Vanilla oily substance, preparation method thereof, composition and application of vanilla oily substance in preparation of care products

Abstract

The invention discloses a vanilla oily substance, a preparation method thereof, a composition and application of the vanilla oily substance in preparation of nursing products. The method comprises the following steps: providing seeds and pods of vanilla; extracting a first vanilla oily substance from the pods of the vanilla by using an enzymolysis method; gathering seeds of vanilla, and performing supercritical CO2 extraction and separation treatment to obtain a second vanilla oily substance; the vanilla oily substance is prepared from a composition of the first vanilla oily substance and the second vanilla oily substance. The preparation method of the vanilla oily substance comprises the following steps: stripping complete pods of vanilla into pods and seeds, extracting a first vanilla oily substance from the pods by using an enzymolysis method, and extracting a second vanilla oily substance from the seeds by using a supercritical CO2 extraction method, the first vanilla oily substance and the second vanilla oily substance are mixed to prepare the vanilla oily substance which is relatively pure in smell and beautiful in color, the yield of the vanilla oily substance containing vanillin is increased, and the vanilla oily substance has the effect of promoting repair of damaged cells.

Description

Technical Field

[0001] The present application belongs to the technical field of cosmetics, and in particular relates to a vanilla oily substance, a preparation method thereof, a composition thereof, and an application thereof in the preparation of care products. Background Art

[0002] Vanilla planifolia Andr, also known as vanilla, is widely known and understood as the "king of food spices", but its special biological activity as a medicinal plant has also been downplayed. The first documented record of the biological activity of vanilla was recorded in the "Xinhua Compendium of Materia Medica". It is the whole herb of the orchidaceae plant Vanilla orchid, which is bitter and cool, and enters the heart and stomach meridians. It has the effect of clearing away heat and detoxification, and is mainly used to treat heat toxins, sores, unknown swellings, eczema, scabies, and insect and snake bites. Foreign research reports: Vanilla pods have the effects of strengthening the heart, nourishing the kidneys, strengthening the stomach, and expelling wind, and can eliminate obstruction, reduce the viscosity of body fluids, diuresis, and facilitate menstruation. It has a stimulating effect on the nervous system and has been recommended for the treatment of hysteria and low fever. It also has a refreshing effect on brain function and can enhance muscle strength. Vanillin, the main ingredient in vanilla, is believed to have aphrodisiac, carminative, antispasmodic, tonic and stimulant effects; vanillin can be used as an anticonvulsant, and its anticonvulsant effect has been confirmed by experiments on epileptic guinea pigs and convulsive mice. Vanillin reduces epileptic discharges in electroencephalography; vanillin helps protein synthesis and muscle regeneration, and is used for certain types of prostate enlargement after surgery and trauma; vanilla has been officially recorded in the pharmacopoeias of many countries.

[0003] In order to meet the huge demand for vanillin, scientists have developed a chemical synthesis method for vanillin. However, chemically synthesized vanillin has safety issues and poor flavor, which seriously limits its application, especially in high-end value-added products. Natural vanillin is generally obtained by further separation and extraction of vanilla pod extract as raw material. At present, the price of natural vanillin is very expensive. The reason for the high price of natural vanillin is that the source of vanilla pods is very limited, which is restricted by factors such as production area and weather. In particular, the flowers need to be artificially pollinated during the planting process of vanilla, which makes it difficult to plant on a large scale. On the other hand, because the processing of vanilla pods is mainly based on the extensive form of traditional fermentation and aroma production, the content of glucose vanillin in fresh vanilla pods is 15% to 20%. Theoretically, it can be converted into about 5% (dry basis weight) of vanillin after enzymatic hydrolysis. However, after the traditional fermentation and aroma production method, only about 2% (dry basis weight) of vanillin is produced, resulting in a low yield of vanilla extract containing vanillin, which also leads to the high price of natural vanillin. Therefore, it is necessary to improve the preparation method of vanilla pod extract. Summary of the invention

[0004] The embodiment of the present application provides a method for preparing a vanilla oily substance, which can prepare a vanilla oily substance with a relatively pure smell and beautiful color, and improve the yield of the vanilla oily substance containing vanillin, and the prepared vanilla oily substance has the effect of effectively promoting the repair of damaged cells.

[0005] In a first aspect, the present application provides a method for preparing a vanilla oily substance, comprising: providing vanilla seeds and pods; extracting a first vanilla oily substance from the vanilla pods by enzymatic hydrolysis, comprising: refining the vanilla pods to obtain pod powder, and dispersing the pod powder with water to obtain a first dispersion; adding a decomposing enzyme to the first dispersion to perform enzymatic hydrolysis to obtain an enzymatic hydrolysis product; heating the enzymatic hydrolysis product to 80°C to 100°C for a first period of time for cyclic solid-liquid extraction and separation to obtain a first mixed solution; adding a first extractant to the first mixed solution for sedimentation separation to obtain a supernatant; concentrating the supernatant to an extract; adding a second extractant to the extract for extraction to obtain a second mixed solution; removing the second extractant from the second mixed solution to obtain the first vanilla oily substance; aggregating the vanilla seeds and using supercritical CO 2 The second vanilla oily substance is obtained by extraction treatment; and the vanilla oily substance is obtained by preparing the first vanilla oily substance and the second vanilla oily substance.

[0006] According to an embodiment of the first aspect of the present application, providing vanilla seeds and pods includes peeling the pods and seeds of vanilla in a mature stage and placing them separately to provide vanilla seeds and pods.

[0007] According to an embodiment of the first aspect of the present application, refining the vanilla pods includes: grinding or ultrasonically crushing the vanilla pods to obtain pod powder with a particle size of ≤1000 μm.

[0008] According to an embodiment of the first aspect of the present application, the dispersion treatment using water includes: adding water in an amount of 1 to 20 times the mass of the bean pod powder to the bean pod powder to prepare a first dispersion.

[0009] According to an embodiment of the first aspect of the present application, a decomposing enzyme is added to the first dispersion for enzymatic hydrolysis, comprising: adjusting the pH value of the first dispersion to 3.0-7.0, adding a decomposing enzyme and performing enzymatic hydrolysis at 40°C-80°C to obtain an enzymatic hydrolysis product.

[0010] According to an embodiment of the first aspect of the present application, a decomposing enzyme is added to the first dispersion in an amount of 0.01 g / kg to 15 g / kg.

[0011] According to an embodiment of the first aspect, the degrading enzyme is selected from cellulase, hemicellulase, amylase, pectinase, protease, tannase, amylobiase, xylanase, β-glucosidase or a combination thereof.

[0012] According to an embodiment of the first aspect of the present application, the decomposing enzyme comprises cellulase: pectinase: protease in a mass ratio of (1-10): (1-10): (0.5-1).

[0013] According to an embodiment of the first aspect of the present application, the decomposing enzyme comprises cellulase: pectinase: protease in a mass ratio of (1-5): (1-2):1.

[0014] According to an embodiment of the first aspect of the present application, the decomposing enzyme comprises cellulase:β-glucosidase:xylanase in a mass ratio of (1-10):(1-5):(0.5-3).

[0015] According to an embodiment of the first aspect of the present application, the decomposing enzyme includes cellulase, pectinase and protease in a mass ratio of 2:1:1.

[0016] According to an embodiment of the first aspect of the present application, the enzymatic hydrolysis product is heated to 80°C to 100°C for cyclic solid-liquid extraction for a first period of time and filtered to separate, thereby obtaining a first mixed solution.

[0017] According to an embodiment of the first aspect of the present application, the enzymatic hydrolysis product is heated to 80°C to 100°C and subjected to high-temperature magnetic stirring cyclic solid-liquid extraction for a first period of time and filtered to separate, thereby obtaining a first mixed solution.

[0018] According to an embodiment of the first aspect of the present application, the enzymatic hydrolysis product is heated to 80°C to 100°C for high-temperature magnetic stirring cyclic solid-liquid extraction for a first period of 1 hour to 5 hours.

[0019] According to an embodiment of the first aspect of the present application, the first extractant is selected from water or one or a mixture of methanol, ethanol, isopropanol, n-propanol, and isobutanol.

[0020] According to an embodiment of the first aspect of the present application, the mass ratio of the first mixed liquid to the first extractant is 1:(1-10).

[0021] According to an embodiment of the first aspect of the present application, the time for adding the first extractant to the first mixed liquid for sedimentation separation is 1 min to 60 min.

[0022] According to an embodiment of the first aspect of the present application, concentrating the supernatant into an extract comprises: clarifying the supernatant to obtain a transparent liquid; and concentrating and recovering the transparent liquid to obtain the extract.

[0023] According to an embodiment of the first aspect of the present application, the second extractant is selected from one of n-hexane, petroleum ether, ethyl acetate, and acetone, or a mixture of several of them.

[0024] According to the embodiment of the first aspect of the present application, a second extractant is added to the extract, and ultrasound-assisted dispersion is used to dynamically monitor low-temperature extraction, separation and purification to obtain a second mixed solution.

[0025] According to the embodiment of the first aspect of the present application, the extraction time of low-temperature extraction using ultrasound-assisted dispersion combined with dynamic monitoring is 5h to 72h.

[0026] According to the embodiment of the first aspect of the present application, the process conditions for adding the second extractant to the extract for extraction are: the mass ratio of the extract to the second extractant is 1:(1~100), the time of ultrasonic-assisted dispersion is 0.5h~5h, and the extraction temperature is 20℃~50℃.

[0027] According to an embodiment of the first aspect of the present application, removing the second extractant from the second mixed liquid includes: allowing the second mixed liquid to stand for stratification, taking the supernatant and concentrating and distilling it until no second extractant flows out, removing the second extractant from the second mixed liquid, and obtaining a first vanilla oily substance.

[0028] According to the embodiment of the first aspect of the present application, the seeds of vanilla are aggregated using supercritical CO 2 The extraction process includes: collecting the vanilla seeds and using supercritical CO 2 Extraction, the extraction pressure is 20MPa~35MPa, the temperature is 30℃~60℃, and the extraction time is 2h~10h; wherein, the pressure of the first separation kettle is 5MPa~12MPa, and the pressure of the second separation kettle is 2MPa~7MPa; the effluents of the first separation kettle and the second separation kettle are collected and filtered to obtain the second vanilla oily substance.

[0029] According to an embodiment of the first aspect of the present application, the method for preparing vanilla oil further includes: collecting and removing impurities from vanilla seeds, and retaining intact vanilla seeds as the first solid phase.

[0030] In a second aspect, the present application provides a vanilla oil-based substance, comprising: a first vanilla oil-based substance and a second vanilla oil-based substance in a mass ratio of (1~):(5~9).

[0031] In a third aspect, the present application provides a vanilla oil composition, comprising: the above-mentioned vanilla oil.

[0032] According to an embodiment of the third aspect of the present application, the vanilla oil accounts for 10 wt.% to 100 wt.% of the mass of the vanilla oil composition.

[0033] According to an embodiment of the third aspect of the present application, the vanilla oil composition further includes one or a combination of alcohol solvents, thickeners, suspending agents, vegetable oils, mineral oils, and antioxidants.

[0034] According to an embodiment of the third aspect of the present application, the vanilla oil composition further includes a first solid phase, wherein the first solid phase is vanilla seeds in supercritical CO 2 After the second vanilla oil is extracted, the whole vanilla seeds are collected and removed.

[0035] According to an embodiment of the third aspect of the present application, the mass of the first solid phase accounts for 0.5wt% to 10wt.% of the total mass of the vanilla oil composition.

[0036] According to an embodiment of the third aspect of the present application, the alcohol solvent is selected from 1,3-propylene glycol, glycerol, propylene glycol, butylene glycol, 1,2-butylene glycol, octyl dodecanol or a combination thereof.

[0037] According to an embodiment of the third aspect of the present application, the thickener is selected from carbomer 980, carbomer 941, acrylates / C10-30 alkyl acrylate crosspolymer, xanthan gum, carrageenan, dextrin palmitate, dextrin palmitate / ethylhexanoate, hydrogenated castor oil, PEG-30 hydrogenated castor oil or a combination thereof.

[0038] According to an embodiment of the third aspect of the present application, the suspending agent is selected from dibutyl ethylhexanoyl glutamine, dibutyl lauroyl glutamate, hydrogenated lecithin, PEG / PPG-17 / 6 copolymer or a combination thereof.

[0039] According to an embodiment of the third aspect of the present application, the vegetable oil is selected from jojoba oil, almond oil, sunflower seed oil, shea butter or a combination thereof.

[0040] According to an embodiment of the third aspect of the present application, the mineral oil is selected from caprylic / capric triglyceride, white oil, glyceryl polyether-26, neopentyl glycol diheptanoate or a combination thereof.

[0041] According to an embodiment of the third aspect of the present application, the antioxidant is selected from tocopherol acetate, tocopherol, BHT, BHA, TBHQ, ascorbyl palmitate, tea polyphenols, phytic acid or a combination thereof.

[0042] In a fourth aspect, the present application provides an application of the above-mentioned vanilla oil composition in the preparation of a care product, which is one of a lotion, cream, lotion, essence, gel, body milk, care oil, lipstick, and lip glaze.

[0043] According to an embodiment of the fourth aspect of the present application, the proportion of the vanilla oil composition in the care product is 0.01 wt.% to 20 wt.%.

[0044] The preparation method of vanilla oil in the embodiment of the present application comprises the steps of peeling the whole pods of vanilla into pods and seeds, extracting the first vanilla oily substance from the pods by enzymatic hydrolysis and using supercritical CO 2The second vanilla oily substance is extracted from the seeds by an extraction method, and the first vanilla oily substance and the second vanilla oily substance are mixed to prepare a vanilla oily substance with a relatively pure smell and beautiful color, thereby improving the full utilization rate of vanilla resources and further improving the yield rate of vanilla oily substances containing vanillin. In addition, the vanilla oily substance has the function of effectively promoting the repair of damaged cells. BRIEF DESCRIPTION OF THE DRAWINGS

[0045] In order to more clearly illustrate the technical solution of the embodiments of the present application, the following is a brief introduction to the drawings required for use in the embodiments of the present application. For ordinary technicians in this field, other drawings can be obtained based on these drawings without any creative work.

[0046] Figure 1 This is the ultraviolet absorption spectrum of vanilla oil 1 prepared by the method for preparing vanilla oil in Example 1 of the present application.

[0047] Figure 2 This is a comparison chart of the test results in the 3T3 cell scratch test without and with the vanilla oil substance 1 provided in Example 1 of the present application.

[0048] Figure 3 This is a physical picture of the gel care product containing vanilla oil composition 2 prepared in Example 9 of the present application. DETAILED DESCRIPTION

[0049] The features and exemplary embodiments of various aspects of the present application will be described in detail below. In order to make the purpose, technical solutions and advantages of the present application clearer, the present application will be further described in detail below in conjunction with the accompanying drawings and specific embodiments. It should be understood that the specific embodiments described herein are only intended to explain the present application, rather than to limit the present application. For those skilled in the art, the present application can be implemented without the need for some of these specific details. The following description of the embodiments is only to provide a better understanding of the present application by illustrating the examples of the present application.

[0050] It should be noted that, in this article, relational terms such as first and second, etc. are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Moreover, the terms "include", "comprise" or any other variants thereof are intended to cover non-exclusive inclusion, so that a process, method, article or device including a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to such process, method, article or device. In the absence of further restrictions, the elements defined by the statement "include..." do not exclude the presence of other identical elements in the process, method, article or device including the elements.

[0051] In order to solve the problems of the prior art, the present application provides a vanilla oil and a preparation method thereof, a composition and a use thereof, and a cosmetic. The preparation method of the vanilla oil provided in the present application is first introduced below.

[0052] Figure 1 A schematic flow chart of a method for preparing vanilla oil provided in one embodiment of the present application is shown.

[0053] First, as Figure 1 As shown, the present application provides a method for preparing vanilla oil, comprising: providing vanilla seeds and pods; extracting a first vanilla oily substance from the vanilla pods by enzymatic hydrolysis, comprising: refining the vanilla pods to obtain pod powder, and dispersing the pod powder with water to obtain a first dispersion; adding a decomposing enzyme to the first dispersion to perform enzymatic hydrolysis to obtain an enzymatic hydrolysis product; heating the enzymatic hydrolysis product to 80°C to 100°C for a first period of time for cyclic solid-liquid extraction and separation to obtain a first mixed solution; adding a first extractant to the first mixed solution for sedimentation separation to obtain a supernatant; concentrating the supernatant to an extract; adding a second extractant to the extract for extraction to obtain a second mixed solution; removing the second extractant from the second mixed solution to obtain a first vanilla oily substance; aggregating the vanilla seeds and using supercritical CO 2 The second vanilla oily substance is obtained by extraction treatment; and the vanilla oily substance is obtained by preparing the first vanilla oily substance and the second vanilla oily substance.

[0054] The method for preparing the vanilla oily substance in the embodiment of the present application comprises the steps of: peeling the whole vanilla pods into pods and seeds, respectively extracting the first vanilla oily substance from the pods by enzymatic hydrolysis and extracting the second vanilla oily substance from the pods by supercritical CO 2The extraction method extracts the second vanilla oil from the seeds, and the first vanilla oil and the second vanilla oil are mixed to prepare a vanilla oil with a relatively pure smell and beautiful color, thereby improving the full utilization rate of vanilla resources and further improving the yield of vanilla oil containing vanillin, and the vanilla oil has the effect of promoting the repair of damaged cells.

[0055] In some embodiments of the present application, providing vanilla seeds and pods includes peeling vanilla pods and seeds in the physiological maturity stage and placing them separately to provide vanilla seeds and pods. The vanilla pods are complete vanilla pods in the physiological maturity stage, which contain pods and seeds and can be obtained through commercial channels. The complete vanilla pods are preferably fresh vanilla pods in the physiological maturity stage.

[0056] The preparation method of the vanilla oily substance of the embodiment of the present application comprises the following steps: separating the vanilla pods and seeds, subjecting the pods to enzymatic hydrolysis products obtained by enzymatic hydrolysis, performing cyclic solid-liquid extraction for a first period of time and separating to obtain a first mixed solution, and then subjecting the first mixed solution containing vanillin to sedimentation, impurity removal, and extraction separation to obtain a first vanilla oily substance; and combining supercritical CO 2 with the method of preparing the vanilla oily substance without destroying the appearance of the vanilla seeds as much as possible. 2 The extraction method extracts and prepares the second vanilla oil from the seeds, and the first vanilla oil and the second vanilla oil are compounded to obtain a vanilla oil with a relatively pure smell and beautiful color. Compared with the existing vanilla extract extraction method, the yield of the vanilla oil containing vanillin extracted from vanilla can be effectively improved, and the full utilization rate of vanilla resources is also improved.

[0057] In some embodiments of the present application, refining the vanilla pods includes: grinding or ultrasonically crushing the vanilla pods to obtain pod powder with a particle size of ≤1000 μm. Exemplarily, the vanilla pods can be ground by pounding, ball milling, or ultrasonic crushing to obtain pod powder with a particle size of ≤1000 μm. In the embodiments of the present application, refining the vanilla pods into pod powder with a particle size of ≤1000 μm is beneficial for the pod powder to fully contact with the decomposition enzyme, and then be enzymatically hydrolyzed by the decomposition enzyme to release the first vanilla oily substance in the pod powder.

[0058] Exemplarily, the particle size of the bean pod powder can be 200, 300, 400, 450, 500, 600, 700, 750, 800, 900 μm. The smaller the particle size of the bean pod powder, the more conducive it is for the decomposition enzyme to fully contact with the bean pod powder, and then release the first vanilla oil contained therein through enzymatic hydrolysis. It is also beneficial for the first vanilla oil to escape from the enzymatic hydrolysis product (including the bean pod powder that has not been decomposed by the decomposition enzyme and the bean pod powder that has been decomposed by the decomposition enzyme) during the subsequent enzymatic hydrolysis product heating to 80°C to 100°C for circulating liquid extraction and separation, thereby improving the yield of the vanilla oil after the first period of circulating solid-liquid extraction and separation, and after subsequent treatment steps.

[0059] In some embodiments, dispersing the bean pod powder with water includes: adding water 1 to 20 times the mass of the bean pod powder to the bean pod powder to obtain a first dispersion. Exemplarily, the mass ratio of the bean pod powder to water is 1:2, 1:3, 1:5, 1:7, 1:9, 1:11, 1:14, 1:15, 1:16, 1:18, 1:19.

[0060] In some embodiments of the present application, adding a decomposing enzyme to the first dispersion for enzymatic hydrolysis treatment includes: adjusting the pH value of the first dispersion to 3.0-7.0, adding a decomposing enzyme and performing enzymatic hydrolysis treatment at 40°C-80°C for 2h-6h. Exemplarily, adding a decomposing enzyme to the first dispersion can be performed at 45°C, 8°C, 50°C, 55°C, 60°C, 66°C, 70°C, 72°C, 75°C, 78°C, and 80°C for enzymatic hydrolysis treatment, so that the bean pod powder of the dispersion is fully enzymatically hydrolyzed by the decomposing enzyme to obtain a component containing vanilla oil.

[0061] The method for preparing vanilla oil in the embodiment of the present application prepares vanilla oil by an aqueous enzymatic method, which can prepare vanilla oil with a relatively pure smell and beautiful color, and increase the yield of vanilla oil.

[0062] In some embodiments of the present application, a decomposing enzyme is added to the first dispersion in an amount of 0.01 g / kg to 15 g / kg. For example, 0.02 g, 0.03 g, 0.05 g, 0.08 g, 0.1 g, 1 g, 1.2 g, 1.5 g, 1.8 g, 2 g, 2.2 g, 2.5 g, 2.8 g, 3 g, 3.5 g, 3.75 g, 4 g, 4.5 g, 5 g, 5.4 g, 6 g, 6.4 g, 7 g, 7.2 g, 7.5 g, 8 g, 9 g, 9.3 g, 9.5 g, 9.6 g, 10 g, 11 g, 12 g, 13 g, 14 g, 14.8 g, 15 g of the decomposing enzyme can be added to each kilogram of the first dispersion.

[0063] In some embodiments of the present application, the degrading enzyme is selected from cellulase, hemicellulase, amylase, pectinase, protease, tannase, amylobiase, xylanase, β-glucosidase or a combination thereof.

[0064] In some embodiments of the present application, the decomposition enzyme includes cellulase: pectinase: protease in a mass ratio of (1-10): (1-10): (0.5-1). Compared with using only a single type of decomposition enzyme, the decomposition enzyme meeting this ratio can improve the yield of vanilla oil.

[0065] In some embodiments of the present application, the decomposition enzyme includes cellulase: pectinase: protease in a mass ratio of (1-5): (1-2): 1. The decomposition enzyme meeting this ratio can improve the yield of vanilla oil compared with using only a single type of decomposition enzyme.

[0066] In some embodiments of the present application, the decomposition enzyme includes cellulase:β-glucosidase:xylanase in a mass ratio of (1-10):(1-):(0.5-3). The decomposition enzyme meeting this ratio can effectively improve the yield of vanilla oil.

[0067] In some embodiments of the present application, the decomposition enzymes include cellulase, pectinase and protease in a mass ratio of 2:1:1. Compared with using only a single type of decomposition enzyme, the decomposition enzymes meeting this ratio can effectively improve the yield of vanilla oil.

[0068] In some embodiments of the present application, the enzymatic hydrolysis product is heated to 80° C. to 100° C., subjected to cyclic solid-liquid extraction for a first period of time, and filtered and separated to obtain a first mixed solution.

[0069] In an embodiment of the present application, heating the enzymatic hydrolysate to 80°C to 100°C for a first period of time for cyclic solid-liquid extraction and filtration separation means adding water to the enzymatic hydrolysate and heating it to 80°C to 100°C for sealing, and continuously extracting the solid phase and the liquid phase at a certain speed for a first period of time and filtering and separating, and then obtaining a first mixed solution free of bean pod powder residue. Exemplarily, the enzymatic hydrolysate can be heated to 83°C, 85°C, 88°C, 90°C, 92°C, 95°C, -7°C, 98°C for cyclic solid-liquid extraction and separation.

[0070] The method for preparing vanilla oil in the embodiment of the present application heats the enzymatic hydrolysis product to 80°C to 100°C for cyclic solid-liquid extraction and separation, which not only effectively inactivates the decomposing enzyme, but also utilizes the principle of enhanced thermal motion of vanilla oil at high temperature to enable the first vanilla oil to escape from the enzymatic hydrolysis product during continuous extraction and under high temperature environment, and then be extracted by water, thereby improving the yield of the vanilla oil.

[0071] The preparation method of the vanilla oily substance in the embodiment of the present application provides a method for extracting vanilla oily substances that is different from the existing method for extracting vanilla oily substances. No further processing of the vanilla pod raw materials is required, such as no freeze-thaw treatment of the vanilla. The vanilla pods only need to be refined into the pod powder of the above-mentioned limited particle size and combined with subsequent enzymatic hydrolysis treatment and heating the enzymatic hydrolysis product to 80°C to 100°C for a first period of time for cyclic solid-liquid extraction and separation. In this way, a product containing the first vanilla oily substance can be efficiently prepared from the pod powder, and the extraction yield of the first vanilla oily substance can be improved.

[0072] In an embodiment of the present application, the enzymatic hydrolysis product is heated to 80°C to 100°C and water is used as an extractant to perform cyclic solid-liquid extraction for a first period of time and filtered to separate the obtained liquid as the extraction product, i.e., the first mixed liquid.

[0073] In some embodiments of the present application, the enzymatic hydrolysis product is heated to 80° C. to 100° C., subjected to high-temperature magnetic stirring cyclic solid-liquid extraction for a first period of time, and filtered for separation to obtain a first mixed solution.

[0074] In some embodiments of the present application, the first time length of heating the hydrolyzate to 80°C to 100°C for high-temperature magnetic stirring circulation solid-liquid extraction is 1h to 5h. Exemplarily, the hydrolyzate can be heated to 82°C, 85°C, 88°C, 90°C, 93°C, 95°C, 98°C, and 99°C, and the time for high-temperature magnetic stirring circulation solid-liquid extraction is 1.2, 1.5, 1.8, 2.0, 2.4, 2.5, 2.8, 3.0, 3.2, 3.5, 3.6, 4.0, 4.5, 4.6, 4.8, 4.9h. In an embodiment of the present application, the hydrolyzate is heated to 80°C to 100°C for high-temperature magnetic stirring circulation solid-liquid extraction for 1h to 5h, so that the first vanilla oil can be fully extracted from the hydrolyzate, thereby improving the yield of vanilla oil, and obtaining the first mixed solution after filtration and separation.

[0075] In the embodiments of the present application, the above-mentioned thinning treatment and enzymatic hydrolysis treatment are performed on the vanilla pods to improve the yield of the vanilla oil.

[0076] In some embodiments of the present application, the first extractant is selected from water or one or more of methanol, ethanol, isopropanol, n-propanol, and isobutanol. In the embodiments of the present application, the first extractant is used to remove turbidity and colloidal particles in the first mixed liquid, making the liquid clear and transparent, thereby improving the quality of the first vanilla oil.

[0077] In some embodiments of the present application, the mass ratio of the first mixed liquid to the first extractant is 1:(1-10). Exemplarily, the mass ratio of the first mixed liquid to the first extractant is 1:2, 1:3, 1:5, 1:7, 1:8, 1:9.

[0078] In some embodiments of the present application, the time for adding the first extractant to the first mixed liquid for sedimentation separation is 1 min to 60 min.

[0079] In some embodiments of the present application, concentrating the supernatant into an extract comprises: clarifying the supernatant to obtain a transparent liquid; and concentrating and recovering the transparent liquid to obtain the extract.

[0080] In some embodiments of the present application, the second extractant is selected from one of n-hexane, petroleum ether, ethyl acetate, and acetone, or a mixture of several of them.

[0081] In some embodiments of the present application, a second extractant is added to the extract, and ultrasonic dispersion combined with dynamic monitoring of low-temperature extraction, separation and purification are used to obtain a second mixed solution.

[0082] In some embodiments of the present application, the extraction time of ultrasonic-assisted dispersion combined with monitoring low-temperature extraction is 5 to 72 hours. For example, it can be 8, 12, 18, 25, 30, 36, 40, 48, 54, 60, 64, 68, or 70 hours.

[0083] In some embodiments of the present application, the process conditions for adding the second extractant to the extract for extraction are: the mass ratio of the extract to the second extractant is 1: (1-100), the time of ultrasonic assisted dispersion is 0.5h-5h, and the extraction temperature is 20° C.-50° C. Exemplarily, the mass ratio of the extract to the second extractant is 1:2, 1:3, 1:5, 1:8, 1:10, 1:12, 1:15, 1:20, 1:24, 1:28, 1:30, 1:35, 1:38, 1:40, 1:42, 1:45, 1:48, 1:50, 1:55, 1:60, 1:64, 1:67, 1:70, 1:72, 1:75, 1:80, 1:85, 1:90, 1:93, 1:97.

[0084] Compared with the reflux extraction method in the prior art, the embodiment of the present application uses a high-pressure homogenizer to uniformly mix the extract and n-hexane, and uses ultrasound to assist in further dispersion, so that the extract and n-hexane can be more fully in contact, and then a shaking table is used for dynamic monitoring of low-temperature extraction, that is, a shaking table is used to oscillate to achieve dynamic monitoring of low temperature (20°C to 50°C), and extract at a suitable extraction speed and extraction time to obtain a first oily substance mixture. Optionally, in some embodiments, the temperature of the low-temperature extraction can be 25°C, 30°C, 32°C, 35°C, 40°C, 45°C, 48°C, or 50°C.

[0085] In some embodiments of the present application, removing the second extractant from the second mixed liquid includes: allowing the second mixed liquid to stand for stratification, taking the supernatant and concentrating and distilling until no second extractant flows out, removing the second extractant from the second mixed liquid, and obtaining a first vanilla oily substance.

[0086] In an embodiment of the present application, a first mixed liquid is added to a first extractant for sedimentation separation to obtain a supernatant, and the supernatant is concentrated into an extract, and then a second extraction solvent is used for extraction and the second extraction solvent in the extract product is removed, so that the first vanilla oily substance can be efficiently obtained, thereby improving the preparation efficiency of the vanilla oily substance including the second vanilla oily substance.

[0087] In some embodiments of the present application, the seeds of vanilla are aggregated using supercritical CO 2 The extraction process includes: collecting the vanilla seeds and using supercritical CO 2 Extraction, extraction pressure is 20MPa~35MPa, temperature is 30℃~60℃, extraction time is 2h~10h; wherein, the pressure of the first separation kettle is 5MPa~12MPa, and the pressure of the second separation kettle is 2MPa~7MPa; collect the effluent of the first separation kettle and the second separation kettle and filter to obtain the second vanilla oily substance. Wherein, the seeds of vanilla are gathered, that is, the seeds of vanilla are collected and placed together for standby. Extracting the second vanilla oily substance from the seeds of vanilla can improve the yield of vanilla oily substances and make full use of vanilla resources. Exemplarily, the extraction pressure can be 22MPa, 24MPa, 25MPa, 28MPa, 30MPa, 32MPa, 34MPa, the pressure of the first separation kettle can be 6MPa, 8MPa, 10MPa, 11MPa, and the pressure of the second separation kettle can be 3MPa, 5MPa, 6MPa.

[0088] In some embodiments of the present application, the method for preparing vanilla oil further comprises: using supercritical CO 2 The vanilla seeds after the second vanilla oily substance is extracted are collected and impurities are removed, and the intact vanilla seeds are retained as the first solid phase.

[0089] In the embodiments of the present application, the first solid phase is mixed with the vanilla oil, which not only has the efficacy of the vanilla oil itself, but also can be suspended in the cosmetics through the first solid phase to improve the aesthetics of the product.

[0090] The method for preparing the vanilla oily substance in the embodiment of the present application can increase the yield of the vanilla oily substance while increasing the content of vanillin in the vanilla oily substance.

[0091] In a second aspect, the present application provides a vanilla oily substance, comprising: a first vanilla oily substance and a second vanilla oily substance in a mass ratio of (1 to): (5 to 9). Exemplarily, the mass ratio of the first vanilla oily substance to the second vanilla oily substance may be 1:6, 1:7, 1:8, 2:5, 2:7, 2:9, 3:5, 3:7, 3:8, 4:5, 4:7, 4:9, 5:6, 5:7, 5:8.

[0092] In a third aspect, the present application provides a vanilla oil composition, comprising: the above-mentioned vanilla oil.

[0093] In some embodiments of the present application, in the vanilla oil composition, the vanilla oil accounts for 10 wt.% to 100 wt.% of the mass of the vanilla oil composition.

[0094] Exemplarily, the vanilla oily substance accounts for 11 wt.%, 11.5 wt.%, 12 wt.%, 12.3 wt.%, 12.5 wt.%, 13 wt.%, 13.6 wt.%, 14 wt.%, 14.8 wt.%, 15 wt.%, 15.4 wt.%, 16 wt.%, 16.8 wt.%, 17.5 wt.%, 18 wt.%, 18.4 wt.%, 19 wt.%, 19.6 wt.%, 20 wt.%, 20.5 wt.%, 21.7 wt.%, 22 wt.%, 23.2 wt.%, 24 wt.%, 24.5 wt.% of the mass of the vanilla oily substance composition. , 25wt.%, 26wt.%, 27.4wt.%, 28wt.%, 30wt.%, 40wt.%, 42wt.%, 45wt.%, 48wt.%, 50wt.%, 52wt.%, 55wt.%, 56wt.%, 58wt.%, 60wt.%, 63wt. %, 65wt.%, 69wt.%, 70wt.%, 72wt.%, 74wt.%, 75wt.%, 78wt.%, 80wt.%, 83wt.%, 85wt.%, 88wt.%, 90wt.%, 93wt.%, 95wt.%, 98wt.%, 98wt.%.

[0095] In some embodiments of the present application, the vanilla oil composition further comprises: an alcohol solvent, a thickener, a suspending agent, a vegetable oil, a mineral oil, an antioxidant, or a combination of several thereof.

[0096] In the embodiments of the present application, the alcohol solvent, thickener, suspending agent, vegetable oil, mineral oil, and antioxidant of the vanilla oil composition can be added in appropriate amounts according to the specific product.

[0097] In some embodiments of the present application, the alcohol solvent is selected from 1,3-propylene glycol, glycerol, propylene glycol, butylene glycol, 1,2-butylene glycol, octyldodecanol or a combination thereof to fully disperse the vanilla oil.

[0098] In some embodiments of the present application, the thickener is selected from Carbomer 980, Carbomer 941, acrylates / C10-30 alkyl acrylate crosspolymer, xanthan gum, carrageenan, dextrin palmitate, dextrin palmitate / ethylhexanoate, hydrogenated castor oil, PEG-30 hydrogenated castor oil, or a combination thereof, so that the vanilla oil composition has a suitable viscosity.

[0099] In some embodiments of the present application, the suspending agent is selected from dibutyl ethylhexanoyl glutamine, dibutyl lauroyl glutamate, hydrogenated lecithin, PEG / PPG-17 / 6 copolymer or a combination thereof.

[0100] In some embodiments of the present application, the vegetable oil is selected from jojoba oil, almond oil, sunflower oil, shea butter or a combination thereof.

[0101] In some embodiments of the present application, the mineral oil is selected from caprylic capric triglyceride, white oil, glyceryl polyether-26, neopentyl glycol diheptanoate or a combination thereof.

[0102] In some embodiments of the present application, the antioxidant is selected from tocopheryl acetate, tocopherol, BHT, BHA, TBHQ, ascorbyl palmitate, tea polyphenols, phytic acid or a combination thereof.

[0103] In some embodiments of the present application, the vanilla oil composition further comprises a first solid phase, wherein the first solid phase is vanilla seeds in supercritical CO 2 After the second vanilla oil is extracted, the whole vanilla seeds are collected and removed.

[0104] In some embodiments of the present application, the mass proportion of the first solid phase in the vanilla oil composition is 0.5 wt.% to 10 wt.%.

[0105] The first solid phase in the composition of the vanilla oily substance of the embodiment of the present application, i.e., the extracted vanilla seeds, can be recycled and combined with the vanilla oily substance to prepare the vanilla oily substance composition, which not only has the efficacy of the vanilla oily substance, but also, when the vanilla oily substance composition is added to the finished cosmetic product, the vanilla seed particles are suspended in the cosmetic product, which not only has the efficacy of the vanilla oily substance in promoting cell damage repair, but also can improve the aesthetics of the cosmetic product containing the composition. 2 The product after extracting the second vanilla oily substance is used as the first solid phase, which can further improve the utilization rate of vanilla resources.

[0106] In a fourth aspect, the present application provides an application of a vanilla oil composition in the preparation of a care product, wherein the content of the vanilla oil composition is 0.01wt.% to 20wt.%. For example, the content of the vanilla oil composition may be 0.05wt.%, 0.1wt.%, 0.3wt.%, 0.5wt.%, 0.8wt.%, 1wt.%, 2.5wt.%, 3wt.%, 4wt.%, 6wt.%, 8wt.%, 10wt.%, 11wt.%, 12wt.%, 14wt.%, 15wt.%, 16wt.%, 18wt.%, 18.4wt.%, 19wt.%, 19.5wt.%.

[0107] In an embodiment of the present application, the care product may be a skin care product or a body care product. Exemplarily, the care product is one of lotion, cream, toner, essence, gel, body milk, care oil, lipstick, and lip glaze.

[0108] The advantages of the present application are further illustrated by specific examples and comparative examples. In both the examples and comparative examples, a polypropylene membrane with a thickness of 10 μm is used as the microfiltration membrane.

[0109] Example 1

[0110] A method for preparing a vanilla oily substance comprises: providing vanilla seeds and pods, including peeling off the vanilla pods and seeds in a mature stage and placing them separately to provide vanilla seeds and pods; extracting a first vanilla oily substance from the vanilla pods, comprising:

[0111] S1. Crush and ball-mill the vanilla pods to obtain pod powder with a particle size of 800 μm; weigh 100 g of the pod powder, add 2000 g of water and stir evenly to prepare a first dispersion;

[0112] S2, adjusting the pH value of the first dispersion to 5.0, adding 6 g of cellulase to the first dispersion, and performing enzymolysis treatment at 50° C. for 3 h to obtain an enzymolysis product;

[0113] S3, raising the temperature of the enzymatic hydrolyzate to 90° C., performing high-temperature magnetic stirring, and using water circulation for solid-liquid extraction for 2 h, filtering, and centrifuging at a speed of 1000 r / min for 15 min to obtain a first mixed solution;

[0114] S4. Add 2000 g of 95% ethanol to the first mixed solution, stir and mix until flocculent precipitation occurs. Settle and stand for 30 minutes, filter, and take the supernatant liquid on the upper layer;

[0115] S5, concentrating the supernatant until no ethanol flows out to obtain an extract;

[0116] S6, adding 50 g of water to the extract to rinse it completely, adding 200 g of n-hexane to perform ultrasonic mixing for 30 min, and then using a shaker to perform oscillation extraction for 12 h at an extraction temperature of 30° C. to obtain a second mixed solution;

[0117] S7, removing the n-hexane from the upper layer of the second mixed solution, i.e., concentrating until no n-hexane flows out, to obtain a first vanilla oily substance;

[0118] S8. Gather the vanilla seeds and use supercritical CO 2 Extraction, extraction pressure is 35MPa, temperature is 50℃, extraction time is 3h; wherein, the pressure of the first separation kettle is 11MPa, and the pressure of the second separation kettle is 6MPa; the effluents of the first separation kettle and the second separation kettle are collected and filtered to obtain the second vanilla oily substance. wherein, the extracted vanilla seeds are collected and impurities are removed, and the intact vanilla seeds are retained as the first solid phase for standby use.

[0119] S9, preparation of vanilla oily substance: weigh 70 g of the second vanilla oily substance, add it to 30 g of the first vanilla oily substance, stir and ultrasonically mix evenly, filter with a microfiltration membrane, and the obtained liquid is vanilla oily substance 1.

[0120] Example 2

[0121] A method for preparing vanilla oily substances comprises: providing vanilla seeds and pods, including peeling off the pods and seeds of vanilla in a mature stage and placing them separately to provide vanilla seeds and pods; extracting a first vanilla oily substance from the vanilla pods, comprising:

[0122] S1. Crush and ball-mill the vanilla pods to obtain pod powder with a particle size of 800 μm; weigh 100 g of the pod powder, add 500 g of water and stir evenly to prepare a first dispersion;

[0123] S2, adjusting the pH value of the first dispersion to 4.0, adding 1 g of pectinase to the first dispersion, and performing enzymolysis treatment at 45° C. for 3 h to obtain an enzymolysis product;

[0124] S3, raising the temperature of the enzymatic hydrolyzate to 90° C., performing high-temperature magnetic stirring, and using water circulation for solid-liquid extraction for 3 h, filtering, and centrifuging at a speed of 10,000 r / min for 15 min to obtain a first mixed solution;

[0125] S4, add 1500g of isopropanol to the first mixed solution, stir and mix until flocculent precipitation occurs. Separate for 30min of settling, filter, and take the supernatant on the upper layer;

[0126] S5, concentrating the supernatant until no isopropanol flows out, to obtain an extract;

[0127] S6, adding 50 g of water to the extract to rinse it completely, adding 200 g of n-hexane to perform ultrasonic mixing for 30 min, and then using a shaker to perform oscillation extraction for 20 h at an extraction temperature of 30° C. to obtain a second mixed solution;

[0128] S7, removing the n-hexane from the upper layer of the second mixed solution, i.e., concentrating until no n-hexane flows out, to obtain a first vanilla oily substance;

[0129] S8. Gather the vanilla seeds and use supercritical CO 2 Extraction, extraction pressure is 30MPa, temperature is 60℃, extraction time is 3h; wherein, the pressure of the first separation kettle is 10MPa, and the pressure of the second separation kettle is 6MPa; the effluents of the first separation kettle and the second separation kettle are collected and filtered to obtain the second vanilla oily substance. wherein, the extracted vanilla seeds are collected and impurities are removed, and the intact vanilla seeds are retained as the first solid phase for standby use.

[0130] S9, preparation of vanilla oily substance: weigh 50 g of the second vanilla oily substance, add it to 50 g of the first vanilla oily substance, stir and ultrasonically mix evenly, filter with a microfiltration membrane, and the obtained liquid is vanilla oily substance 2.

[0131] Example 3

[0132] A method for preparing vanilla oily substances comprises: providing vanilla seeds and pods, including peeling off the pods and seeds of vanilla in a mature stage and placing them separately to provide vanilla seeds and pods; extracting a first vanilla oily substance from the vanilla pods, comprising:

[0133] S1. Crush and ball-mill the vanilla pods to obtain pod powder with a particle size of 800 μm; weigh 100 g of the pod powder, add 1000 g of water and stir evenly to prepare a first dispersion;

[0134] S2, adjusting the pH value of the first dispersion to 5.0, adding 6g of cellulase, 3g of protease and 3g of pectinase to the first dispersion, and performing enzymolysis treatment at 50°C for 3h to obtain an enzymolysis product;

[0135] S3, raising the temperature of the enzymatic hydrolyzate to 90° C., performing high-temperature magnetic stirring, and using water circulation for solid-liquid extraction for 2 h, filtering, and centrifuging at a speed of 10,000 r / min for 15 min to obtain a first mixed solution;

[0136] S4, add 3000g of 95% ethanol to the first mixed solution, stir and mix until flocculent precipitation occurs. Settle and stand for 30 minutes, filter, and take the supernatant liquid on the upper layer;

[0137] S5, concentrating the supernatant until no ethanol flows out to obtain an extract;

[0138] S6, adding 50 g of water to the extract to rinse it completely, adding 300 g of n-hexane to perform ultrasonic mixing for 30 min, and then using a shaker to perform oscillation extraction for 24 h at an extraction temperature of 30° C. to obtain a second mixed solution;

[0139] S7, removing the n-hexane from the upper layer of the second mixed solution, i.e., concentrating until no n-hexane flows out, to obtain a first vanilla oily substance;

[0140] S8. Gather the vanilla seeds and use supercritical CO 2 Extraction, extraction pressure is 30MPa, temperature is 60℃, extraction time is 3h; wherein, the pressure of the first separation kettle is 10MPa, and the pressure of the second separation kettle is 6MPa; the effluents of the first separation kettle and the second separation kettle are collected and filtered to obtain the second vanilla oily substance. wherein, the extracted vanilla seeds are collected and impurities are removed, and the intact vanilla seeds are retained as the first solid phase for standby use.

[0141] S9, preparation of vanilla oily substance: weigh 90 g of the second vanilla oily substance, add it to 10 g of the first vanilla oily substance, stir and mix evenly by ultrasonication, filter with a microfiltration membrane, and the obtained liquid is vanilla oily substance 3.

[0142] Example 4

[0143] A method for preparing vanilla oily substances comprises: providing vanilla seeds and pods, including peeling off the pods and seeds of vanilla in a mature stage and placing them separately to provide vanilla seeds and pods; extracting a first vanilla oily substance from the vanilla pods, comprising:

[0144] S1. Crush and ball-mill the vanilla pods to obtain pod powder with a particle size of 800 μm; weigh 100 g of the pod powder, add 1000 g of water and stir evenly to prepare a first dispersion;

[0145] S2, adjusting the pH value of the first dispersion to 5.0, adding 6g of cellulase, 3g of protease and 2g of pectinase to the first dispersion, and performing enzymolysis treatment at 50°C for 3h to obtain an enzymolysis product;

[0146] S3, raising the temperature of the enzymatic hydrolyzate to 90° C., performing high-temperature magnetic stirring, and using water circulation for solid-liquid extraction for 2 h, filtering, and centrifuging at a speed of 10,000 r / min for 15 min to obtain a first mixed solution;

[0147] S4, add 3000g of 95% ethanol to the first mixed solution, stir and mix until flocculent precipitation occurs. Settle and stand for 30 minutes, filter, and take the supernatant liquid on the upper layer;

[0148] S5, concentrating the supernatant until no ethanol flows out to obtain an extract;

[0149] S6, adding 50 g of water to the extract to rinse it completely, adding 300 g of n-hexane to perform ultrasonic mixing for 30 min, and then using a shaker to perform oscillation extraction for 8 h at an extraction temperature of 30° C. to obtain a second mixed solution;

[0150] S7. Taking the upper layer of the second mixed liquid and removing the n-hexane, i.e. concentrating until no n-hexane flows out, to obtain the first vanilla oily substance.

[0151] S8. Gather the vanilla seeds and use supercritical CO 2 Extraction, extraction pressure is 30MPa, temperature is 60℃, extraction time is 3h; wherein, the pressure of the first separation kettle is 10MPa, and the pressure of the second separation kettle is 6MPa; the effluents of the first separation kettle and the second separation kettle are collected and filtered to obtain the second vanilla oily substance. wherein, the extracted vanilla seeds are collected and impurities are removed, and the intact vanilla seeds are retained as the first solid phase for standby use.

[0152] S9, preparation of vanilla oily substance: weigh 50 g of the second vanilla oily substance and add it to 50 g of the first vanilla oily substance, stir and mix evenly by ultrasonication, filter with a microfiltration membrane, and the obtained liquid is vanilla oily substance 4.

[0153] Example 5

[0154] A method for preparing vanilla oily substances comprises: providing vanilla seeds and pods, including peeling off the pods and seeds of vanilla in a mature stage and placing them separately to provide vanilla seeds and pods; extracting a first vanilla oily substance from the vanilla pods, comprising:

[0155] S1. Crush and ball-mill the vanilla pods to obtain pod powder with a particle size of 800 μm; weigh 100 g of the pod powder, add 1000 g of water and stir evenly to prepare a first dispersion;

[0156] S2, adjusting the pH value of the first dispersion to 5.0, adding 2 g of cellulase, 2 g of β-glucanase and 1 g of xylanase to the first dispersion, and performing enzymolysis treatment at 50° C. for 3 h to obtain an enzymolysis product;

[0157] S3, raising the temperature of the enzymatic hydrolyzate to 90° C., performing high-temperature magnetic stirring, and using water circulation for solid-liquid extraction for 2 h, filtering, and centrifuging at a speed of 10,000 r / min for 15 min to obtain a first mixed solution;

[0158] S4, add 3000g of 95% ethanol to the first mixed solution, stir and mix until flocculent precipitation occurs. Settle and stand for 30 minutes, filter, and take the supernatant liquid on the upper layer;

[0159] S5, concentrating the supernatant until no ethanol flows out to obtain an extract;

[0160] S6, adding 50 g of water to the extract to rinse it completely, adding 300 g of n-hexane to perform ultrasonic mixing for 30 min, and then using a shaker to perform oscillation extraction for 8 h at an extraction temperature of 30° C. to obtain a second mixed solution;

[0161] S7. Taking the upper layer of the second mixed liquid and removing the n-hexane, i.e. concentrating until no n-hexane flows out, to obtain the first vanilla oily substance.

[0162] S8. Gather the vanilla seeds and use supercritical CO 2 Extraction, extraction pressure is 30MPa, temperature is 60℃, extraction time is 3h; wherein, the pressure of the first separation kettle is 10MPa, and the pressure of the second separation kettle is 6MPa; the effluents of the first separation kettle and the second separation kettle are collected and filtered to obtain the second vanilla oily substance. wherein, the extracted vanilla seeds are collected and impurities are removed, and the intact vanilla seeds are retained as the first solid phase for standby use.

[0163] S9, preparation of vanilla oily substance: weigh 50 g of the second vanilla oily substance and add it to 50 g of the first vanilla oily substance, stir and mix evenly by ultrasonication, filter with a microfiltration membrane, and the obtained liquid is vanilla oily substance 5.

[0164] Comparative Example 1

[0165] Crush 100g of vanilla, add 2000g of water, stir evenly, adjust the pH to 4, maintain at 45℃ for 3h, increase the temperature to 90℃, extract for 3h, filter, centrifuge at a speed of 10000r / min and a centrifugal time of 15min, take the supernatant, add 1500g of isopropanol, stir and mix until flocculent precipitate appears, let it settle and stand for 30min, take the upper layer liquid, concentrate until no isopropanol flows out, add 50g of water, rinse completely, mix with the upper layer precipitate A, add 200g of n-hexane, ultrasonically mix for 30min, shake and extract overnight, take the upper layer liquid and concentrate until no n-hexane flows out to obtain vanilla oily substance.

[0166] Comparative Example 2

[0167] Crush 100 g of vanilla, add 500 g of water, stir evenly, adjust the pH to 4, maintain at 50 ° C for 3 h, increase the temperature to 95 ° C, extract for 3 h, filter, centrifuge at a speed of 10000 r / min, centrifuge for 15 min, take the supernatant, add 1500 g of isopropanol, stir and mix until flocculent precipitate appears, let it settle and stand for 30 min, take the upper layer liquid, concentrate until no isopropanol flows out, add 50 g of water, rinse completely, mix with the upper precipitate A, add 200 g of n-hexane, ultrasonically mix for 30 min, shake and extract overnight, take the upper layer liquid and concentrate until no n-hexane flows out to obtain vanilla oily substance.

[0168] 1. Calculation formula for the yield of vanilla oil

[0169] The yield of vanilla oil is calculated according to the following formula (1):

[0170] Yield (%) = amount of vanilla oil / mass of vanilla*100% (1).

[0171] Table 1

[0172]

[0173]

[0174] It can be concluded from Table 1 that the preparation method of the vanilla oily substance of the examples of the present application can more efficiently extract the vanilla oily substance from the whole vanilla pods, and the yield of the vanilla oily substance can be increased by 1.01% to 5.36% on the existing basis (the yields of the vanilla oily substances in Examples 1-5 are calculated based on the yield of Comparative Example 1).

[0175] 2. GC-MS determination of the vanilla oily substance 3 prepared in Example 3

[0176] GC-MS test method

[0177] 1.1 Chromatographic reference conditions

[0178] GC conditions

[0179] Capillary column: DB-WAX, column length 60m, inner diameter 0.25mm, film thickness 0.25μm. Injector temperature: 250℃.

[0180] Program temperature rise: initial temperature 80°C, lasting 1 min;

[0181] 80℃~180℃, heating rate 20℃ / min;

[0182] 180℃~220℃, heating rate 10℃ / min;

[0183] 220℃~240℃, heating rate 1℃ / min, hold for 5min.

[0184] Carrier gas: nitrogen. Split ratio: 40:1. Injection volume: 1.0 μL. Flow rate: 1 mL / min. Detection conditions should meet the theoretical plate number (n) of at least 2000 / m and the resolution (R) of at least 1.25.

[0185] MS conditions:

[0186] Ionization mode: EI; electron energy: 70 eV; transfer line temperature: 290 °C; ion source temperature: 230 °C; quadrupole temperature: 150 °C; mass range: 50-600.

[0187] 1.2 Sample determination

[0188] 10 μl of vanilla oil 3 was dissolved in 990 μl of isooctane and filtered through a 0.22 μm nylon membrane to obtain a sample solution. The sample solution prepared from the vanilla oil 3 prepared in Example 3 was injected into a gas chromatograph under the above chromatographic conditions and quantified by the peak area of ​​the chromatographic peak.

[0189] 1.3 Analysis results using area normalization method

[0190]

[0191] In formula (2):

[0192] Y i ——The percentage of a certain fatty acid in the sample to the total fatty acids, %;

[0193] A si ——Peak area of ​​each fatty acid methyl ester in the sample solution;

[0194] F FAMEi-FAi ——The conversion coefficient of fatty acid methyl ester i into fatty acids, see Appendix D;

[0195] ∑A si ——The sum of the peak areas of each fatty acid methyl ester in the sample solution.

[0196] The calculation result shall be rounded to 3 significant figures.

[0197] Table 2 Ingredients of the vanilla oil of Example 3

[0198] Element % Hexacosane 7.27 4-Methoxybenzyl alcohol 49.18 Tetracosane 2.99 Pentacosane 8.02 Vanillin 13.56 Octa(ethylene glycol) mono(dodecyl) ether 11.61 Palmitic acid 0.22 Oleic acid 0.07 4-Methylguaiacol 0.08 4-Methoxymethylphenol 0.20 Vanillyl alcohol ethyl ether 0.71 Vanillin 0.68 Vanillic acid 0.94

[0199] Table 2 is a table showing the contents of vanillin and other components in the vanilla oil prepared in Example 3, wherein the content of vanillin reaches 13.56 wt.%. It can be seen that the preparation method of the vanilla oil in the embodiment of the present application can increase the yield of the vanilla oil and effectively increase the content of vanillin to about 13.56 wt.%.

[0200] 3. UV-Visible Light Test

[0201] Figure 1The UV-visible spectrum of the vanilla oil prepared in Example 1 is shown in FIG. The vanilla oil was diluted with n-hexane in a volume ratio of 1:1000 to obtain a vanilla oil solution, and the vanilla oil solution was subjected to UV full wavelength scanning of 190 nm to 1000 nm. Figure 1 As shown, the vanilla oil solution has a strong absorption peak in the ultraviolet band of 190nm to 400nm, indicating that the vanilla oil prepared in the present application contains vanillin.

[0202] 4. Effects of Vanilla Oil on 3T3 Cell Scratches

[0203] A 3T3 cell scratch test was performed using vanilla oil to verify that the vanilla oil has a repairing effect on 3T3 cells. The 3T3 cells are 3T3 mouse embryonic fibroblasts, which can be obtained through commercial channels. The vanilla oil used in the experiment is prepared in Example 1. The method for performing a 3T3 cell scratch test using vanilla oil includes:

[0204] 1) 3T3 cell recovery: 3T3 cells were cultured in DMEM containing 10% FBS and 2% FBS;

[0205] 2) Cell digestion: Observe the growth of 3T3 cells under a microscope. When the cell fusion rate reaches 80‰ to 90%, use 0.25% trypsin to digest the cells, add 10% FBS and 2% DMEM as culture medium to terminate the digestion, and transfer to a centrifuge tube:

[0206] 3) Centrifugation: 1500 rpm at room temperature for 5 min;

[0207] 4) Resuspend the cells and inoculate a certain number of cells in a 24-well plate at 37°C and 5% CO 2 Incubate for 24 hours; observe cell growth under a microscope, and when the cell fusion rate reaches 80% to 90%, use a 00μL gun tip to scratch the cultured cells under the limit of a ruler, with a width of 300μm. After the cultured cells are scratched, use PBS to wash the floating cells, and then add DMEM culture medium and DMEM culture medium containing 0.5wt.% of the vanilla oil prepared in Example 1 to continue culturing. Collect images of cell migration at 0h and 24h after scratching, and evaluate the healing ability of the sample by observing the distance of cell migration. And take 3T3 cells cultured without adding the vanilla oil of Example 1 under the same conditions as a comparative example.

[0208] like Figure 2 As shown in a and b, the 3T3 cell scratches without the addition of the vanilla oil prepared in Example 1 were used as the control group, wherein the scratch width of the 3T3 cells remained unchanged after 0 h (as shown in FIG. Figure 2In the middle), the scratch width decreases after 24 (e.g. Figure 2 In b), the 3T3 cells' own healing ability reduces the width of the scratch. Figure 2 As shown in c and d, the 3T3 cells scratched with the vanilla oil prepared in Example 1 were used as the experimental group, wherein the scratch width of the 3T3 cells remained unchanged after 0 h (as shown in FIG. Figure 2 In (c), the width of the scratch is significantly reduced after 24 hours, which is about 1 / 2 of the width of the scratch (e.g. Figure 2 d), indicating that the width of the scratch on the 3T3 cells after adding the vanilla oil is significantly narrowed. The comparison results of the scratch widths above show that the addition of the vanilla oil prepared in Example 1 is compared with the addition of the vanilla oil prepared in Example 1, indicating that the vanilla oil has a more obvious effect of promoting the repair of damaged 3T3 cells.

[0209] Example 6

[0210] A vanilla oil composition comprises 3 g of the vanilla oil 1 prepared in Example 1, 20 g of jojoba oil, and 1 g of tocopherol acetate. The preparation method comprises: taking 3 g of the vanilla oil prepared in Example 1, adding 20 g of jojoba oil, heating and stirring at 85° C. to fully dissolve, and cooling to 50° C. to 60° C. Then filtering, adding g of tocopherol acetate and stirring to mix evenly, and obtaining the vanilla oil composition 1.

[0211] Example 7

[0212] A vanilla oil composition comprises 10 g of the vanilla oil 1 prepared in Example 1, 0.5 g of dibutyl ethylhexanoyl glutamine, 88.5 g of caprylic capric triglyceride (GTCC), and 1 g of a first solid phase. The preparation method comprises: taking 10 g of the vanilla oil 1 prepared in Example 1, 0.5 g of dibutyl ethylhexanoyl glutamine, adding 88.5 g of caprylic capric triglyceride, heating and stirring at 85° C. to fully dissolve, cooling to 50° C. to 60° C., adding the first solid phase, and stirring evenly to obtain a vanilla oil composition 2.

[0213] Example 8

[0214] A night cream comprising the components in Table 3 below:

[0215] Table 3

[0216]

[0217]

[0218] The preparation method of night cream comprises: weighing phase A and phase B raw materials respectively, heating and stirring in a water bath at 85°C until completely dissolved, adding phase A to phase B under stirring, stirring sufficiently and quickly, processing with a high-speed homogenizer for 5min to 10min, stirring and cooling to 50°C, adding phase C, and stirring and mixing evenly.

[0219] Example 9

[0220] A lipstick comprising the components in Table 4 below:

[0221] Table 4

[0222]

[0223] The preparation method of lipstick comprises: weighing phase A and phase B raw materials respectively, heating and stirring in a water bath at 85°C until phase A is completely dissolved and phase B is mixed uniformly, adding phase A into phase B under stirring conditions, stirring sufficiently and rapidly, performing cyclic treatment in a three-roll grinder, and cooling to room temperature to obtain the lipstick raw material.

[0224] Example 10

[0225] A gel comprising the components listed in Table 5 below:

[0226] Table 5

[0227]

[0228] The preparation method of the gel comprises: accurately weighing each component of phase A, stirring evenly, heating and stirring in a water bath at 85°C until completely dissolved, taking out and cooling to 50°C, adding phase B and phase C respectively, stirring and mixing evenly, and cooling to room temperature to obtain the gel. Figure 3 As shown, it is a gel care product containing a vanilla oil composition prepared in this example, which contains black, intact vanilla seeds, and the vanilla seeds are introduced from the vanilla oil composition 2.

[0229] The above is only a specific implementation method of the present application. Those skilled in the art can clearly understand that for the convenience and simplicity of description, the specific working process described above can refer to the corresponding process in the aforementioned method embodiment, and will not be repeated here. It should be understood that the protection scope of the present application is not limited to this. Any technician familiar with the technical field can easily think of various equivalent modifications or replacements within the technical scope disclosed in the present application, and these modifications or replacements should be included in the protection scope of the present application.

Claims

1. A method for preparing a vanilla oily substance, characterized in that: include: Provides vanilla seeds and pods; Extracting a first vanilla oily substance from vanilla pods by enzymatic hydrolysis, comprising: refining the vanilla pods to obtain pod powder, and dispersing the pod powder with water to obtain a first dispersion; adding a decomposing enzyme to the first dispersion to perform enzymatic hydrolysis to obtain an enzymatic hydrolysis product; heating the enzymatic hydrolysis product to 80°C to 100°C for a first period of time for cyclic solid-liquid extraction and separation to obtain a first mixed solution; adding a first extractant to the first mixed solution for sedimentation separation to obtain a supernatant; concentrating the supernatant to an extract; adding a second extractant to the extract for extraction to obtain a second mixed solution; removing the second extractant from the second mixed solution to obtain a first vanilla oily substance; Gathering the seeds of vanilla and subjecting them to supercritical CO2 extraction to obtain a second vanilla oily substance; The vanilla oily substance is prepared by mixing the first vanilla oily substance and the second vanilla oily substance.

2. The method for preparing the vanilla oily substance according to claim 1, characterized in that: The method of providing the seeds and pods of vanilla comprises peeling the pods and seeds of the vanilla in a mature stage to provide the seeds and pods of vanilla.

3. The method for preparing the vanilla oily substance according to claim 1, characterized in that: Meet any of the following requirements: 1) The process of refining the vanilla pods comprises: grinding or ultrasonically crushing the vanilla pods to obtain pod powder with a particle size of ≤1000 μm; 2) the dispersing treatment of the bean pod powder with water comprises: adding water 1 to 20 times the mass of the bean pod powder to the bean pod powder to obtain a first dispersion; 3) the step of adding a decomposition enzyme to the first dispersion for enzymatic hydrolysis comprises: adjusting the pH value of the first dispersion to 3.0-7.0, adding the decomposition enzyme to perform enzymatic hydrolysis at 40° C.-80° C., and obtaining an enzymatic hydrolysis product; 4) adding the decomposing enzyme to the first dispersion in an amount of 0.01 g / kg to 15 kg / kg; 5) the decomposing enzyme is selected from cellulase, hemicellulase, amylase, pectinase, protease, tannase, amylodisaccharidase, xylanase, β-glucosidase or a combination thereof; 6) The decomposing enzymes include cellulase: pectinase: protease in a mass ratio of (1-10): (1-10): (0.5-1); 7) The decomposition enzyme comprises cellulase: pectinase: protease in a mass ratio of (1-5): (1-2): 1; or, the decomposition enzyme comprises cellulase: β-glucanase: xylanase in a mass ratio of (1-10): (1-5): (0.5-3); 8) heating the enzymatic hydrolyzate to 80° C. to 100° C. for a first period of solid-liquid extraction and filtering to obtain a first mixed solution; 9) The first extractant is selected from water or one or a mixture of methanol, ethanol, isopropanol, n-propanol, and isobutanol; 10) The mass ratio of the first mixed solution to the first extractant is 1:(1-10); 11) The step of concentrating the supernatant into an extract comprises: Clarifying the supernatant to obtain a transparent liquid; Concentrating and recovering the transparent liquid to obtain an extract; 12) The second extracting agent is selected from one of n-hexane, petroleum ether, ethyl acetate, and acetone, or a mixture of several of them; 13) the step of adding a second extractant to the extract for extraction comprises: adding a second extractant to the extract, using ultrasound-assisted dispersion combined with dynamic monitoring of low-temperature extraction, separation and purification to obtain a second mixed solution; 14) The process conditions of adding the second extractant to the extract and using ultrasonic-assisted dispersion combined with dynamic monitoring of low-temperature extraction are as follows: the time of ultrasonic-assisted dispersion is 0.5h to 5h, the extraction time of ultrasonic-assisted dispersion combined with dynamic monitoring of low-temperature extraction is 5h to 72h, the mass ratio of the extract to the second extractant is 1:(1-100), and the extraction temperature is 20°C to 50°C; 15) The method of removing the second extractant from the second mixed liquid comprises: allowing the second mixed liquid to stand for stratification, taking the supernatant and concentrating and distilling it until no second extractant flows out, so as to remove the second extractant from the second mixed liquid and obtain a first vanilla oily substance.

4. The method for preparing the vanilla oily substance according to any one of claims 1 to 3, characterized in that: The method of aggregating the vanilla seeds and subjecting them to supercritical CO2 extraction treatment comprises: The seeds of the vanilla are gathered and extracted by supercritical CO2 with an extraction pressure of 20MPa-35MPa, a temperature of 30°C-60°C, and an extraction time of 2h-10h; wherein the pressure of the first separation kettle is 5MPa-12MPa, and the pressure of the second separation kettle is 2MPa-7MPa; the effluents of the first separation kettle and the second separation kettle are collected and filtered to obtain a second vanilla oily substance.

5. A vanilla oily substance, characterized in that: The invention comprises the first vanilla oily substance and the second vanilla oily substance prepared according to any one of claims 1 to 4 in a mass ratio of (1 to 5): (5 to).

6. A vanilla oil composition, characterized in that: The vanilla oil composition comprises the vanilla oil as claimed in claim 5, wherein the vanilla oil accounts for 10 wt.% to 100 wt.% of the mass of the vanilla oil composition.

7. A vanilla oil composition, characterized in that: The invention comprises the vanilla oily substance as claimed in claim 5, wherein the vanilla oily substance accounts for 10wt.% to 100wt.% of the mass of the vanilla oily substance composition; and further comprises one or a combination of several of an alcohol solvent, a thickener, a suspending agent, a vegetable oil, a mineral oil, an antioxidant, and a first solid phase, wherein the first solid phase is the vanilla seeds which are collected and impurity-removed to retain intact vanilla seeds after the second vanilla oily substance is extracted with supercritical CO2.

8. The vanilla oil composition according to claim 7, characterized in that: Meet at least one of the following requirements: The alcohol solvent is selected from 1,3-propylene glycol, glycerol, propylene glycol, butylene glycol, 1,2-butylene glycol, octyl dodecanol or a combination thereof; The thickener is selected from carbomer 980, carbomer 941, acrylates / C10-30 alkyl acrylate crosspolymer, xanthan gum, carrageenan, dextrin palmitate, dextrin palmitate ethylhexanoate, hydrogenated castor oil, PEG-30 hydrogenated castor oil or a combination thereof; The suspending agent is selected from dibutyl ethylhexanoyl glutamine, dibutyl lauroyl glutamate, hydrogenated lecithin, PEG / PPG-17 / 6 copolymer or a combination thereof; The vegetable oil is selected from jojoba oil, almond oil, sunflower oil, shea butter or a combination thereof; The mineral oil is selected from caprylic capric triglyceride, white oil, glyceryl polyether-26, neopentyl glycol diheptanoate or a combination thereof; The antioxidant is selected from tocopheryl acetate, tocopherol, BHT, BHA, TBHQ, ascorbyl palmitate, tea polyphenols, phytic acid or a combination thereof.

9. The vanilla oil composition according to claim 7, characterized in that: The mass of the first solid phase accounts for 0.5 wt% to 10 wt.% of the total mass of the vanilla oil composition.

10. Use of the vanilla oil composition according to any one of claims 6 to 9 in the preparation of a care product, wherein the care product is one of a lotion, a cream, a toner, an essence, a gel, a body lotion, a care oil, a lipstick, and a lip glaze, wherein: The content of the vanilla oil composition according to any one of claims 6 to 9 in the care product is 0.01 wt.% to 20 wt.%.

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