Preparation method and application of colored grease

Abstract

The invention provides a preparation method and application of colored grease, and belongs to the technical field of biological fermentation. The preparation method comprises the following steps: (1) mixing plants and vegetable fat, adding a multi-element enzyme system, and stirring to obtain a mixed solution of the plants and the vegetable fat; and (2) separating the mixed solution, taking an oil phase in the mixed solution to obtain a crude grease product, and further purifying the crude grease product to obtain the colored grease, the multi-element enzyme system comprises cellulase, pectinase and hemicellulase. The mass ratio of the plant to the vegetable fat is 1: (3-100); the mass of the cellulase, the mass of the pectinase and the mass of the hemicellulase are respectively 0.1-1.5% of the total mass of the plant and the vegetable fat. The colored grease obtained through the method has good color stability, meanwhile, the colored grease obtained through the method contains plant active ingredients, and the effect of the grease in cosmetics can be enhanced.

Description

Technical Field

[0001] The present invention relates to the technical field of biological fermentation, and particularly relates to a preparation method and application of colored oil. Background Art

[0002] In the field of cosmetic formulation applications, oils are an extremely important and crucial part, and are widely used in products such as makeup remover oils, facial serums, creams, and essential oils. Since in our skin structure, both the sebum film and the stratum corneum are lipophilic and not hydrophilic, oil-based skin care products are more likely to penetrate into the skin compared to water-based skin care products. Therefore, "nourishing the skin with oil" has become a new type of skin care method that is popular in various cosmetics.

[0003] Consumers have many requirements for the oils used in cosmetics, such as a pleasant skin feel, good stability, and efficacy. In addition, the color of the oil is also a feature that attracts consumers' attention. However, due to the relatively strong non-polarity of oils, the natural pigments that can be added to oils are relatively limited at present. Commonly used natural pigments include lycopene, carotene, zeaxanthin, lutein, etc. After adding these pigments to the oil, it often fades under strong light and cannot maintain a stable state. Therefore, oils that can maintain color stability have attracted the attention of users. Summary of the Invention

[0004] In view of the above problems existing in the prior art, the present invention provides a preparation method and application of colored oil. The colored oil obtained by the method of the present invention has relatively good color stability, and at the same time, the colored oil obtained by this method has plant active ingredients, which can enhance the efficacy of the oil in cosmetics.

[0005] The technical solution of the present invention is as follows: A preparation method of colored oil, the preparation method comprising the following steps: (1) Mixing a plant with a plant oil and adding a multi-enzyme system, and stirring to obtain a mixed solution of the plant and the plant oil; (2) Separating the mixed solution, taking the oil phase therein to obtain a crude oil product, and further purifying the crude oil product to obtain the colored oil; The multi-enzyme system includes cellulase, pectinase, and hemicellulase.

[0006] Furthermore, the vegetable oils include soybean oil, coconut oil, sunflower seed oil, jojoba oil, rosehip oil, grape seed oil, almond oil, Limnanthes alba seed oil, macadamia nut oil, olive fruit oil, Aleurites moluccana seed oil, camellia seed oil, Prinsepia utilis Royle oil, seabuckthorn seed oil, peony seed oil, European hazelnut oil, rice germ oil, wheat germ oil, borage seed oil, safflower oil, Echium plantagineum seed oil, Vaccinium myrtillus seed oil, Adansonia digitata seed oil, palm fruit oil, Chilean hazelnut oil, Irvingia gabonensis oil, flueggea oil, olive shell oil, etc.; Furthermore, the plants include Lithospermum erythrorhizon, chamomile, avocado, camellia, saffron, Centella asiatica, ginseng, chrysanthemum, rose, rhododendron, Caulerpa lentillifera, peony, madder, turmeric, lavender, etc.

[0007] Furthermore, when preparing the colored oil, the selected vegetable oil can be from the used plant or not. For example, when the selected vegetable oil is sunflower seed oil, the used plants can be Lithospermum erythrorhizon and chamomile.

[0008] Preferably, in step (1), the mass ratio of the plant to the vegetable oil is 1:3 - 100; the masses of the cellulase, pectinase, and hemicellulase are respectively 0.1 - 1.5% of the total mass of the plant and the vegetable oil.

[0009] Preferably, during the stirring in step (1), the temperature is 20 - 120°C and the stirring time is 1 - 10 h.

[0010] Preferably, the methods for separating the mixed liquid in step (2) include static separation, suction filtration separation, plate and frame separation, or centrifugal separation; the methods for further purifying the crude oil product include filtration and centrifugation.

[0011] Furthermore, in the method for further purifying the crude oil product, the filtration can be carried out by suction filtration to remove the plant residues in the crude oil product; during centrifugation, 0.3 - 5 wt% of anhydrous sodium sulfate can be added first, and then centrifuged at 8000 - 12000 rpm for 5 - 20 min to remove the anhydrous sodium sulfate, and the supernatant is the colored oil.

[0012] Preferably, the step of separating the mixed liquid in step (2) can be replaced by extraction with a supercritical system, and the extraction pressure of the supercritical system is 15 - 30 MPa and the extraction temperature is 30 - 70°C.

[0013] Preferably, the preparation method further includes a step of fermenting the crude oil product obtained in step (2), and the fermentation process includes the following steps: S1. Cultivate the microbial seed liquid, the cultivation temperature is 30 - 45°C, and the cultivation time is 5 - 30 h; S2. Inoculate the microbial seed liquid into the fermentation medium for fermentation culture; S3. Then add the crude oil product obtained in step (2) and continue the fermentation culture; after the fermentation is completed, centrifuge to obtain the oil phase, and then carry out subsequent purification steps.

[0014] Preferably, the microorganisms described in step S1 include but are not limited to lactic acid bacteria, bacillus, and yeast; the fermentation culture temperature described in step S2 is 30-45 °C, and the culture time is 2-10 h; the continued fermentation culture temperature described in step S3 is 15-45 °C, and the culture time is 8-60 h.

[0015] Preferably, the mass of the microbial seed liquid described in step S2 accounts for 1-10% of the fermentation medium; the mass of the crude oil product described in step S3 accounts for 50-200% of the fermentation medium; Furthermore, the medium for culturing the microbial seed liquid in step S1 is MRS medium or LB medium; Furthermore, the fermentation medium described in step S2 is: glucose 15-30 g / L, soybean extract 15-30 g / L, corn flour 5-15 g / L, whey powder 20-40 g / L.

[0016] Furthermore, the centrifugation in step S3 is carried out at 8000-12000 rpm for 5-20 min.

[0017] The present invention also provides the application of the colored oil obtained by the preparation method in the preparation of cosmetics.

[0018] The present invention further provides a cosmetic, which includes the colored oil obtained by the preparation method and cosmetically acceptable excipients.

[0019] The beneficial technical effects of the present invention are as follows: (1) The colored oil of the present invention is obtained by mixing plant oils and plants, and can extract the effective active ingredients in the plants, which can bring antioxidant, anti-wrinkle and other effects when used in cosmetics. The present invention uses a multi-enzyme system for treatment to improve the extraction efficiency.

[0020] (2) The present invention uses a supercritical extraction system to extract the effective components in plants, thereby enhancing the color of the plant oil. The co-fermentation of microbial strains, plant oils and plants enhances the stability of the oil color, so that the color of the colored oil can be stably present for a long time. Description of the Drawings

[0021] Figure 1 is the determination result of the antioxidant ability of lithospermum essence oil; Figure 2It is the determination result of the makeup remover effect of the Lithospermum erythrorhizon plant extract cleansing oil. Specific Embodiments

[0022] The present invention will be specifically described below in conjunction with the accompanying drawings and embodiments. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without creative efforts shall fall within the protection scope of the present invention.

[0023] Basic Comparative Example 1: Lithospermum erythrorhizon essence oil is obtained by simply mixing sunflower seed oil and Lithospermum erythrorhizon Taking Lithospermum erythrorhizon as an example, Lithospermum erythrorhizon is mixed with sunflower seed oil. The ratio of Lithospermum erythrorhizon to sunflower seed oil is 1:20. Stir at 50 °C for 2 h, and then let it stand for 5 h to separate Lithospermum erythrorhizon from sunflower seed oil. Take the upper oil phase to obtain a crude oil product, and further filter it to completely remove the Lithospermum erythrorhizon residue. Add 3 wt% of anhydrous sodium sulfate to the filtrate, and centrifuge at 10000 rpm for 10 min to remove anhydrous sodium sulfate. The supernatant after centrifugation is the Lithospermum erythrorhizon essence oil colored oil. The Lithospermum erythrorhizon essence oil obtained by this process is named Lithospermum erythrorhizon essence oil I.

[0024] Example 1: Preparation of Lithospermum erythrorhizon essence oil by treating the mixture of sunflower seed oil and Lithospermum erythrorhizon with a multi-enzyme system Taking Lithospermum erythrorhizon as an example, Lithospermum erythrorhizon is mixed with sunflower seed oil. The ratio of Lithospermum erythrorhizon to sunflower seed oil is 1:20. Then add 0.5% cellulase, 0.5% pectinase and 0.5% hemicellulase based on the total mass of Lithospermum erythrorhizon and sunflower seed oil. Stir at 50 °C for 2 h, and then let it stand for 5 h to separate Lithospermum erythrorhizon from sunflower seed oil. Take the upper oil phase to obtain a crude oil product, and further filter it to completely remove the Lithospermum erythrorhizon residue. Add 3 wt% of anhydrous sodium sulfate to the filtrate, and centrifuge at 10000 rpm for 10 min to remove anhydrous sodium sulfate. The supernatant after centrifugation is the Lithospermum erythrorhizon essence oil colored oil. The Lithospermum erythrorhizon essence oil obtained by this process is named Lithospermum erythrorhizon essence oil II.

[0025] Example 2: Preparation of Lithospermum erythrorhizon essence oil by treating the mixture of sunflower seed oil and Lithospermum erythrorhizon with a multi-enzyme system + supercritical treatment Taking Lithospermum erythrorhizon as an example, Lithospermum erythrorhizon is mixed with sunflower seed oil at a ratio of 1:20. Then, cellulase, pectinase, and hemicellulase, each accounting for 0.5% of the total mass of Lithospermum erythrorhizon and sunflower seed oil, are added, and the mixture is stirred at 50°C for 2 h. Then, the mixture is transferred to a supercritical device for treatment. The supercritical extraction pressure is set at 28 MPa, and the extraction temperature is set at 50°C to obtain a crude oil product of Lithospermum erythrorhizon essence oil. The crude product of Lithospermum erythrorhizon essence oil is further filtered by suction to completely remove Lithospermum erythrorhizon residues. 3 wt% of anhydrous sodium sulfate is added to the filtrate, and the mixture is centrifuged at 10,000 rpm for 10 min to remove anhydrous sodium sulfate. The supernatant after centrifugation is the colored oil of Lithospermum erythrorhizon essence oil, and the Lithospermum erythrorhizon essence oil obtained by this process is named Lithospermum erythrorhizon essence oil III.

[0026] Example 3: Preparation of Lithospermum erythrorhizon essence oil by treating the mixture of sunflower seed oil and Lithospermum erythrorhizon with a multi-enzyme system + supercritical + microbial fermentation Taking Lithospermum erythrorhizon as an example, Lithospermum erythrorhizon is mixed with sunflower seed oil at a ratio of 1:20. Then, cellulase, pectinase, and hemicellulase, each accounting for 0.5% of the total mass of Lithospermum erythrorhizon and sunflower seed oil, are added, and the mixture is stirred at 50°C for 2 h. Then, the mixture is transferred to a supercritical device for treatment. The supercritical extraction pressure is set at 28 MPa, and the extraction temperature is set at 50°C to obtain a crude oil product of Lithospermum erythrorhizon essence oil. S1. Cultivate the Lactobacillus seed liquid. The Lactobacillus is purchased from Chr. Hansen, and the culture medium is MRS medium, which is purchased from Jingzhou Yinjie Chemical Co., Ltd. The culture temperature is 37°C, and the culture time is 12 h.

[0027] S2. Inoculate the Lactobacillus seed liquid into the fermentation medium at an inoculation amount of 5%. The composition of the fermentation medium is: 20 g / L of glucose, 20 g / L of soybean extract, 10 g / L of corn flour, and 30 g / L of whey powder. Ferment and culture at 37°C for 6 h.

[0028] S3. In the fermentation system, add the prepared crude product of Lithospermum erythrorhizon essence oil at 100% of the weight of the fermentation medium, and continue to ferment and culture at 24°C for 18 h.

[0029] After fermentation, centrifuge at 10,000 rpm for 10 min to separate the oil phase from the water phase. The obtained oil phase is further filtered by suction to remove impurities. 3 wt% of anhydrous sodium sulfate is added to the obtained filtrate, and the mixture is centrifuged at 10,000 rpm for 10 min to remove anhydrous sodium sulfate. The supernatant after centrifugation is the colored oil of Lithospermum erythrorhizon essence oil, and the Lithospermum erythrorhizon essence oil obtained by this process is named Lithospermum erythrorhizon essence oil IV.

[0030] Test Example 1: Chromaticity Test The chromaticity difference of lithospermum erythrorhizon oil I, lithospermum erythrorhizon oil II, lithospermum erythrorhizon oil III and lithospermum erythrorhizon oil IV was measured by a colorimeter to determine the color difference between them. The measurement results are shown in Table 1 below. As can be seen from the table, the red color of the lithospermum erythrorhizon oil prepared by Example 1, Example 2 and Example 3 is significantly stronger than that of the lithospermum erythrorhizon oil prepared by the process of Basic Comparative Example 1. Among them, the lithospermum erythrorhizon oil prepared by Example 3 has the deepest red color.

[0031] Table 1 Chromaticity determination of lithospermum officinale extract oil

[0032] Test Example 2: Shikonin content test Shikonin is a bioactive ingredient extracted from the root of Lithospermum officinale, which has multiple activities such as antioxidant, anti-inflammatory and antibacterial. Shikonin is a characteristic component of Lithospermum officinale, so the shikonin content of Lithospermum officinale essential oil I, Lithospermum officinale essential oil II, Lithospermum officinale essential oil III and Lithospermum officinale essential oil IV was measured respectively. The shikonin content was measured by high performance liquid chromatography (HPLC method), and the measurement results are shown in Table 2 below. It can be seen from the results that the shikonin content in the Lithospermum officinale essential oil prepared by Example 1, Example 2 and Example 3 is significantly higher than that of the Lithospermum officinale essential oil prepared by Basic Comparative Example 1. Among them, the shikonin content in Lithospermum officinale essential oil IV is 9.5 times that of Lithospermum officinale essential oil I.

[0033] Table 2 Determination of shikonin content in lithospermum officinale extract oil

[0034] Test Example 3: Antioxidant Test The antioxidant capacity of sunflower seed oil, lithospermum officinale oil I, lithospermum officinale oil II, lithospermum officinale oil III and lithospermum officinale oil IV was determined by DPPH free radical scavenging ability test. Figure 1 As shown in the figure, compared with the sunflower seed oil as the base oil, the prepared comfrey essential oil not only brings about a change in color, but also significantly improves the antioxidant capacity of the comfrey essential oil, among which comfrey essential oil IV has the strongest antioxidant capacity, reaching 95%.

[0035] Test Example 4: Stability Test Under light conditions, the stabilities of Lithospermum erythrorhizon essence oil I, Lithospermum erythrorhizon essence oil II, Lithospermum erythrorhizon essence oil III, and Lithospermum erythrorhizon essence oil IV were determined. The color change of Lithospermum erythrorhizon essence oil was mainly measured. After 30 days of storage, the chromaticities of each Lithospermum erythrorhizon essence oil obtained are shown in Table 3. By comparing Table 1 and Table 3, it can be seen that the red values of Lithospermum erythrorhizon essence oil I, Lithospermum erythrorhizon essence oil II, and Lithospermum erythrorhizon essence oil III all showed a significant decrease. Visually, all three showed obvious fading. Among them, Lithospermum erythrorhizon essence oil I faded the most severely and appeared yellow to the naked eye. Although the red value of Lithospermum erythrorhizon essence oil IV also decreased to a certain extent, it only decreased by 8.6%, and there was no obvious change in color visually, thus proving that Lithospermum erythrorhizon essence oil IV has very excellent stability.

[0036] Table 3 Chromaticity determination of Lithospermum erythrorhizon essence oil after 30 days of light exposure

[0037] Example 4: Preparation of chamomile essence oil by treating the mixture of sunflower oil and chamomile with multi-enzyme system + supercritical + microbial fermentation Chamomile was mixed with sunflower oil at a ratio of 1:10. Then, 0.6% cellulase, 0.4% pectinase, and 0.6% hemicellulase based on the total mass of chamomile and sunflower oil were added, and the mixture was stirred at 50 °C for 2 h and then continued to be stirred at 80 °C for 2 h. Then, the mixture was transferred to a supercritical device for treatment. The supercritical extraction pressure was set at 27 MPa, and the extraction temperature was set at 60 °C to obtain the crude oil of chamomile essence oil. The obtained crude chamomile essence oil was fermented using lactic acid bacteria. The specific fermentation steps were as follows: S1. Cultivate the lactic acid bacteria seed liquid. The lactic acid bacteria were purchased from Chr. Hansen, and the culture medium was MRS medium, which was purchased from Jingzhou Yinjie Chemical Co., Ltd. The culture temperature was 37 °C, and the culture time was 12 h.

[0038] S2. Inoculate the lactic acid bacteria seed liquid into the fermentation medium at an inoculation amount of 5%. The composition of the fermentation medium was: 20 g / L glucose, 20 g / L soy extract, 10 g / L corn flour, and 30 g / L whey powder. Ferment and culture at 37 °C for 6 h.

[0039] S3. In the fermentation system, add the obtained crude chamomile essence oil to the fermentation medium at 100% of the medium weight and continue to ferment and culture at 24 °C for 18 h.

[0040] After fermentation, centrifuge at 8000 rpm for 15 min to separate the oil phase from the water phase, and further remove impurities from the obtained oil phase by suction filtration. 1 wt% anhydrous sodium sulfate is added to the obtained filtrate, and then centrifuge at 8000 rpm for 15 min to remove anhydrous sodium sulfate. The supernatant after centrifugation is the chamomile essence oil colored grease.

[0041] Example 5: Preparation of avocado essence oil by treating avocado oil and avocado mixture with multi - enzyme system + supercritical + microbial fermentation Mix avocado oil and avocado, with the ratio of avocado to avocado oil being 1:15. Then add 1% cellulase, 1% pectinase and 0.5% hemicellulase based on the total mass of avocado oil and avocado, stir at 45°C for 2 h, and then continue to stir at 60°C for 2 h. Then transfer the mixture to a supercritical device for treatment. The supercritical extraction pressure is set at 28 MPa and the extraction temperature is set at 50°C to obtain the crude product of avocado essence oil. Ferment the obtained crude product of avocado essence oil with Bacillus sp., and the specific fermentation steps are as follows: S1. Culture the seed liquid of Bacillus sp. (from patent CN202310251292.5). The medium is LB medium, the culture temperature is 37°C, and the culture time is 12 h. The composition of LB medium is 5 g / L yeast powder, 10 g / L peptone, and 10 g / L glucose.

[0042] S2. Inoculate the seed liquid of Bacillus sp. into the fermentation medium at an inoculation amount of 5%. The composition of the fermentation medium is: 20 g / L glucose, 20 g / L soy extract, 10 g / L corn flour, and 30 g / L whey powder. Ferment and culture at 37°C for 6 h.

[0043] S3. In the fermentation system, add the obtained crude product of avocado essence oil to the fermentation system at 100% of the weight of the medium, and continue to ferment and culture at 24°C for 18 h.

[0044] After fermentation, centrifuge at 12000 rpm for 5 min to separate the oil phase from the water phase, and further remove impurities from the obtained oil phase by suction filtration. 5 wt% anhydrous sodium sulfate is added to the obtained filtrate, and then centrifuge at 12000 rpm for 5 min to remove anhydrous sodium sulfate. The supernatant after centrifugation is the avocado essence oil colored grease.

[0045] Test Example 5: Chromaticity test of chamomile essence oil and avocado essence oil Use a chromaticity meter to measure the chromaticity of chamomile essence oil and avocado essence oil respectively. The measurement results are shown in Table 4 below. Chamomile essence oil is blue, and avocado essence oil is dark green.

[0046] Table 4 Colorimetric Determination of Chamomile Essential Oil and Avocado Essential Oil

[0047] Test Example 6: Stability Test of Chamomile Essential Oil and Avocado Essential Oil The stabilities of chamomile essential oil and avocado essential oil were determined under light conditions. The color changes of chamomile essential oil and avocado essential oil were mainly measured. After 30 days of storage, the colorimetric values of the obtained chamomile essential oil and avocado essential oil are shown in Table 5. By comparing Table 4 and Table 5, it can be seen that after 30 days under light conditions, neither chamomile essential oil nor avocado essential oil showed obvious fading, which proves that chamomile essential oil and avocado essential oil have excellent stability.

[0048] Table 5 Colorimetric Determination of Chamomile Essential Oil and Avocado Essential Oil after 30 Days of Illumination

[0049] Application Example: Preparation of Makeup Remover Oil Containing Lithospermum Essential Oil A makeup remover oil containing Lithospermum essential oil was prepared according to the formula described in Table 6 to obtain Lithospermum Phytoclean Makeup Remover Oil, which is red in color. The makeup removal effect of this makeup remover oil is as Figure 2 shown. It can be seen from this figure that Lithospermum Phytoclean Makeup Remover Oil has a very good makeup removal effect.

[0050] Table 6 Formula of Lithospermum Phytoclean Makeup Remover Oil

[0051] Although the embodiments of the present invention have been disclosed as above, they are not limited to the applications listed in the specification and embodiments. It can be fully applied to various fields suitable for the present invention. For those skilled in the art, for ordinary technical personnel in the art, various changes, modifications, substitutions, and variations can be made to these embodiments without departing from the principles and spirits of the present invention. Therefore, without departing from the general concept defined by the claims and their equivalent scopes, the present invention is not limited to specific details.

Claims

1. A method for preparing colored grease, characterized in that: The preparation method comprises the following steps: (1) After mixing the plant and the plant oil, a multi-enzyme system is added, and the mixture is stirred to obtain a mixture of the plant and the plant oil; (2) separating the mixed liquid, taking the oil phase therein to obtain a crude oil product, and further purifying the crude oil product to obtain the colored oil; The multi-enzyme system includes cellulase, pectinase and hemicellulase.

2. The preparation method according to claim 1, characterized in that: In step (1), the mass ratio of the plant to the plant oil is 1:3-100; the mass of the cellulase, pectinase and hemicellulase is 0.1-1.5% of the total mass of the plant and the plant oil, respectively.

3. The preparation method according to claim 1, characterized in that: During the stirring process in step (1), the temperature is 20-120° C. and the stirring time is 1-10 h.

4. The preparation method according to claim 1, characterized in that: The method for separating the mixed liquid in step (2) includes static separation, suction filtration separation, plate and frame separation or centrifugal separation; the method for further purifying the crude oil product includes filtration and centrifugation.

5. The preparation method according to claim 1, characterized in that: The step of separating the mixed solution in step (2) is replaced by extraction with a supercritical system, wherein the extraction pressure of the supercritical system is 15-30 MPa and the extraction temperature is 30-70°C.

6. The preparation method according to claim 1, characterized in that: The preparation method further comprises the step of fermenting the crude oil product obtained in step (2), wherein the fermentation process comprises the following steps: S1. Cultivate microbial seed solution at a temperature of 30-45°C for 5-30 h; S2, inoculating the microbial seed liquid into the fermentation medium for fermentation culture; S3, then add the crude oil product described in step (2) to continue fermentation and cultivation; after the fermentation is completed, centrifuge to obtain the oil phase, and then perform subsequent purification steps.

7. The preparation method according to claim 6, characterized in that: The microorganisms described in step S1 include but are not limited to lactic acid bacteria, bacillus, and yeast; the fermentation culture temperature in step S2 is 30-45°C and the culture time is 2-10 h; the continued fermentation culture temperature in step S3 is 15-45°C and the culture time is 8-60 h.

8. The preparation method according to claim 6, characterized in that: The mass of the microbial seed liquid described in step S2 accounts for 1-10% of the fermentation medium; the mass of the crude oil product described in step S3 accounts for 50-200% of the fermentation medium.

9. Use of the colored oil obtained by the preparation method according to any one of claims 1 to 8 in the preparation of cosmetics.

10. A cosmetic, characterized in that: The cosmetic comprises the colored oil obtained by the preparation method according to any one of claims 1 to 8, and cosmetically acceptable auxiliary materials.

Images