, putting the mutual leaf white stem layer branches and leaves into a flask, adding ultrapure water into the flask, and soaking for 5-6h, wherein the material-liquid ratio of the mutual leaf white stem layer branches and leaves to the ultrapure water is 1: 18-20;
extraction: slowly heating to boil, keeping refluxing for 4-5h until the oil amount is not increased, naturally cooling, collecting oil liquid with volatile oil extractor, adding anhydrous magnesium sulfate into the collected oil liquid, and removing water to obtain tea tree essential oil.
4. The preparation method of the plant essential oil compound extract as claimed in claim 2, which comprises the extraction of rose essential oil, and the extraction method of the rose essential oil comprises the following steps:
drying and crushing: vacuum freeze drying fresh flos Rosae Rugosae for 10-12 hr, pulverizing, and sieving with 40 mesh sieve;
supercritical CO2 extraction: extracting the fresh rose flowers by a supercritical CO2 extraction device, wherein the extraction pressure of the supercritical CO2 extraction device is set to be 20-25MPa, the extraction temperature is set to be 30-40 ℃, the flow rate of supercritical CO2 is set to be 1.2-1.4/h, and the extraction time is set to be 1.5-2h, so that the rose essential oil is obtained.
5. The preparation method of the plant essential oil composite extract as claimed in claim 2, which comprises the extraction of kumquat essential oil, wherein the extraction method of kumquat essential oil comprises the following steps:
drying and crushing: cleaning fresh Fortunella margarita, air drying, removing pulp, vacuum freeze drying Fortunella margarita peel for 10-12 hr, pulverizing, and sieving with 80 mesh sieve to obtain Fortunella margarita peel powder;
and (3) extraction: and (2) filling the kumquat peel powder into a balance kettle, sealing the balance kettle, wrapping an electric heating belt outside the balance kettle, filling R134 a-10.0-12.0 Mpa into the balance kettle at a temperature of 45-50 ℃ at a flow rate of R134a of 1.5-2.0L/min, extracting for 1.5-2h at the temperature of the balance kettle, and after extraction is finished, discharging the liquid in the balance kettle until yellow oily liquid does not exist and collecting to obtain the kumquat essential oil.
6. The use of the plant essential oil composite extract as claimed in claim 2, wherein the rosemary lipid extract is extracted, and the extraction method of the rosemary lipid extract comprises the following steps:
crushing: pulverizing herba Rosmarini officinalis with pulverizer, and sieving with 30 mesh sieve to obtain herba Rosmarini officinalis powder:
extraction: putting rosemary powder into a flask, adding ethanol into the flask, wherein the concentration of the ethanol is 80%, the material-liquid ratio of the rosemary powder to the ethanol is 1:10-12, performing ultrasonic-assisted extraction at 50-60 ℃, filtering, the extraction time is 45-50min, the frequency of the ultrasonic-assisted extraction is 25-30kHz and the power is 200W, repeating the operation for 2-3 times, combining the filtrates obtained by the 2-3 times of extraction, and concentrating to dryness to obtain the rosemary lipid extract.
7. The use of the plant essential oil complex extract as claimed in claim 2, wherein the extraction of the green tea extract, the extraction method of the green tea extract, comprises the following steps:
crushing: pulverizing green tea leaves by a pulverizer, and sieving by a 60-mesh sieve to obtain green tea powder;
leaching and suction filtration: placing green tea powder into a flask, adding ultrapure water into the flask, heating the green tea powder and the ultrapure water to 70-80 ℃, leaching at the constant temperature of 70-80 ℃ for 0.5-1h, repeating the operation for 2-3 times, and filtering and combining the leaching liquor;
concentration and extraction: concentrating the leaching solution under reduced pressure, adding ethyl acetate with the same volume, stirring uniformly, standing for layering, repeating the operation for 2-3 times, and collecting a water phase; adding equal volume of ethyl acetate into the collected water phase, stirring uniformly, standing for layering, collecting an organic phase, adding equal volume of ethyl acetate into the lower layer water phase, extracting repeatedly for 2-3 times, distilling the organic phase under reduced pressure, drying to obtain an extract I, adding anhydrous ethanol into the combined water phase for 2-3 times for precipitation, standing for 10-12h, centrifuging and drying to obtain an extract II, and uniformly mixing the extract I and the extract II to obtain the green tea extract.
8. Use of a plant essential oil complex extract according to claim 1, wherein the plant essential oil complex extract is used in cosmetics, including basic cosmetics, beauty cosmetics, and therapeutic cosmetics.
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* Cited by examiner, † Cited by third party
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