Olive oil with repairing, soothing and anti-wrinkle properties, preparation method and application thereof
By optimizing the centrifugation process and combining enzymatic fermentation with modified adsorbent treatment, the problems of active ingredient loss and insufficient stability in existing olive oil preparation have been solved, and the high biological activity and stability of olive oil have been achieved, making it suitable for repair and anti-wrinkle effects in cosmetics.
Patent Information
- Application Number
- CN202411981707.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-30
- Publication Date
- 2025-09-26
- Estimated Expiration
- 2044-12-30
AI Technical Summary
Existing olive oil preparation methods have problems such as high requirements for fruit quality, low oil yield, high cost, high equipment maintenance cost, and ingredient loss caused by the use of chemical solvents. It is difficult to maximize the retention of natural activity and improve quality.
By optimizing the centrifugation process, adding enzymatic hydrolysis and fermentation treatment to the pomace, and using modified adsorbents for purification, including enzymatic hydrolysis with cellulase and pectinase, fermentation with abnormal Hansenula and Bacillus amyloliquefaciens, and treatment with a multifunctional adsorbent composed of modified zeolite powder, diatomaceous earth and modified chitosan, the biological activity and stability of olive oil are improved.
It improves the biological activity and storage stability of olive oil, enhances its antioxidant and anti-wrinkle effects, maintains its fresh fruity scent and clear transparency, and is suitable for repairing and soothing effects in cosmetics.
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Abstract
Description
Technical Field
[0001] The present 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 considered a treasure of Mediterranean culinary culture. This natural oil is rich in monounsaturated fatty acids and a variety of health-promoting antioxidants, such as vitamin E and polyphenols. These active ingredients not only help maintain cardiovascular health but also provide the foundation for olive oil's cosmetic applications. The antioxidants in olive oil effectively fight free radicals, reducing damage to skin cells and thereby slowing the aging process. Olive oil's benefits for the skin extend beyond its anti-aging properties. It also deeply moisturizes the skin, helping to maintain its moisture barrier and increase its softness and elasticity. Olive oil also acts as a moisturizer, helping to restore the skin's natural radiance while promoting cell renewal. The squalene component in olive oil has a similar structure to human sebum, making it suitable for sensitive or dry skin. By enhancing the skin's self-repairing ability, olive oil helps improve skin texture and reduce the appearance of fine lines and wrinkles. Furthermore, olive oil protects the skin from UV rays and other environmental factors, making it a versatile and gentle skincare ingredient.
[0003] At present, the main methods for preparing olive oil in the existing technology 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 of the olives. In particular, extra virgin olive oil has the advantages of high quality and rich 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 through organic solvents. This method can increase the oil yield and is relatively low in cost.
[0004] Although each of the above methods has its own unique advantages, there are also some shortcomings. For example, the cold pressing method has very 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 lead to the partial loss of natural antioxidant components in olive oil. Therefore, there is an urgent need to provide a method for preparing olive oil, which can maximize the retention of the natural activity of olive oil and improve its 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. The olive oil can be used in cosmetics to have 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.) fruit, then rinsing with water, crushing in a crusher, and sieving to obtain olive pulp; adding the olive pulp to a rotary evaporator for rotary evaporation, then adding water and mixing evenly, and then centrifuging in a centrifuge to obtain a supernatant and olive pomace, respectively; allowing the supernatant to stand for separation, and collecting the upper oil phase to obtain crude olive 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 is completed to obtain pomace fermentation liquid; placing the pomace fermentation liquid in a centrifuge for centrifugation to obtain a supernatant; standing to separate layers, and taking the upper oil phase to obtain olive crude oil II;
[0011] Step A4: uniformly mix the crude olive oil I obtained in step A1 and the crude olive oil II obtained in step A3, then add a modified adsorbent, heat and stir, cool, and filter to obtain crude olive oil; vacuum deodorize the crude olive oil, cool, and obtain the olive oil with the repairing, soothing, and anti-wrinkle properties.
[0012] Preferably, a method for preparing olive oil having the functions of repairing, soothing and anti-wrinkle comprises the following steps:
[0013] Step A1: removing impurities from fresh olive fruits, 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 and mixing evenly, and then placing it in a centrifuge and centrifuging it at 7000-9000 r / min for 2-4 minutes to obtain a supernatant and olive pomace, respectively; allowing the supernatant to stand for stratification, and taking the upper oil phase to obtain olive crude oil I; wherein, rotary evaporation can cause small oil droplets in the pulp to merge into large oil droplets, which helps to quickly separate the pomace in a subsequent centrifugation operation;
[0014] Step A2, mixing the olive pomace obtained in step A1 with water, ultrasonicating for 20-30 minutes at an ultrasonic power of 150-250 W and an 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 hours, sterilizing at 115-125° C. for 10-20 minutes, 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, and cooling to room temperature to obtain pomace fermentation liquid; placing the pomace fermentation liquid in a centrifuge, centrifuging at 7000-9000 r / min for 2-4 minutes, discarding the precipitate to obtain a supernatant; standing to separate, taking the upper oil phase to obtain olive crude oil II;
[0016] Step A4: uniformly mix the crude olive oil I obtained in step A1 and the crude olive oil II obtained in step A3, then add the modified adsorbent, stir at 40-50° C. and 100-150 r / min for 40-60 min, cool to room temperature, and filter to obtain crude olive oil; vacuum deodorize the crude olive oil at 0.5-1 mbar and 160-180° C. for 2-4 h, and cool to room temperature to obtain 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 0.5-0.7 wt% of the weight of the olive pomace, and the amount of pectinase added is 0.3-0.5 wt% 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 anomala and Bacillus amyloliquefaciens, and the ratio of the number of Hansenula anomala to Bacillus amyloliquefaciens is 1:1-3.
[0022] Preferably, the number of Hansenula anomala is CICC 32234, and the number of Bacillus amyloliquefaciens is CICC 20164, and they are purchased from the China Industrial Microorganism Culture Collection Center.
[0023] The present invention optimizes the centrifugation process and adds enzymatic hydrolysis and fermentation with specific fermentation bacteria to reprocess the olive pomace, thereby further improving the biological activity and storage stability of olive oil, so that the olive oil maintains a fresh fruity aroma, 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 complex polysaccharide structures such as cellulose and pectin in the pomace through the enzymatic hydrolysis of cellulase and pectinase, releasing more oil and active ingredients, such as polyphenols, vitamin E, and other fat-soluble antioxidants. These ingredients 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 Hansenula anomala helps to increase the extraction efficiency and biological activity of olive oil. Bacillus amyloliquefaciens can secrete a variety of enzymes, such as proteases, lipases, and amylases, which can further decompose macromolecules in the pomace, releasing and converting them into more bioactive substances, such as squalene, β-carotene, and vitamins. These ingredients further enhance the antioxidant and anti-wrinkle effects of olive oil. Hansenula anomala has good metabolic activity and can assist Bacillus amyloliquefaciens in metabolizing carbohydrates in the pomace during the fermentation process and produce a variety of beneficial metabolites. These substances 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 aroma 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 a sodium hydroxide aqueous solution, and ultrasonically treated. 3-5 parts by weight of sodium bicarbonate are then added, heated and stirred, cooled, filtered, and dried to obtain an activated complex;
[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. The reaction is protected from light, and 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, which can effectively adsorb impurities, pigments and odor substances in olive oil. At the same time, the alkaline environment they provide helps 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 scavenge free radicals, inhibit oxidation reactions, and further reduce peroxide value and acid value. The above-mentioned activated complex and modified chitosan work synergistically to form a multifunctional adsorption system that can both physically adsorb impurities and 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 a 0.5-1.5 wt% sodium hydroxide aqueous solution, and ultrasonicated for 30-50 minutes at an ultrasonic power of 100-200 W and an ultrasonic frequency of 20-30 kHz. Then, 3-5 parts by weight of sodium bicarbonate are added, and the mixture is stirred at 55-65° C. and 150-300 rpm for 40-60 minutes. The mixture is cooled to room temperature, filtered, and dried to obtain an activated complex.
[0032] 2-4 parts by weight of chitosan are added to 150-300 parts by weight of a 2-4wt% citric acid aqueous solution, and ultrasonicated for 15-30 minutes at an ultrasonic power of 100-200W and an ultrasonic frequency of 20-30kHz. 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. The mixture is 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 are evenly mixed with 1-2 parts by weight of the modified chitosan to obtain a modified adsorbent.
[0033] The present 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, etc.
[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 properties. By optimizing the centrifugation process and adding enzymatic hydrolysis and fermentation to the pomace, the bioactivity of the olive oil is further enhanced. Purification using a specific modified adsorbent improves the stability of the olive oil. The present invention also provides the use of the olive oil in the preparation of cosmetics, which exhibit excellent repairing, soothing, and anti-wrinkle properties.
[0037] 2. The present invention adds enzymatic hydrolysis and fermentation with specific fermentative bacteria to reprocess the olive pomace, further improving the biological activity and storage stability of olive oil. The enzymatic hydrolysis of cellulase and pectinase can effectively decompose complex polysaccharide structures such as cellulose and pectin in the pomace, facilitating the release of 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 convert it into a variety of bioactive substances, such as squalene, β-carotene and vitamins. These active substances further enhance the antioxidant and anti-wrinkle effects of olive oil.
[0038] 3. The present invention utilizes a specific modified adsorbent, creating a multifunctional adsorption system through the synergistic action of multiple components. This system can both physically adsorb impurities and chemically bind harmful substances, further enhancing the storage stability of olive oil. The activated complex, with its rich pore structure and large specific surface area, effectively physically adsorbs impurities, pigments, and odorous substances from olive oil. The alkaline environment it provides helps neutralize acidic components and reduce the acid value. The modified chitosan enhances its adsorption capacity and antioxidant activity, not only absorbing various impurities in olive oil but also effectively scavenging free radicals and inhibiting oxidation reactions, further reducing the peroxide value and acid value. DETAILED DESCRIPTION
[0039] The following is a clear and complete description of the technical solutions in the embodiments of the present invention. Obviously, the embodiments described are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making any creative efforts 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, rinse them with water, and then add them to a crusher for crushing, and pass them through a 35-mesh sieve to obtain olive pulp; add the olive pulp to a rotary evaporator, and rotary evaporate it 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 it in a centrifuge and centrifuge it at 8000 r / min for 2.5 minutes to obtain a supernatant and olive pomace respectively; place the supernatant in a separatory funnel and let it stand for 12 hours, and take the upper oil phase to 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 the mixture under conditions of an ultrasonic power of 200 W and an ultrasonic frequency of 45 kHz for 25 minutes, 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 Hansenula anomala and Bacillus amyloliquefaciens, and the number ratio of the Hansenula anomala to Bacillus amyloliquefaciens is 1:2; after the fermentation, the liquid is sterilized at 121° C. for 15 minutes and cooled to room temperature to obtain a pomace fermentation liquid; the pomace fermentation liquid is placed in a centrifuge, centrifuged at 8000 r / min for 2.5 minutes, and the precipitate is discarded to obtain a supernatant; the supernatant is placed in a separatory funnel and allowed to stand for 12 hours, and the upper oil phase is collected to obtain olive crude oil II; wherein the Hansenula anomala is numbered CICC 32234 and the Bacillus amyloliquefaciens is numbered CICC 20164, and they are purchased from the China Industrial Microbiological Culture Collection Administration Center;
[0045] Step A4: uniformly mix the crude olive oil I obtained in step A1 and the crude olive oil II obtained in step A3, then add a modified adsorbent in an amount of 2 wt% of the total weight of the crude olive oil, stir at 45° C. and 120 r / min for 50 min, cool to room temperature, and filter to obtain crude olive oil; deodorize the crude olive oil in a vacuum at 0.5 mbar and 180° C. for 3 h, and cool to room temperature to obtain the olive oil with repairing, soothing, and anti-wrinkle properties.
[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 were added to 200 parts by weight of a 1 wt% sodium hydroxide aqueous solution, and ultrasonicated for 40 minutes at an ultrasonic power of 100 W and an ultrasonic frequency of 25 kHz. Then, 4 parts by weight of sodium bicarbonate were added, and the mixture was stirred at 60° C. and 200 rpm for 50 minutes. The mixture was cooled to room temperature, filtered, and dried to obtain an activated composite; wherein the average particle size of the natural zeolite powder was 500 mesh, and the average particle size of the natural diatomaceous earth was 800 mesh;
[0048] 2.5 parts by weight of chitosan are added to 200 parts by weight of a 3% by weight citric acid aqueous solution and ultrasonically treated at an ultrasonic power of 100 W and an ultrasonic frequency of 25 kHz for 20 minutes. Then, 4 parts by weight of 20% by weight 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. The mixture is reacted at 27°C in the dark for 12 hours, precipitated with anhydrous ethanol, filtered, and dried to obtain a modified chitosan. 10 parts by weight of the activated complex and 1.5 parts by weight of the modified chitosan are uniformly mixed to obtain a modified adsorbent. The chitosan has an average molecular weight of 100,000 and a degree of deacetylation of 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, rinse them with water, and then add them to a crusher for crushing, and pass them through a 30-mesh sieve to obtain olive pulp; add the olive pulp to a rotary evaporator, and evaporate it at 20° C. and 100 mbar for 50 minutes, then add water and mix them evenly, wherein the amount of water added is 100wt% of the weight of the olive pulp, and then place it in a centrifuge and centrifuge it at 7000 r / min for 4 minutes to obtain a supernatant and olive pomace respectively; place the supernatant in a separatory funnel and let it stand for 10 hours, and take the upper oil phase to 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 the mixture under conditions of an ultrasonic power of 150 W and an ultrasonic frequency of 40 kHz for 30 minutes, 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 400 u / mg, and the enzyme activity of the pectinase is 35 u / 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 Hansenula anomala and Bacillus amyloliquefaciens, and the number ratio of the Hansenula anomala to Bacillus amyloliquefaciens is 1:1; after the fermentation is completed, the liquid is sterilized at 115°C for 20 minutes and cooled to room temperature to obtain a pomace fermentation liquid; the pomace fermentation liquid is placed in a centrifuge, centrifuged at 7000 r / min for 4 minutes, and the precipitate is discarded to obtain a supernatant; the supernatant is placed in a separatory funnel and allowed to stand for 10 hours, and the upper oil phase is collected to obtain olive crude oil II; wherein the Hansenula anomala is numbered CICC 32234 and the Bacillus amyloliquefaciens is numbered CICC 20164, and they are purchased from the China Industrial Microbiological Culture Collection Center;
[0054] Step A4: uniformly mix the crude olive oil I obtained in step A1 and the crude olive oil II obtained in step A3, then add a modified adsorbent in an amount of 1.5 wt% based on the total weight of the crude olive oil; stir at 40° C. and 100 rpm for 40 minutes, cool to room temperature, and filter to obtain crude olive oil; and vacuum deodorize the crude olive oil at 0.5 mbar and 160° C. for 4 hours, cool to room temperature, and obtain the olive oil having the properties 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, rinse them with water, and then add them to a crusher for crushing, and pass them through a 40-mesh sieve to obtain olive pulp; add the olive pulp to a rotary evaporator, and evaporate it at 30° C. and 300 mbar for 30 minutes, then add water and mix them evenly, wherein the amount of water added is 120wt% of the weight of the olive pulp, and then place it in a centrifuge and centrifuge it at 9000 r / min for 2 minutes to obtain a supernatant and olive pomace respectively; place the supernatant in a separatory funnel and let it stand for 15 hours, and take the upper oil phase to 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 the mixture under conditions of an ultrasonic power of 250 W and an ultrasonic frequency of 50 kHz for 20 minutes, then adding cellulase and pectinase, wherein the amount of the cellulase added is 0.7 wt% of the weight of the olive pomace, and the amount of the pectinase added is 0.5 wt% 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 400 u / mg, and the enzyme activity of the pectinase is 35 u / 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 Hansenula anomala and Bacillus amyloliquefaciens, and the number ratio of the Hansenula anomala to Bacillus amyloliquefaciens is 1:3; after the fermentation is completed, the liquid is sterilized at 125°C for 10 minutes and cooled to room temperature to obtain a pomace fermentation liquid; the pomace fermentation liquid is placed in a centrifuge, centrifuged at 9000 r / min for 2 minutes, and the precipitate is discarded to obtain a supernatant; the supernatant is placed in a separatory funnel and allowed to stand for 15 hours, and the upper oil phase is collected to obtain olive crude oil II; wherein the Hansenula anomala is numbered CICC 32234 and the Bacillus amyloliquefaciens is numbered CICC 20164, and they are purchased from the China Industrial Microbiological Culture Collection Center;
[0061] Step A4: uniformly mix the crude olive oil I obtained in step A1 and the crude olive oil II obtained in step A3, then add a modified adsorbent, wherein the amount of the modified adsorbent added is 3wt% of the total weight of the crude olive oil, stir at 50°C and 150r / min for 60min, cool to room temperature, and filter to obtain crude olive oil; deodorize the crude olive oil in a vacuum at 1mbar and 180°C for 2h, and cool to room temperature to obtain the olive oil with repairing, soothing, and anti-wrinkle properties.
[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, ultrasonically treated for 25 minutes at an ultrasonic power of 200 W and an 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 method for preparing the olive oil with repairing, soothing and anti-wrinkle properties is different, specifically as follows: placing the pomace pretreatment liquid in a centrifuge and centrifuging it at 8000 r / min for 2.5 min, discarding the precipitate to obtain a supernatant; placing the supernatant in a separatory funnel and letting it stand for 12 h, 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 the function of repairing, soothing and anti-wrinkle is different in step A3, which is as follows: fermentation bacteria are inoculated into the pomace pre-treated 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 Hansenula anomala; after fermentation, 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 and centrifuged at 8000 r / min for 2.5 minutes, and the precipitate is discarded to obtain a supernatant; the supernatant is placed in a separatory funnel and allowed to stand for 12 hours, and the upper oil phase is collected to obtain olive crude oil II; wherein, Hansenula anomala is numbered CICC 32234 and purchased from the China Industrial Microbiological Culture Collection Administration 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 the function of repairing, soothing and anti-wrinkle is different in step A3, which is as follows: fermentation bacteria are inoculated into the pomace pre-treated 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 a pomace fermentation liquid; the pomace fermentation liquid is placed in a centrifuge, centrifuged at 8000 r / min for 2.5 minutes, and the precipitate is discarded to obtain a supernatant; the supernatant is placed in a separatory funnel and allowed to stand for 12 hours, and the 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 Administration 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 properties 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 uniformly mixed, and then a modified adsorbent is added, wherein the amount of the modified adsorbent added is 2 wt% of the total weight of the crude olive oil. The mixture is stirred at 45°C and 120 r / min for 50 min, cooled to room temperature, and filtered to obtain crude olive oil; the crude olive oil is vacuum deodorized at 0.5 mbar and 180°C for 3 h, and cooled to room temperature to obtain the olive oil with repairing, soothing and anti-wrinkle properties.
[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 were added to 200 parts by weight of a 1 wt% sodium hydroxide aqueous solution, and ultrasonicated for 40 minutes at an ultrasonic power of 100 W and an ultrasonic frequency of 25 kHz. Then, 4 parts by weight of sodium bicarbonate were added, and the mixture was stirred at 60° C. and 200 rpm for 50 minutes. The mixture was cooled to room temperature, filtered, and dried to obtain an activated composite; wherein the average particle size of the natural zeolite powder was 500 mesh, and the average particle size of the natural diatomaceous earth was 800 mesh;
[0075] 10 parts by weight of the activated complex was mixed with 1.5 parts by weight of chitosan to obtain a modified adsorbent. The chitosan had an average molecular weight of 100,000 and a degree of deacetylation of 90%.
[0076] Comparative Example 6
[0077] This comparative example differs from Example 1 in that step A4 of the preparation method for the olive oil with repairing, soothing, and anti-wrinkle properties is different and is specifically as follows: The crude olive oil I obtained in step A1 and the crude olive oil II obtained in step A3 are uniformly mixed, and then an adsorbent, activated carbon, is added in an amount of 2 wt% of the total weight of the crude olive oil. The mixture is stirred at 45°C and 120 rpm for 50 minutes, cooled to room temperature, and filtered to obtain crude olive oil. The crude olive oil is then vacuum deodorized at 0.5 mbar and 180°C for 3 hours, and cooled to room temperature to obtain the olive oil with repairing, soothing, and anti-wrinkle properties. The activated carbon is commercially available coconut shell powdered activated carbon with an average particle size of 300 mesh.
[0078] Performance Testing
[0079] 1. The olive oils prepared in Examples 1-3 and Comparative Examples 1-6 were stored at room temperature in the dark for one month. The transparency and odor of the olive oils were observed, and the insoluble impurity content, peroxide value, and acid value were measured according to the method in GB / T 15688-2008, GB 5009.227-2016, and GB 5009.229-2016, respectively. The test results are shown in Table 1.
[0080] Table 1: Storage stability test results of olive oil
[0081]
[0082]
[0083] 2. Take 6 wt% of olive oil, 7 wt% of glycerol, 3 wt% of 1,3-propylene glycol, 1.5 wt% of isopropyl palmitate, 0.2 wt% of carbomer prepared in Examples 1-3 and Comparative Examples 1-6 above, mix them to make cosmetic samples, and perform efficacy tests.
[0084] The test method involved 90 female volunteers aged 30-40 with no skin conditions. They were randomly divided into nine groups of 10 each and each group was given the aforementioned cosmetic samples. Specifically, the volunteers applied the cosmetic samples to the left half of their face, while the right half remained unapplied as a blank control. The samples were applied once in the morning and once in the evening for 45 consecutive days. At the beginning and end of the trial, the volunteers' skin was analyzed using a skin analyzer to assess the improvement in cheek skin elasticity and fine lines around the eyes. "+" indicates an increase, while "-" indicates a decrease. The results are shown in Table 2.
[0085] Table 2: Results of efficacy tests on olive oil for cosmetics
[0086]
[0087]
[0088] The above test results show that the olive oils prepared in Examples 1-3 maintain excellent quality after storage for a period of time, exhibiting a fresh, fruity aroma, clear transparency, low peroxide value, and low acid value. Furthermore, they exhibit excellent anti-wrinkle and repairing properties when used in cosmetics. The olive oil prepared in Example 1, in particular, exhibits the most outstanding overall performance. This is because the present invention improves the olive oil preparation process, adding enzymatic hydrolysis and fermentation steps to further process the pomace, and employing a specific modified adsorbent for purification, further enhancing the bioactivity and storage stability of the olive oil, resulting in the olive oil having excellent storage stability and anti-wrinkle properties.
[0089] In comparison, Comparative Examples 1-6 did not adopt the necessary technical solutions, resulting in their corresponding performance tests being significantly worse than Examples 1-3. In Comparative Examples 1-4, enzymatic hydrolysis and specific fermentation bacteria fermentation treatment were not used simultaneously, and Comparative Examples 5-6 did not use modified adsorbents for purification. The results show that this led to a decrease in the performance of olive oil. The above experimental results further demonstrate 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 within the scope of protection of the present invention.
Claims
1. A method for preparing olive oil with repairing, soothing and anti-wrinkle properties, characterized in that: The following steps are involved: Step A1, removing impurities from the olive fruit, then rinsing it with water, adding it to a crusher for crushing, and sieving to obtain olive pulp; adding the olive pulp to a rotary evaporator for rotary evaporation, then adding water and mixing evenly, and then centrifuging it in a centrifuge to obtain a supernatant and olive pomace respectively; the supernatant is allowed to stand for separation, and the upper oil phase is collected 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 is completed to obtain pomace fermentation liquid; placing the pomace fermentation liquid in a centrifuge for centrifugation to obtain a supernatant; standing to separate layers, and taking the upper oil phase to obtain olive crude oil II; The fermentation bacteria in step A3 are composed of Hansenula anomalosa numbered CICC 32234 and Bacillus amyloliquefaciens numbered CICC 20164, and the ratio of Hansenula anomalosa to Bacillus amyloliquefaciens is 1:1-3; Step A4: uniformly mix the crude olive oil I obtained in step A1 and the crude olive oil II obtained in step A3, then add a modified adsorbent, heat and stir, cool, and filter to obtain crude olive oil; vacuum deodorize the crude olive oil, cool, and obtain the olive oil with the repairing, soothing, and anti-wrinkle properties.
2. The method for preparing olive oil having the functions of repairing, soothing and anti-wrinkle according to claim 1, 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 a sodium hydroxide aqueous solution, and ultrasonically treated. 3-5 parts by weight of sodium bicarbonate are then added, heated and stirred, cooled, filtered, and dried to obtain an activated complex; 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. The reaction is protected from light, and 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.
3. 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 the olive fruit, then rinsing it with water, and then adding it to a crusher for crushing, and passing it 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 and mixing it evenly, and then placing it in a centrifuge and 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 separation, 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 minutes at an ultrasonic power of 150-250 W and an 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 hours, sterilizing at 115-125° C. for 10-20 minutes, 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, and cooling to room temperature to obtain pomace fermentation liquid; placing the pomace fermentation liquid in a centrifuge, centrifuging at 7000-9000 r / min for 2-4 minutes, discarding the precipitate to obtain a supernatant; standing to separate, taking the upper oil phase to obtain olive crude oil II; The fermentation bacteria in step A3 are composed of Hansenula anomalosa numbered CICC 32234 and Bacillus amyloliquefaciens numbered CICC 20164, and the ratio of Hansenula anomalosa to Bacillus amyloliquefaciens is 1:1-3; Step A4: uniformly mix the crude olive oil I obtained in step A1 and the crude olive oil II obtained in step A3, then add the modified adsorbent, stir at 40-50° C. and 100-150 r / min for 40-60 min, cool to room temperature, and filter to obtain crude olive oil; vacuum deodorize the crude olive oil at 0.5-1 mbar and 160-180° C. for 2-4 h, and cool to room temperature to obtain the olive oil with repairing, soothing, and anti-wrinkle properties.
4. The method for preparing olive oil having the functions of repairing, soothing and anti-wrinkle according to any one of claims 1 to 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 a 0.5-1.5 wt% sodium hydroxide aqueous solution, and ultrasonicated for 30-50 minutes at an ultrasonic power of 100-200 W and an ultrasonic frequency of 20-30 kHz. Then, 3-5 parts by weight of sodium bicarbonate are added, and the mixture is stirred at 55-65° C. and 150-300 rpm for 40-60 minutes. The mixture is cooled to room temperature, filtered, and dried to obtain an activated complex. 2-4 parts by weight of chitosan are added to 150-300 parts by weight of a 2-4wt% citric acid aqueous solution, and ultrasonicated for 15-30 minutes at an ultrasonic power of 100-200W and an ultrasonic frequency of 20-30kHz. 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. The mixture is 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 are evenly mixed with 1-2 parts by weight of the modified chitosan 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, 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 olive oil having the functions of repairing, soothing and anti-wrinkle according to claim 1, 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, characterized in that: The amount of the modified adsorbent added in step A4 is 1.5-3 wt % of the total weight of the crude olive oil.
8. An olive oil with the functions of repairing, soothing and anti-wrinkle, characterized in that: Prepared according to the method according to any one of claims 1 to 7.
9. Use of the olive oil having the repairing, soothing and anti-wrinkle properties according to claim 8 in the preparation of cosmetics.
Citation Information
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