Olive oil capable of repairing, relieving and resisting wrinkles as well as preparation method and application of olive oil
By optimizing the centrifugal process of olive oil, increasing enzymatic decomposition and fermentation, retreating the pomace, and purifying it with modified adsorbent, the problems of low oil yield, high cost and loss of antioxidant components in the existing olive oil preparation methods are solved, and the high biological activity and storage stability of olive oil are achieved.
Patent Information
- Application Number
- CN202411981707.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-30
- Publication Date
- 2025-03-18
- Estimated Expiration
- 2044-12-30
AI Technical Summary
The existing olive oil preparation methods have problems such as low oil yield, high production cost, and loss of natural antioxidant components, making it difficult to maximize the natural activity of olive oil and improve quality.
By optimizing the centrifugation process, increasing enzymatic decomposition and fermentation, the olive pom beans are further improved, and the biological activity of olive oil is purified by a specific modified adsorbent.
It improves the bioactivity and storage stability of olive oil, maintains fresh fruity aroma, clear transparency, low peroxide value and low acid value, and its antioxidant and anti-wrinkle effects are also improved.
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Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of cosmetics, and in particular relates to an olive oil with the functions of repairing, soothing and anti-wrinkle, and a preparation method and application thereof. Background Art
[0002] Olive oil, a natural oil extracted from the fruit of the olive tree, has long been regarded as a treasure of the Mediterranean food culture. This natural oil is rich in monounsaturated fatty acids and a variety of healthy antioxidant ingredients, such as vitamin E and polyphenols. These active ingredients not only help maintain the health of the cardiovascular system, but also provide a basis for the application of olive oil in the field of cosmetics. The antioxidants in olive oil can effectively fight free radicals and reduce the damage of free radicals to skin cells, thereby slowing down the aging process of the skin. The benefits of olive oil for the skin are not only its anti-aging properties, but it can also deeply moisturize the skin, help maintain the skin's moisture barrier, and increase the skin's softness and elasticity. Olive oil can also act as a moisturizing ingredient to help restore the skin's natural radiance while promoting cell renewal. The squalene component contained in olive oil is similar to the structure of human sebum, making it suitable for the care of sensitive or dry skin. Olive oil helps improve skin quality and reduce the appearance of fine lines and wrinkles by enhancing the skin's self-repair ability. In addition, olive oil can protect the skin from damage caused by ultraviolet rays and other environmental factors, making it a versatile and gentle skin care ingredient.
[0003] At present, the main methods for preparing olive oil in the prior art are: cold pressing, centrifugation and solvent extraction. Among them, the cold pressing method is to use mechanical pressure to directly squeeze olive oil from freshly picked olives without heating. This method can maximize the retention of the natural nutrients and flavor in the olives, especially the advantages of virgin olive oil, which is high quality and rich in antioxidants. The centrifugation method is to use a high-speed rotating centrifuge to separate the oil from the pulp and water after the olives are crushed into a paste. This process is fast and efficient, and can ensure the freshness and purity of the olive oil, while reducing the impact of external factors on the quality of the olive oil. The solvent extraction method is mainly used to process olive pomace, and the remaining oil is extracted by organic solvents. This method can increase the oil yield and is relatively low in cost.
[0004] Although each of the above methods has its unique advantages, there are also some shortcomings. For example, the cold pressing method has high requirements on the quality of olive fruits. Any impurities or unfresh olives will affect the quality of the final product. In addition, the oil yield of this method is relatively low, and the production cost is high, resulting in expensive finished products. The centrifugation method requires high-precision equipment and technical support, and the equipment maintenance cost is not low. If it is not operated properly, it may introduce too much water or pomace, affecting the purity and storage stability of olive oil. The solvent extraction method requires the use of chemical solvents and multiple refining treatments, which may cause partial loss of natural antioxidant components in olive oil. Therefore, it is urgent to provide a method for preparing olive oil, which can maximize the retention of the natural activity of olive oil and improve the quality by improving and optimizing the existing preparation process. Summary of the invention
[0005] The purpose of the present invention is to provide a method for preparing olive oil with repairing, soothing and anti-wrinkle effects. By optimizing the centrifugation process and adding enzymatic hydrolysis and fermentation to reprocess the pomace, the biological activity of the olive oil is further improved, and the olive oil is used in cosmetics with good repairing, soothing and anti-wrinkle effects.
[0006] In order to achieve the above object, the present invention provides the following technical solutions:
[0007] The present invention provides a method for preparing olive oil having the functions of repairing, soothing and anti-wrinkle, comprising the following steps:
[0008] Step A1, removing impurities from olive (scientific name: Canarium oleosum (Lam.) Engl.) fruits, then washing with water, adding them to a crusher for crushing, sieving, and obtaining olive pulp; adding the olive pulp to a rotary evaporator for rotary evaporation, then adding water to mix evenly, and then placing them in a centrifuge for centrifugation to obtain a supernatant and olive pomace respectively; the supernatant is allowed to stand for stratification, and the upper oil phase is taken to obtain olive crude oil I;
[0009] Step A2, mixing the olive pomace obtained in step A1 with water, performing ultrasonic treatment, then adding cellulase and pectinase for enzymolysis, sterilizing, and cooling to obtain a pomace pretreatment liquid;
[0010] Step A3, inoculating fermentation bacteria into the pomace pretreatment liquid obtained in step A2 for fermentation, sterilizing and cooling after the fermentation to obtain pomace fermentation liquid; placing the pomace fermentation liquid in a centrifuge for centrifugation to obtain a supernatant; standing and stratifying, taking the upper oil phase to obtain olive crude oil II;
[0011] Step A4, uniformly mixing the crude olive oil I obtained in step A1 and the crude olive oil II obtained in step A3, then adding a modified adsorbent, heating and stirring, cooling, filtering, and obtaining crude olive oil; vacuum deodorizing the crude olive oil, cooling, and obtaining the olive oil having the functions of repairing, soothing, and anti-wrinkle.
[0012] Preferably, a method for preparing olive oil having repairing, soothing and anti-wrinkle effects comprises the following steps:
[0013] Step A1, removing impurities from fresh olive fruits, then rinsing them with water, and then adding them to a crusher for crushing, and passing them through a 30-40 mesh screen to obtain olive pulp; adding the olive pulp to a rotary evaporator, rotary evaporating it at 20-30° C. and 100-300 mbar for 30-50 minutes, then adding water to mix evenly, and then placing it in a centrifuge, centrifuging it at 7000-9000 r / min for 2-4 minutes to obtain a supernatant and olive pomace respectively; the supernatant is allowed to stand for stratification, and the upper oil phase is taken to obtain olive crude oil I; wherein, rotary evaporation can make small oil droplets in the pulp merge into large oil droplets, which helps to quickly separate the pomace in subsequent centrifugal operation;
[0014] Step A2, mixing the olive pomace obtained in step A1 with water, ultrasonicating for 20-30 min under the conditions of ultrasonic power of 150-250 W and ultrasonic frequency of 40-50 kHz, then adding cellulase and pectinase, adjusting the pH to 4.5-5.5, performing enzymolysis at 45-55° C. for 7-10 h, sterilizing at 115-125° C. for 10-20 min, and cooling to room temperature to obtain a pomace pretreatment liquid;
[0015] Step A3, inoculating fermentation bacteria into the pomace pretreatment liquid obtained in step A2, fermenting at a constant temperature of 25-30° C. for 70-75 hours, sterilizing at 115-125° C. for 10-20 minutes after the fermentation, cooling to room temperature, and obtaining pomace fermentation liquid; placing the pomace fermentation liquid in a centrifuge, centrifuging at 7000-9000 r / min for 2-4 minutes, discarding the precipitate, and obtaining a supernatant; standing for stratification, taking the upper oil phase, and obtaining olive crude oil II;
[0016] Step A4, mixing the crude olive oil I obtained in step A1 and the crude olive oil II obtained in step A3 evenly, then adding the modified adsorbent, stirring at 40-50° C. and 100-150 r / min for 40-60 min, cooling to room temperature, filtering to obtain crude olive oil; vacuum deodorizing the crude olive oil at 0.5-1 mbar and 160-180° C. for 2-4 h, cooling to room temperature, and obtaining the olive oil with repairing, soothing and anti-wrinkle properties.
[0017] Preferably, the amount of water added in step A1 is 100-120 wt % of the weight of the olive pulp.
[0018] Preferably, the weight ratio of the olive pomace to water in step A2 is 1:4-6.
[0019] Preferably, the amount of cellulase added in step A2 is 0.5-0.7wt% of the weight of the olive pomace, and the amount of pectinase added is 0.3-0.5wt% of the weight of the olive pomace.
[0020] Preferably, the inoculation amount of the fermentation bacteria in step A3 is 1×10 8 -2×10 8 cfu / mL pomace pretreatment solution.
[0021] Preferably, the fermentation bacteria in step A3 are composed of Hansenula anomalosa and Bacillus amyloliquefaciens, and the ratio of the Hansenula anomalosa to Bacillus amyloliquefaciens is 1:1-3.
[0022] Preferably, the number of Hansenula anomalosa is CICC 32234, and the number of Bacillus amyloliquefaciens is CICC20164, which are purchased from China Industrial Microbiological Culture Collection Center.
[0023] The present invention optimizes the centrifugation process, adds enzymatic hydrolysis and fermentation by specific fermentation bacteria to reprocess the olive pomace, thereby further improving the biological activity and storage stability of olive oil, allowing the olive oil to maintain a fresh fruity smell, clear transparency, low peroxide value and low acid value, and its antioxidant and anti-wrinkle effects are also further enhanced.
[0024] First, the present invention can effectively decompose the complex polysaccharide structures such as cellulose and pectin in the pomace through the enzymatic hydrolysis of cellulase and pectinase, and release more oils and active ingredients, such as polyphenol compounds, vitamin E and other fat-soluble antioxidant substances, which not only enhance the antioxidant capacity of olive oil, but also effectively inhibit the oxidation reaction of oil, reduce the peroxide value and acid value, and improve the stability of olive oil. Secondly, the combined fermentation of Bacillus amyloliquefaciens and Hansen yeast is helpful to increase the extraction efficiency and biological activity of olive oil. Bacillus amyloliquefaciens can secrete a variety of enzymes, such as protease, lipase and amylase, etc. These enzymes can further decompose the macromolecular substances in the pomace, release and convert them into more biologically active substances, such as squalene, β-carotene and vitamins, etc. These ingredients further enhance the antioxidant and anti-wrinkle effects of olive oil; Hansen yeast has good metabolic activity, which can assist Bacillus amyloliquefaciens to metabolize carbohydrates in the pomace during the fermentation process, and produce a variety of beneficial metabolites, which not only enrich the aroma components of olive oil, but also enhance its moisturizing and repairing functions. In addition, the microbial metabolism during the fermentation process can consume the oxygen in the pomace, reduce the contact between oil and oxygen, thereby reducing the chance of oxidation reactions and maintaining the fresh fruity smell and clear transparency of olive oil.
[0025] Preferably, the amount of the modified adsorbent added in step A4 is 1.5-3 wt % of the total weight of the crude olive oil.
[0026] Preferably, the modified adsorbent is prepared by the following method:
[0027] 25-40 parts by weight of natural zeolite powder and 15-30 parts by weight of natural diatomaceous earth are added to 150-300 parts by weight of sodium hydroxide aqueous solution, and then 3-5 parts by weight of sodium bicarbonate are added, heated and stirred, cooled, filtered, and dried to obtain an activated composite;
[0028] 2-4 parts by weight of chitosan are added to 150-300 parts by weight of citric acid aqueous solution, and ultrasonic treatment is performed. Then, 3-5 parts by weight of hydrogen peroxide, 1.2-1.8 parts by weight of caffeic acid and 0.1-0.3 parts by weight of vitamin C are added in sequence under nitrogen protection, and the reaction is carried out in the dark. The mixture is precipitated with anhydrous ethanol, filtered and dried to obtain modified chitosan. 8-12 parts by weight of the activated complex and 1-2 parts by weight of the modified chitosan are evenly mixed to obtain a modified adsorbent.
[0029] Compared with traditional activated carbon adsorbents, the modified adsorbent used in the present invention further improves the storage stability of olive oil through the synergistic effect of multiple components. Among them, natural zeolite powder and diatomaceous earth are treated with sodium hydroxide aqueous solution to form an activated complex. These materials have rich pore structures and large specific surface areas, and can effectively adsorb impurities, pigments and odor substances in olive oil. At the same time, the alkaline environment provided by them helps to neutralize acidic components and reduce acid value; chitosan is grafted with caffeic acid under the initiation of vitamin C / hydrogen peroxide to form modified chitosan, which further enhances the adsorption capacity and antioxidant activity of chitosan. The modified chitosan can not only adsorb various impurities in olive oil, but also can efficiently remove free radicals, inhibit oxidation reactions, and further reduce peroxide value and acid value; the above-mentioned activated complex and modified chitosan synergistically form a multifunctional adsorption system, which can not only physically adsorb impurities, but also chemically bind harmful substances, thereby ensuring the stability and high biological activity of olive oil.
[0030] Furthermore, the modified adsorbent is prepared by the following method:
[0031] 25-40 parts by weight of natural zeolite powder and 15-30 parts by weight of natural diatomaceous earth are added to 150-300 parts by weight of 0.5-1.5wt% sodium hydroxide aqueous solution, and ultrasonicated for 30-50 minutes at an ultrasonic power of 100-200W and an ultrasonic frequency of 20-30kHz, and then 3-5 parts by weight of sodium bicarbonate are added, and stirred at 55-65°C and 150-300r / min for 40-60 minutes, cooled to room temperature, filtered, and dried to obtain an activated composite;
[0032] 2-4 parts by weight of chitosan are added to 150-300 parts by weight of 2-4wt% citric acid aqueous solution, and ultrasonicated for 15-30 minutes under the conditions of ultrasonic power of 100-200W and ultrasonic frequency of 20-30kHz, and then 3-5 parts by weight of 18-22wt% hydrogen peroxide, 1.2-1.8 parts by weight of caffeic acid and 0.1-0.3 parts by weight of vitamin C are added in sequence under nitrogen protection, reacted at 25-30°C in the dark for 10-15 hours, precipitated with anhydrous ethanol, filtered, and dried to obtain modified chitosan; 8-12 parts by weight of the activated complex and 1-2 parts by weight of the modified chitosan are evenly mixed to obtain a modified adsorbent.
[0033] The invention also provides an olive oil with the functions of repairing, soothing and anti-wrinkle, which is prepared by the above method.
[0034] The present invention also provides the use of the above olive oil with repairing, soothing and anti-wrinkle effects in the preparation of cosmetics; the application includes but is not limited to creams, lotions, essences and the like.
[0035] Compared with the prior art, the advantages and beneficial effects of the present invention are:
[0036] 1. The present invention provides a method for preparing olive oil with repairing, soothing and anti-wrinkle effects. The centrifugal process is optimized, and the pomace is further treated by enzymatic hydrolysis and fermentation, thereby further improving the biological activity of the olive oil. Then, a specific modified adsorbent is used for purification, thereby improving the stability of the olive oil. The present invention also provides the use of the above olive oil in the preparation of cosmetics, which has good repairing, soothing and anti-wrinkle effects.
[0037] 2. The present invention adds enzymatic hydrolysis and fermentation with specific fermentation bacteria to reprocess the olive pomace, which further improves the biological activity and storage stability of olive oil. The enzymatic hydrolysis of cellulase and pectinase can effectively decompose the complex polysaccharide structures such as cellulose and pectin in the pomace, which is convenient for releasing more oil and active ingredients. The combined fermentation of Bacillus amyloliquefaciens and Hansenula anomalosa helps to increase the extraction efficiency and biological activity of olive oil, and can also be converted into a variety of biologically active substances, such as squalene, β-carotene and vitamins, etc. These active substances further enhance the antioxidant and anti-wrinkle effects of olive oil.
[0038] 3. The present invention adopts a specific modified adsorbent, and through the synergistic effect of multiple components, a multifunctional adsorption system is formed, which can not only physically adsorb impurities, but also chemically bind harmful substances, further improving the storage stability of olive oil. Among them, the activated complex has a rich pore structure and a large specific surface area, which can effectively physically adsorb impurities, pigments and odor substances in olive oil. At the same time, the alkaline environment it provides helps to neutralize acidic components and reduce acid value; the adsorption capacity and antioxidant activity of the modified chitosan are enhanced, which can not only adsorb various impurities in olive oil, but also efficiently remove free radicals, inhibit oxidation reactions, and further reduce peroxide value and acid value. DETAILED DESCRIPTION
[0039] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.
[0040] Example 1
[0041] This embodiment provides a method for preparing olive oil with repairing, soothing and anti-wrinkle properties, comprising the following steps:
[0042] Step A1, remove impurities from fresh olive fruits, then rinse with water, add them into a crusher for crushing, and pass through a 35-mesh screen to obtain olive pulp; add the olive pulp into a rotary evaporator, rotary evaporate at 25° C. and 200 mbar for 40 minutes, then add water and mix evenly, wherein the amount of water added is 110wt% of the weight of the olive pulp, and then place in a centrifuge, centrifuge at 8000r / min for 2.5 minutes, respectively obtain a supernatant and olive pomace; place the supernatant into a separatory funnel and let it stand for 12 hours, take the upper oil phase, and obtain olive crude oil I;
[0043] Step A2, mixing the olive pomace obtained in step A1 with water in a weight ratio of 1:5, ultrasonically treating for 25 minutes under the conditions of an ultrasonic power of 200 W and an ultrasonic frequency of 45 kHz, then adding cellulase and pectinase, wherein the amount of the cellulase added is 0.6 wt % of the weight of the olive pomace, and the amount of the pectinase added is 0.4 wt % of the weight of the olive pomace, adjusting the pH to 5.0, performing enzymolysis at 50° C. for 8 hours, sterilizing at 121° C. for 15 minutes, and cooling to room temperature to obtain a pomace pretreatment liquid; wherein the enzyme activity of the cellulase is 400 u / mg, and the enzyme activity of the pectinase is 35 u / mg;
[0044] Step A3: inoculate fermentation bacteria into the pomace pretreatment liquid obtained in step A2, and ferment at a constant temperature of 28°C for 72 hours. The inoculation amount of the fermentation bacteria is 1.7×10 8 cfu / mL pomace pretreatment liquid, wherein the fermentation bacteria are composed of abnormal Hansenula and Bacillus amyloliquefaciens, and the number ratio of the abnormal Hansenula to the Bacillus amyloliquefaciens is 1:2; after the fermentation is completed, sterilize at 121°C for 15 minutes, cool to room temperature, and obtain pomace fermentation liquid; place the pomace fermentation liquid in a centrifuge, centrifuge at 8000r / min for 2.5 minutes, discard the precipitate, and obtain a supernatant; place the supernatant in a separatory funnel and let it stand for 12 hours, take the upper oil phase, and obtain olive crude oil II; wherein the abnormal Hansenula is numbered CICC 32234, and the Bacillus amyloliquefaciens is numbered CICC20164, which are purchased from the China Industrial Microbiological Culture Collection Management Center;
[0045] Step A4, the crude olive oil I obtained in step A1 and the crude olive oil II obtained in step A3 are evenly mixed, and then a modified adsorbent is added, wherein the amount of the modified adsorbent added is 2wt% of the total weight of the crude olive oil, and the mixture is stirred at 45°C and 120r / min for 50min, cooled to room temperature, and filtered to obtain crude olive oil; the crude olive oil is vacuum deodorized at 0.5mbar and 180°C for 3h, and cooled to room temperature to obtain the olive oil having the functions of repairing, soothing, and anti-wrinkle.
[0046] The modified adsorbent is prepared by the following method:
[0047] 30 parts by weight of natural zeolite powder and 20 parts by weight of natural diatomaceous earth are added to 200 parts by weight of 1wt% sodium hydroxide aqueous solution, ultrasonicated for 40 minutes at an ultrasonic power of 100W and an ultrasonic frequency of 25kHz, then 4 parts by weight of sodium bicarbonate are added, stirred at 60°C and 200r / min for 50 minutes, cooled to room temperature, filtered, and dried to obtain an activated composite; wherein the average particle size of the natural zeolite powder is 500 mesh, and the average particle size of the natural diatomaceous earth is 800 mesh;
[0048] 2.5 parts by weight of chitosan are added to 200 parts by weight of 3wt% citric acid aqueous solution, ultrasonicated for 20 minutes under the conditions of ultrasonic power of 100W and ultrasonic frequency of 25kHz, then 4 parts by weight of 20wt% hydrogen peroxide, 1.6 parts by weight of caffeic acid and 0.2 parts by weight of vitamin C are added in sequence under nitrogen protection, reacted at 27°C in the dark for 12 hours, precipitated with anhydrous ethanol, filtered and dried to obtain modified chitosan; 10 parts by weight of activated complex and 1.5 parts by weight of modified chitosan are mixed evenly to obtain modified adsorbent. Among them, the average molecular weight of chitosan is 100000 and the degree of deacetylation is 90%.
[0049] Example 2
[0050] This embodiment provides a method for preparing olive oil with repairing, soothing and anti-wrinkle properties, comprising the following steps:
[0051] Step A1, remove impurities from fresh olive fruits, then rinse with water, add them into a crusher for crushing, and pass through a 30-mesh screen to obtain olive pulp; add the olive pulp into a rotary evaporator, rotary evaporate at 20° C. and 100 mbar for 50 minutes, then add water and mix evenly, wherein the amount of water added is 100wt% of the weight of the olive pulp, and then place in a centrifuge, centrifuge at 7000 r / min for 4 minutes to obtain a supernatant and olive pomace respectively; place the supernatant into a separatory funnel and let it stand for 10 hours, take the upper oil phase, and obtain olive crude oil I;
[0052] Step A2, mixing the olive pomace obtained in step A1 with water in a weight ratio of 1:4, ultrasonically treating for 30 minutes under the conditions of an ultrasonic power of 150 W and an ultrasonic frequency of 40 kHz, then adding cellulase and pectinase, wherein the amount of the cellulase added is 0.5wt% of the weight of the olive pomace, and the amount of the pectinase added is 0.3wt% of the weight of the olive pomace, adjusting the pH to 4.5, performing enzymolysis at 45° C. for 7 hours, sterilizing at 115° C. for 20 minutes, and cooling to room temperature to obtain a pomace pretreatment liquid; wherein the enzyme activity of the cellulase is 400u / mg, and the enzyme activity of the pectinase is 35u / mg;
[0053] Step A3: inoculate fermentation bacteria into the pomace pretreatment liquid obtained in step A2, and ferment at a constant temperature of 25°C for 70 hours. The inoculation amount of the fermentation bacteria is 1×10 8 cfu / mL pomace pretreatment liquid, wherein the fermentation bacteria are composed of abnormal Hansenula and Bacillus amyloliquefaciens, and the number ratio of the abnormal Hansenula and Bacillus amyloliquefaciens is 1:1; after the fermentation is completed, sterilize at 115°C for 20 minutes, cool to room temperature, and obtain pomace fermentation liquid; place the pomace fermentation liquid in a centrifuge, centrifuge at 7000r / min for 4 minutes, discard the precipitate, and obtain a supernatant; place the supernatant in a separatory funnel and let it stand for 10 hours, take the upper oil phase, and obtain olive crude oil II; wherein the abnormal Hansenula is numbered CICC 32234, and the Bacillus amyloliquefaciens is numbered CICC20164, which are purchased from the China Industrial Microbiological Culture Collection Management Center;
[0054] Step A4, the crude olive oil I obtained in step A1 and the crude olive oil II obtained in step A3 are evenly mixed, and then a modified adsorbent is added, wherein the amount of the modified adsorbent added is 1.5wt% of the total weight of the crude olive oil, and the mixture is stirred at 40°C and 100r / min for 40min, cooled to room temperature, and filtered to obtain crude olive oil; the crude olive oil is vacuum deodorized at 0.5mbar and 160°C for 4h, and cooled to room temperature to obtain the olive oil having the functions of repairing, soothing, and anti-wrinkle.
[0055] The modified adsorbent is the same as that in Example 1.
[0056] Example 3
[0057] This embodiment provides a method for preparing olive oil with repairing, soothing and anti-wrinkle properties, comprising the following steps:
[0058] Step A1, remove impurities from fresh olive fruits, then rinse with water, add them into a crusher for crushing, and pass through a 40-mesh screen to obtain olive pulp; add the olive pulp into a rotary evaporator, rotary evaporate at 30° C. and 300 mbar for 30 minutes, then add water and mix evenly, wherein the amount of water added is 120wt% of the weight of the olive pulp, and then place in a centrifuge, centrifuge at 9000r / min for 2 minutes to obtain a supernatant and olive pomace respectively; place the supernatant into a separatory funnel and let stand for 15 hours, take the upper oil phase, and obtain olive crude oil I;
[0059] Step A2, mixing the olive pomace obtained in step A1 with water in a weight ratio of 1:6, ultrasonically treating for 20 minutes under the conditions of an ultrasonic power of 250 W and an ultrasonic frequency of 50 kHz, then adding cellulase and pectinase, wherein the amount of cellulase added is 0.7wt% of the weight of the olive pomace, and the amount of pectinase added is 0.5wt% of the weight of the olive pomace, adjusting the pH to 5.5, performing enzymolysis at 55° C. for 10 hours, sterilizing at 125° C. for 10 minutes, and cooling to room temperature to obtain a pomace pretreatment liquid; wherein the enzyme activity of the cellulase is 400u / mg, and the enzyme activity of the pectinase is 35u / mg;
[0060] Step A3: inoculate fermentation bacteria into the pomace pretreatment liquid obtained in step A2, and ferment at a constant temperature of 30°C for 70 hours. The inoculation amount of the fermentation bacteria is 2×10 8 cfu / mL pomace pretreatment liquid, wherein the fermentation bacteria are composed of abnormal Hansenula and Bacillus amyloliquefaciens, and the number ratio of the abnormal Hansenula to the Bacillus amyloliquefaciens is 1:3; after the fermentation is completed, sterilize at 125°C for 10 minutes, cool to room temperature, and obtain pomace fermentation liquid; place the pomace fermentation liquid in a centrifuge, centrifuge at 9000r / min for 2 minutes, discard the precipitate, and obtain a supernatant; place the supernatant in a separating funnel and let it stand for 15 hours, take the upper oil phase, and obtain olive crude oil II; wherein the abnormal Hansenula is numbered CICC 32234, and the Bacillus amyloliquefaciens is numbered CICC20164, which are purchased from the China Industrial Microbiological Culture Collection Management Center;
[0061] Step A4, the crude olive oil I obtained in step A1 and the crude olive oil II obtained in step A3 are evenly mixed, and then a modified adsorbent is added, wherein the amount of the modified adsorbent added is 3wt% of the total weight of the crude olive oil, and the mixture is stirred at 50°C and 150r / min for 60min, cooled to room temperature, and filtered to obtain crude olive oil; the crude olive oil is vacuum deodorized at 1mbar and 180°C for 2h, and cooled to room temperature to obtain the olive oil having the functions of repairing, soothing, and anti-wrinkle.
[0062] The modified adsorbent is the same as that in Example 1.
[0063] Comparative Example 1
[0064] The difference between this comparative example and Example 1 is that step A2 in the preparation method of the olive oil with repairing, soothing and anti-wrinkle properties is different, specifically as follows: the olive pomace obtained in step A1 is mixed with water in a weight ratio of 1:5, ultrasonicated for 25 minutes under the conditions of ultrasonic power of 200 W and ultrasonic frequency of 45 kHz, then sterilized at 121° C. for 15 minutes, and cooled to room temperature to obtain a pomace pretreatment liquid.
[0065] Comparative Example 2
[0066] The difference between this comparative example and Example 1 is that the step A3 in the preparation method of the olive oil with repairing, soothing and anti-wrinkle properties is different, specifically as follows: placing the pomace pretreatment liquid in a centrifuge, centrifuging at 8000r / min for 2.5min, discarding the precipitate to obtain a supernatant; placing the supernatant in a separatory funnel and letting it stand for 12h, taking the upper oil phase to obtain olive crude oil II.
[0067] Comparative Example 3
[0068] The difference between this comparative example and Example 1 is that the preparation method of the olive oil with repairing, soothing and anti-wrinkle properties is different in step A3, which is as follows: fermentation bacteria are inoculated into the pomace pretreatment liquid obtained in step A2, and the fermentation is carried out at a constant temperature of 28°C for 72 hours. The inoculation amount of the fermentation bacteria is 1.7×10 8 cfu / mL pomace pretreatment liquid, wherein the fermentation bacteria is abnormal Hansenula; after the fermentation is completed, sterilize at 121°C for 15 minutes, cool to room temperature, and obtain pomace fermentation liquid; place the pomace fermentation liquid in a centrifuge, centrifuge at 8000r / min for 2.5 minutes, discard the precipitate, and obtain a supernatant; place the supernatant in a separatory funnel and let it stand for 12 hours, take the upper oil phase, and obtain olive crude oil II; wherein the abnormal Hansenula is numbered CICC 32234 and is purchased from the China Industrial Microbiological Culture Collection Management Center.
[0069] Comparative Example 4
[0070] The difference between this comparative example and Example 1 is that the preparation method of the olive oil with repairing, soothing and anti-wrinkle properties is different in step A3, which is as follows: fermentation bacteria are inoculated into the pomace pretreatment liquid obtained in step A2, and the fermentation is carried out at a constant temperature of 28°C for 72 hours. The inoculation amount of the fermentation bacteria is 1.7×10 8 cfu / mL pomace pretreatment liquid, wherein the fermentation bacteria is Bacillus amyloliquefaciens; after the fermentation is completed, the liquid is sterilized at 121°C for 15 minutes and cooled to room temperature to obtain pomace fermentation liquid; the pomace fermentation liquid is placed in a centrifuge, centrifuged at 8000r / min for 2.5 minutes, the precipitate is discarded, and a supernatant is obtained; the supernatant is placed in a separatory funnel and allowed to stand for 12 hours, and an upper oil phase is taken to obtain olive crude oil II; wherein the Bacillus amyloliquefaciens is numbered CICC 20164 and is purchased from the China Industrial Microbiological Culture Collection Management Center.
[0071] Comparative Example 5
[0072] The difference between this comparative example and Example 1 is that step A4 in the preparation method of the olive oil with repairing, soothing and anti-wrinkle effects is different, specifically as follows: the crude olive oil I obtained in step A1 and the crude olive oil II obtained in step A3 are evenly mixed, and then a modified adsorbent is added, wherein the amount of the modified adsorbent added is 2wt% of the total weight of the crude olive oil; the mixture is stirred at 45°C and 120r / min for 50min, cooled to room temperature, and filtered to obtain crude olive oil; the crude olive oil is vacuum deodorized at 0.5mbar and 180°C for 3h, cooled to room temperature, and the olive oil with repairing, soothing and anti-wrinkle effects is obtained.
[0073] The modified adsorbent is prepared by the following method:
[0074] 30 parts by weight of natural zeolite powder and 20 parts by weight of natural diatomaceous earth are added to 200 parts by weight of 1wt% sodium hydroxide aqueous solution, ultrasonicated for 40 minutes at an ultrasonic power of 100W and an ultrasonic frequency of 25kHz, then 4 parts by weight of sodium bicarbonate are added, stirred at 60°C and 200r / min for 50 minutes, cooled to room temperature, filtered, and dried to obtain an activated composite; wherein the average particle size of the natural zeolite powder is 500 mesh, and the average particle size of the natural diatomaceous earth is 800 mesh;
[0075] 10 parts by weight of the activated complex and 1.5 parts by weight of chitosan were mixed evenly to obtain a modified adsorbent. The average molecular weight of the chitosan was 100,000 and the degree of deacetylation was 90%.
[0076] Comparative Example 6
[0077] The difference between this comparative example and Example 1 is that the preparation method of the olive oil with repairing, soothing and anti-wrinkle properties is different in step A4, which is as follows: the olive crude oil I obtained in step A1 and the olive crude oil II obtained in step A3 are mixed evenly, and then an adsorbent is added, the adsorbent is activated carbon, and the amount of the adsorbent added is 2wt% of the total weight of the olive crude oil, stirred at 45°C and 120r / min for 50min, cooled to room temperature, filtered, and olive crude oil is obtained; the olive crude oil is vacuum deodorized at 0.5mbar and 180°C for 3h, cooled to room temperature, and the olive oil with repairing, soothing and anti-wrinkle properties is obtained. Among them, the activated carbon uses commercially available coconut shell powder activated carbon with an average particle size of 300 meshes.
[0078] Performance Testing
[0079] 1. The olive oil prepared in the above Examples 1-3 and Comparative Examples 1-6 was stored at room temperature and in the dark for 1 month. The transparency and smell of the olive oil were observed after taking it out, and the content of insoluble impurities was determined by referring to the method in GB / T 15688-2008, the peroxide value was determined by referring to the method in GB 5009.227-2016, and the acid value was determined by referring to the method in GB 5009.229-2016. The test results are shown in Table 1.
[0080] Table 1: Storage stability test results of olive oil
[0081]
[0082]
[0083] 2. Take 6wt% of olive oil, 7wt% of glycerol, 3wt% of 1,3-propylene glycol, 1.5wt% of isopropyl palmitate, 0.2wt% of carbomer prepared in the above Examples 1-3 and Comparative Examples 1-6, and water as the balance, mix them to make cosmetic samples, and conduct efficacy tests.
[0084] The test method is: invite 90 female volunteers aged between 30 and 40 years old without skin diseases, randomly divide them into 9 groups, 10 people in each group, and use the above cosmetic samples respectively. The details are as follows: During the whole process, the volunteers apply the cosmetic samples on the left half of their faces, and do not apply any cosmetics on the right half of their faces as a blank control. The samples are used once in the morning and evening for 45 consecutive days. At the beginning and end of the test, the skin of the volunteers is tested and analyzed using a skin detector to evaluate the improvement of the above cosmetic samples on the skin elasticity of the cheeks and fine lines at the corners of the eyes. Among them, "+" means increase, and "-" means decrease. The results are shown in Table 2.
[0085] Table 2: Results of efficacy test on olive oil used in cosmetics
[0086]
[0087]
[0088] It can be seen from the above test results that the olive oils prepared in Examples 1-3 can still maintain good quality after being stored for a period of time, have a fresh fruity smell, clear transparency, low peroxide value and low acid value, and have good anti-wrinkle and repair effects when used in cosmetics, especially the olive oil prepared in Example 1, whose comprehensive performance is the most outstanding. This is because the present invention improves the preparation process of olive oil, adds enzymatic hydrolysis and fermentation steps to reprocess the pomace, and uses a specific modified adsorbent for purification, which further improves the biological activity and storage stability of olive oil, so that the obtained olive oil has good storage stability and anti-wrinkle effect.
[0089] In comparison, since Comparative Examples 1-6 did not adopt the necessary technical solutions, they were significantly worse than Examples 1-3 in the corresponding performance tests. In Comparative Examples 1-4, enzymatic hydrolysis and specific fermentation bacteria were not used simultaneously, and Comparative Examples 5-6 did not use modified adsorbents for purification. It can be seen from the results that this led to a decrease in the performance of olive oil. The above experimental results further prove the importance of the technical solutions defined in the present invention for its technical effects.
[0090] The above is a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principles of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.
Claims
1. A method for preparing olive oil with repairing, soothing and anti-wrinkle effects, characterized in that: The following steps are involved: Step A1, removing impurities from olive fruits, then washing them with water, and then adding them to a crusher for crushing, sieving, and obtaining olive pulp; adding the olive pulp to a rotary evaporator for rotary evaporation, then adding water to mix evenly, and then placing them in a centrifuge for centrifugation to obtain a supernatant and olive pomace respectively; the supernatant is allowed to stand for stratification, and the upper oil phase is taken to obtain olive crude oil I; Step A2, mixing the olive pomace obtained in step A1 with water, performing ultrasonic treatment, then adding cellulase and pectinase for enzymolysis, sterilizing, and cooling to obtain a pomace pretreatment liquid; Step A3, inoculating fermentation bacteria into the pomace pretreatment liquid obtained in step A2 for fermentation, sterilizing and cooling after the fermentation to obtain pomace fermentation liquid; placing the pomace fermentation liquid in a centrifuge for centrifugation to obtain a supernatant; standing and stratifying, taking the upper oil phase to obtain olive crude oil II; Step A4, uniformly mixing the crude olive oil I obtained in step A1 and the crude olive oil II obtained in step A3, then adding a modified adsorbent, heating and stirring, cooling, filtering, and obtaining crude olive oil; vacuum deodorizing the crude olive oil, cooling, and obtaining the olive oil having the functions of repairing, soothing, and anti-wrinkle.
2. The method for preparing olive oil having the functions of repairing, soothing and anti-wrinkle according to claim 1, characterized in that: The following steps are involved: Step A1, removing impurities from olive fruits, then washing them with water, and then adding them to a crusher for crushing, and passing them through a 30-40 mesh screen to obtain olive pulp; adding the olive pulp to a rotary evaporator, rotary evaporating at 20-30° C. and 100-300 mbar for 30-50 minutes, then adding water to mix evenly, and then placing them in a centrifuge, centrifuging at 7000-9000 r / min for 2-4 minutes to obtain a supernatant and olive pomace respectively; the supernatant is allowed to stand for stratification, and the upper oil phase is taken to obtain olive crude oil I; Step A2, mixing the olive pomace obtained in step A1 with water, ultrasonicating for 20-30 min under the conditions of ultrasonic power of 150-250 W and ultrasonic frequency of 40-50 kHz, then adding cellulase and pectinase, adjusting the pH to 4.5-5.5, performing enzymolysis at 45-55° C. for 7-10 h, sterilizing at 115-125° C. for 10-20 min, and cooling to room temperature to obtain a pomace pretreatment liquid; Step A3, inoculating fermentation bacteria into the pomace pretreatment liquid obtained in step A2, fermenting at a constant temperature of 25-30° C. for 70-75 hours, sterilizing at 115-125° C. for 10-20 minutes after the fermentation, cooling to room temperature, and obtaining pomace fermentation liquid; placing the pomace fermentation liquid in a centrifuge, centrifuging at 7000-9000 r / min for 2-4 minutes, discarding the precipitate, and obtaining a supernatant; standing for stratification, taking the upper oil phase, and obtaining olive crude oil II; Step A4, mixing the crude olive oil I obtained in step A1 and the crude olive oil II obtained in step A3 evenly, then adding the modified adsorbent, stirring at 40-50° C. and 100-150 r / min for 40-60 min, cooling to room temperature, filtering to obtain crude olive oil; vacuum deodorizing the crude olive oil at 0.5-1 mbar and 160-180° C. for 2-4 h, cooling to room temperature, and obtaining the olive oil with repairing, soothing and anti-wrinkle properties.
3. The method for preparing olive oil having the functions of repairing, soothing and anti-wrinkle according to claim 1 or 2, characterized in that: The modified adsorbent is prepared by the following method: 25-40 parts by weight of natural zeolite powder and 15-30 parts by weight of natural diatomaceous earth are added to 150-300 parts by weight of sodium hydroxide aqueous solution, and then 3-5 parts by weight of sodium bicarbonate are added, heated and stirred, cooled, filtered, and dried to obtain an activated composite; 2-4 parts by weight of chitosan are added to 150-300 parts by weight of citric acid aqueous solution, and ultrasonic treatment is performed. Then, 3-5 parts by weight of hydrogen peroxide, 1.2-1.8 parts by weight of caffeic acid and 0.1-0.3 parts by weight of vitamin C are added in sequence under nitrogen protection, and the reaction is carried out in the dark. The mixture is precipitated with anhydrous ethanol, filtered and dried to obtain modified chitosan. 8-12 parts by weight of the activated complex and 1-2 parts by weight of the modified chitosan are evenly mixed to obtain a modified adsorbent.
4. The method for preparing olive oil having the functions of repairing, soothing and anti-wrinkle according to claim 3, characterized in that: The modified adsorbent is prepared by the following method: 25-40 parts by weight of natural zeolite powder and 15-30 parts by weight of natural diatomaceous earth are added to 150-300 parts by weight of 0.5-1.5wt% sodium hydroxide aqueous solution, and ultrasonicated for 30-50 minutes at an ultrasonic power of 100-200W and an ultrasonic frequency of 20-30kHz, and then 3-5 parts by weight of sodium bicarbonate are added, and stirred at 55-65°C and 150-300r / min for 40-60 minutes, cooled to room temperature, filtered, and dried to obtain an activated composite; 2-4 parts by weight of chitosan are added to 150-300 parts by weight of 2-4wt% citric acid aqueous solution, and ultrasonicated for 15-30 minutes under the conditions of ultrasonic power of 100-200W and ultrasonic frequency of 20-30kHz, and then 3-5 parts by weight of 18-22wt% hydrogen peroxide, 1.2-1.8 parts by weight of caffeic acid and 0.1-0.3 parts by weight of vitamin C are added in sequence under nitrogen protection, reacted at 25-30°C in the dark for 10-15 hours, precipitated with anhydrous ethanol, filtered, and dried to obtain modified chitosan; 8-12 parts by weight of the activated complex and 1-2 parts by weight of the modified chitosan are evenly mixed to obtain a modified adsorbent.
5. The method for preparing olive oil having the functions of repairing, soothing and anti-wrinkle according to claim 1 or 2, characterized in that: In step A2, the amount of cellulase added is 0.5-0.7wt% of the weight of the olive pomace, and the amount of pectinase added is 0.3-0.5wt% of the weight of the olive pomace.
6. The method for preparing the olive oil having the functions of repairing, soothing and anti-wrinkle according to claim 1 or 2, characterized in that: The inoculum size of the fermentation bacteria in step A3 is 1×10 8 -2×10 8 cfu / mL pomace pretreatment solution.
7. The method for preparing olive oil having the functions of repairing, soothing and anti-wrinkle according to claim 1 or 2, characterized in that: The fermentation bacteria in step A3 are composed of Hansenula anomalosa and Bacillus amyloliquefaciens, and the ratio of the Hansenula anomalosa to the Bacillus amyloliquefaciens is 1:1-3.
8. The method for preparing olive oil having the functions of repairing, soothing and anti-wrinkle according to claim 1 or 2, characterized in that: The amount of the modified adsorbent added in step A4 is 1.5-3wt% of the total weight of the crude olive oil.
9. An olive oil with repairing, soothing and anti-wrinkle properties, characterized in that: Prepared according to the method according to any one of claims 1 to 8.
10. Use of the olive oil with repairing, soothing and anti-wrinkle effects according to claim 9 in the preparation of cosmetics.
Citation Information
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