Green coffee seed oil as well as preparation method and application thereof in cosmetics

Abstract

The invention relates to the field of personal care, in particular to green coffee seed oil and a preparation method and application thereof in cosmetics, and the method comprises the following steps: freeze-drying, crushing and sieving green coffee seeds, adding deionized water, preparing the green coffee seeds into suspension liquid by using a colloid mill, performing high-voltage pulsed electric field treatment on the suspension liquid, and drying to obtain the green coffee seed oil. And standing the solution, performing ultrasonic treatment, adding a compound enzyme into the suspension, performing enzymolysis, and performing supercritical CO2 extraction to obtain the green coffee seed oil. The green coffee seed oil disclosed by the invention has the advantages of high stability, good moisturizing effect and the like.

Description

Technical Field

[0001] The present invention relates to the field of personal care, and in particular to green coffee seed oil, a preparation method thereof, and application thereof in cosmetics. Background Art

[0002] Green coffee seed oil is a natural oil extracted from green coffee fruit of the Rubiaceae family by cold pressing. This oil is light green in color, fresh in smell, and has a unique green fragrance. It not only has a pleasant sensory experience, but is also rich in a variety of ingredients that are beneficial to the skin, such as caffeine, stearic acid, oleic acid, linolenic acid, palm oil, and chlorogenic acid. Green coffee seed oil can be used as a magic tool for eye moisturizing and repairing, reducing dark circles and wrinkles around the eyes; it can also be used for moisturizing and nourishing the skin all over the body, making the skin smoother, more delicate, and more elastic.

[0003] Although green coffee seed oil has broad application prospects in the field of skin care, the existing extraction methods still have some defects, which limit its large-scale production and wide application. At present, green coffee seed oil is usually obtained by cold pressing or solvent extraction. However, the cold pressing method has low extraction efficiency and requires a large amount of coffee beans to extract a small amount of oil. This not only increases production costs, but also limits the large-scale production of green coffee seed oil. The cold pressing method is also unable to completely extract all the oil in the coffee beans, resulting in low extraction efficiency.

[0004] Although the solvent extraction method has a high extraction efficiency, it may involve the use of harmful solvents, which not only increases costs but also may pollute the environment. During the extraction process, due to the selectivity of the solvent and the influence of the extraction conditions, some active ingredients may be destroyed or lost, thus affecting the skin care effect of the oil. In addition, coffee seed oil contains a variety of fatty acids, among which the content of unsaturated fatty acids is relatively high, which makes coffee seed oil more susceptible to oxidation and deterioration than other vegetable oils. Especially under high temperature or light conditions, coffee seed oil has poor stability and is prone to lose its original quality and flavor. Summary of the invention

[0005] In order to solve the above problems, the present invention provides a green coffee seed oil and a preparation method thereof and application in cosmetics, which has the advantages of high stability, good moisturizing effect and the like.

[0006] To achieve the purpose of the present invention, the technical solution adopted by the present invention is:

[0007] A method for preparing green coffee seed oil comprises the following steps: freeze-drying, crushing and sieving green coffee seeds, adding deionized water and preparing them into a suspension using a colloid mill, subjecting the suspension to high-voltage pulse electric field treatment, subjecting the solution to ultrasonic treatment after standing, adding a composite enzyme to the suspension, and extracting with supercritical CO2 after enzymolysis to obtain green coffee seed oil.

[0008] Furthermore, the mass ratio of the freeze-dried, crushed and sieved green coffee seeds to deionized water is 3-4:8-10; the freeze-drying is specifically: freezing at -20--15°C for 5-8h, then freezing at -10--5°C for 6-19h, then keeping at -2-2°C for 3-4h, and finally keeping at 15-25°C for 3-5h; the vacuum degree during the freeze-drying process is 0.5-0.6mbar.

[0009] Furthermore, the power of the colloid mill is 40-50W, the rotation speed is 1000-1500r / min, and the grinding time is 3-5h.

[0010] Furthermore, the conditions of the supercritical CO2 extraction are: extraction pressure of 30-40 MPa; extraction temperature of 40-50°C; extraction time of 50-80 min, and CO2 flow rate of 0.3-0.6 L / min.

[0011] Furthermore, the ultrasonic treatment is intermittent ultrasonic treatment, wherein the intermittent ultrasonic treatment is ultrasonic treatment for 10 to 20 seconds and a pause of 5 to 10 seconds; the power of the ultrasonic treatment is 400 to 600 W; and the time of the ultrasonic treatment is 10 to 20 minutes.

[0012] Furthermore, the complex enzyme includes pectinase, cellulase and β-glucan, the weight ratio of pectinase, cellulase and β-glucan is 2-3:5-6:1-2; the enzymolysis temperature is 35-40°C, the enzymolysis time is 3-5h; the total amount of enzyme is 0.05wt% of the mixed solution.

[0013] The intensity of the high-voltage pulse electric field treatment is 35-40 kV / cm, the frequency is 1600-1800 Hz, the pulse width is 60-70 μs, the treatment time is 2-4 min, and the treatment temperature is 35-40° C. A green coffee seed oil is prepared by the above preparation method.

[0014] The present invention also provides application of green coffee seed oil in cosmetics, wherein the cosmetics are bath oil, body lotion, skin essence or moisturizing spray.

[0015] Furthermore, the mass percentage of the green coffee seed oil in the cosmetic is 0.001 to 20%.

[0016] Beneficial Effects

[0017] Green coffee seed oil is rich in a variety of active ingredients that are beneficial to the skin, such as caffeine, chlorogenic acid, phytosterol esters and fatty acids. These ingredients have multiple effects such as anti-oxidation, anti-inflammatory, moisturizing and skin tightening. In the process of extracting green coffee seed oil, the green coffee seeds are first freeze-dried. During the freeze-drying process, the internal chemical composition and physical properties (such as porous structure, colloidal properties, etc.) of the green coffee seeds can be well maintained, avoiding the destruction of the active ingredients, and making the ingredients rich in green coffee seed oil easier to dissolve. Then, a colloid mill is used to prepare a suspension. During the extraction process of green coffee seed oil, the colloid mill can quickly grind the green coffee seeds into fine particles, thereby accelerating the release of oil. The ground green coffee seed particles are fine and uniform, making it easier for the green coffee seed oil to be evenly mixed and dispersed in the subsequent processing process.

[0018] Pulsed electric field technology can act on the cell membrane in a short time, forming tiny holes, allowing the oil and other molecules in the green coffee seed cells to leak out without being squeezed. This physical method avoids the use of high temperature and chemical solvents, thereby reducing the oxidation and degradation of oils. Ultrasonic technology uses the cavitation effect, thermal effect and mechanical action generated by high-frequency vibration to destroy plant cell walls and promote the release of intracellular substances. When used in combination with pulsed electric fields, the extraction efficiency of oils can be further improved. Pulsed electric field combined with ultrasonic treatment can be carried out at a lower temperature, thereby reducing the oxidation reaction of oils during the extraction process. Through pulsed electric field and ultrasonic treatment, unstable components in green coffee seed oil can be effectively removed or transformed, thereby improving its stability. DETAILED DESCRIPTION

[0019] To make the purpose, technical solutions and advantages of the embodiments of the present invention more clear, the embodiments of the present invention will be described below.

[0020] Example 1

[0021] A method for preparing green coffee seed oil comprises the following steps:

[0022] The green coffee seeds are freeze-dried, crushed and sieved, and then deionized water is added and a colloid mill is used to prepare a suspension, the suspension is treated with a high-voltage pulse electric field, the solution is allowed to stand and then ultrasonically treated, a composite enzyme is added to the suspension, and after enzymatic hydrolysis, supercritical CO2 extraction is used to obtain green coffee seed oil;

[0023] The mass ratio of the freeze-dried, crushed and sieved green coffee seeds to deionized water is 3:8; the freeze-drying is specifically as follows: freezing at -20°C for 6 hours, then freezing at -10°C for 10 hours, then keeping at 0°C for 3 hours, and finally keeping at 20°C for 4 hours; the vacuum degree during the freeze-drying process is 0.5 mbar.

[0024] The power of the colloid mill is 40W, the rotation speed is 1000r / min, and the grinding time is 4h; the conditions of the supercritical CO2 extraction are: extraction pressure is 30MPa; extraction temperature is 40°C; extraction time is 60min, and CO2 flow rate is 0.4L / min.

[0025] The intensity of the high-voltage pulse electric field treatment is 40 kV / cm, the frequency is 1800 Hz, the pulse width is 60 μs; the treatment time is 2 min, and the treatment temperature is 35° C. The ultrasonic treatment is intermittent ultrasonic treatment, and the intermittent ultrasonic treatment is ultrasonic treatment for 10 s and pause for 5 s; the power of the ultrasonic treatment is 500 W; the ultrasonic treatment time is 15 min;

[0026] The complex enzyme comprises pectinase, cellulase and beta-glucan, the weight ratio of pectinase, cellulase and beta-glucan is 2:5:1; the enzymolysis temperature is 35°C, the enzymolysis time is 4h; the total amount of enzyme is 0.05% of the weight of the mixed solution.

[0027] Example 2

[0028] A method for preparing green coffee seed oil comprises the following steps:

[0029] The green coffee seeds are freeze-dried, crushed and sieved, and then deionized water is added and a colloid mill is used to prepare a suspension, the suspension is treated with a high-voltage pulse electric field, the solution is allowed to stand and then ultrasonically treated, a composite enzyme is added to the suspension, and after enzymatic hydrolysis, supercritical CO2 extraction is used to obtain green coffee seed oil;

[0030] The mass ratio of the freeze-dried, crushed and sieved green coffee seeds to deionized water is 3:10; the freeze-drying is specifically: freezing at -20°C for 8 hours, then freezing at -10°C for 12 hours, then keeping at -2°C for 4 hours, and finally keeping at 15°C for 3 hours; the vacuum degree during the freeze-drying process is 0.5 mbar.

[0031] The power of the colloid mill is 40W, the rotation speed is 1000r / min, and the grinding time is 3h; the conditions of the supercritical CO2 extraction are: extraction pressure is 30MPa; extraction temperature is 40°C; extraction time is 50min, and CO2 flow rate is 0.3L / min.

[0032] The intensity of the high-voltage pulse electric field treatment is 35 kV / cm, the frequency is 1600 Hz, the pulse width is 70 μs; the treatment time is 4 min, and the treatment temperature is 40° C. The ultrasonic treatment is intermittent ultrasonic treatment, and the intermittent ultrasonic treatment is ultrasonic treatment for 10 s and pause for 5 s; the power of the ultrasonic treatment is 400 W; the ultrasonic treatment time is 10 min;

[0033] The complex enzyme comprises pectinase, cellulase and beta-glucan, the weight ratio of pectinase, cellulase and beta-glucan is 2:5:1; the enzymolysis temperature is 35°C, the enzymolysis time is 3h; the total amount of enzyme is 0.05% of the weight of the mixed solution.

[0034] Example 3

[0035] A method for preparing green coffee seed oil comprises the following steps:

[0036] The green coffee seeds are freeze-dried, crushed and sieved, and then deionized water is added and a colloid mill is used to prepare a suspension, the suspension is treated with a high-voltage pulse electric field, the solution is allowed to stand and then ultrasonically treated, a composite enzyme is added to the suspension, and after enzymatic hydrolysis, supercritical CO2 extraction is used to obtain green coffee seed oil;

[0037] The mass ratio of the freeze-dried, crushed and sieved green coffee seeds to deionized water is 2:5; the freeze-drying is specifically: freezing at -15°C for 8 hours, then freezing at -5°C for 19 hours, then keeping at 2°C for 4 hours, and finally keeping at 25°C for 5 hours; the vacuum degree during the freeze-drying process is 0.6 mbar.

[0038] The power of the colloid mill is 50W, the rotation speed is 1500r / min, and the grinding time is 5h; the conditions of the supercritical CO2 extraction are: extraction pressure is 40MPa; extraction temperature is 50°C; extraction time is 80min, and CO2 flow rate is 0.6L / min.

[0039] The intensity of the high-voltage pulse electric field treatment is 35 kV / cm, the frequency is 1800 Hz, the pulse width is 60 μs; the treatment time is 2 min, and the treatment temperature is 35° C. The ultrasonic treatment is intermittent ultrasonic treatment, and the intermittent ultrasonic treatment is ultrasonic treatment for 20 s and pause for 10 s; the power of the ultrasonic treatment is 600 W; the ultrasonic treatment time is 20 min;

[0040] The complex enzyme comprises pectinase, cellulase and beta-glucan, the weight ratio of pectinase, cellulase and beta-glucan is 3:6:2; the enzymolysis temperature is 40°C, the enzymolysis time is 3h; the total amount of enzyme is 0.05% of the weight of the mixed solution.

[0041] Example 4

[0042] The green coffee seed oil obtained by the method of Example 1 was added to the bath oil at a mass ratio of 1%. The formula of the bath oil was as follows:

[0043]

[0044]

[0045] Comparative Example 1

[0046] This comparative example provides a bath oil, which differs from Example 4 in that it does not contain the green coffee seed oil described in Example 4, and the other conditions are exactly the same as those in Example 4.

[0047] Comparative Example 2

[0048] This comparative example provides a bath oil, which is different from Example 4 in that the freeze-drying step is not used in the preparation of the green coffee seed oil, and the other conditions are exactly the same as those in Example 4.

[0049] Comparative Example 3

[0050] This comparative example provides a bath oil, which is different from Example 4 in that the colloid mill treatment step is not used in the preparation of the green coffee seed oil, and the other conditions are exactly the same as those in Example 4.

[0051] Comparative Example 4

[0052] This comparative example provides a bath oil, which is different from Example 4 in that the high-voltage pulse electric field treatment step is not used in the preparation of the green coffee seed oil, and the other conditions are exactly the same as those in Example 4.

[0053] Comparative Example 5

[0054] This comparative example provides a bath oil, which is different from Example 4 in that no enzymatic treatment step is used in the preparation of green coffee seed oil, and the other conditions are exactly the same as those in Example 4.

[0055] Comparative Example 6

[0056] This comparative example provides a bath oil, which differs from Example 4 in that, in the preparation of green coffee seed oil, supercritical CO2 extraction is not used, but cold pressing extraction is used, and the other conditions are exactly the same as those in Example 4.

[0057] Comparative Example 7

[0058] This comparative example provides a bath oil, which is different from Example 4 in that ultrasonic treatment is not used in the preparation of green coffee seed oil, and the other conditions are exactly the same as those in Example 4.

[0059] Comparative Example 8

[0060] This comparative example provides a bath oil, which is different from Example 4 in that, in the preparation of green coffee seed oil, there is no pause during the ultrasonic treatment process, and the other conditions are exactly the same as those in Example 4.

[0061] Example 5

[0062] Volunteers aged between 20 and 50 years old with healthy skin were selected and divided into groups. Each person evenly applied 3g of bath oil to the 3cm×3cm area on the inner side of the forearms of both arms. The products prepared in Example 4 and Comparative Examples 1 to 8 were used. During the experiment, the volunteers could not apply any cosmetics on the experimental parts. The test method was as follows: before each test, the test area was cleaned, and the test area was placed in a laboratory with a temperature of 21±1°C and a humidity of 50±5% RH for 30 minutes, and the bath oil was applied. After 2 minutes of massage, the skin moisture content was detected using a skin moisture test probe Corneometer CM 825 before and after using the product. The test was performed three times, and the results were averaged. The moisture content change rate before and after using the product was calculated, and the results were as follows:

[0063]

[0064] It can be seen from the above table that the green coffee seed oil prepared by the method of Example 4 can effectively increase the moisture content of the skin when added to the bath oil, while the product prepared by the comparative example method has an increased moisture content, but the increase is small.

[0065] Example 6

[0066] Volunteers aged between 20 and 50 years old with healthy skin were selected and divided into groups on average. The products prepared in Example 4 and Comparative Examples 1 to 8 were used as bathing agents respectively. They were used continuously for 4 weeks at the normal bathing frequency. The TEWL values ​​of the volunteers' forearms were tested. During the experiment, the volunteers were not allowed to apply any cosmetics on the test area. The test method is: before each test, clean the test area, sit in a laboratory with a temperature of 21±1°C and a humidity of 50±5% RH for 30 minutes, and then test. The skin water loss test probe Tewameter TM HEX was used to detect the transepidermal water loss of the skin before using the product, after using the product for 2 weeks, and after using the product for 4 weeks. Each test point was tested three times, and the results were averaged. The improvement rate of the TEWL value was calculated, and the results are as follows:

[0067]

[0068] TEWL value is an important indicator of the quality of skin barrier. The lower the TEWL value of the skin, the better the barrier function of the skin, and vice versa. The greater the TEWL value improvement rate, the stronger the immediate skin barrier damage repair ability of the skin care product; as can be seen from the above table, the green coffee seed oil prepared by the method of Example 4 is added to the bath oil, which can fully utilize the moisturizing and barrier functions of the coffee seed oil, thereby improving the skin's moisturizing barrier and making the skin healthier, more hydrated and elastic.

[0069] Example 7

[0070] The bath oils prepared in Example 4 and Comparative Examples 1 to 8 were distributed to volunteers for use, and divided into 9 groups, with 3 people in each group. All people bathed in the same way, once every two days, and used it continuously for one week. The volunteers scored according to their feelings. The scoring standard adopted a 5-point system, with 1 point (tight and itchy skin) representing the worst, and 5 points (comfortable skin, no reaction) representing the best. The higher the score, the better the effect. The statistical results were averaged.

[0071]

[0072]

[0073] The above skin feel evaluation after use shows that Example 4 has better use effect, can make the bath oil foam richer, the skin feel more refreshing after washing, moisturizing, and better fragrance retention, effectively improving the use effect of the bath oil.

Claims

1. A method for preparing green coffee seed oil, characterized in that: The following steps are involved: The green coffee seeds are freeze-dried, crushed and sieved, and then deionized water is added and a colloid mill is used to prepare a suspension. The suspension is treated with a high-voltage pulse electric field, and the solution is ultrasonically treated after standing. A complex enzyme is added to the suspension, and after enzymatic hydrolysis, supercritical CO2 extraction is used to obtain green coffee seed oil.

2. The method for preparing green coffee seed oil according to claim 1, characterized in that: The mass ratio of the green coffee seeds after freeze drying, crushing and sieving to deionized water is 3-4:8-10; the freeze drying is specifically: freezing at -20--15°C for 5-8h, then freezing at -10--5°C for 6-19h, then keeping at -2-2°C for 3-4h, and finally keeping at 15-25°C for 3-5h; the vacuum degree during the freeze drying process is 0.5-0.6mbar.

3. The method for preparing green coffee seed oil according to claim 1, characterized in that: The power of the colloid mill is 40-50W, the rotation speed is 1000-1500r / min, and the grinding time is 3-5h.

4. The method for preparing green coffee seed oil according to claim 1, characterized in that: The conditions of the supercritical CO2 extraction are: extraction pressure of 30-40 MPa; extraction temperature of 40-50°C; extraction time of 50-80 min, and CO2 flow rate of 0.3-0.6 L / min.

5. The method for preparing green coffee seed oil according to claim 1, characterized in that: The ultrasonic treatment is intermittent ultrasonic treatment, wherein the intermittent ultrasonic treatment is ultrasonic treatment for 10 to 20 seconds and a pause of 5 to 10 seconds; the power of the ultrasonic treatment is 400 to 600 W; and the time of the ultrasonic treatment is 10 to 20 minutes.

6. The method for preparing green coffee seed oil according to claim 1, characterized in that: The complex enzyme comprises pectinase, cellulase and beta-glucan, the weight ratio of pectinase, cellulase and beta-glucan is 2-3:5-6:1-2; the enzymolysis temperature is 35-40°C, the enzymolysis time is 3-5h; the total amount of enzyme is 0.05wt% of the mixed solution.

7. The method for preparing green coffee seed oil according to claim 1, characterized in that: The intensity of the high-voltage pulse electric field treatment is 35-40 kV / cm, the frequency is 1600-1800 Hz, the pulse width is 60-70 μs; the treatment time is 2-4 minutes, and the treatment temperature is 35-40° C.

8. A green coffee seed oil, characterized in that Prepared by the preparation method according to any one of claims 1 to 7.

9. The use of green coffee seed oil in cosmetics according to claim 8, characterized in that: The cosmetic is a bath oil, a body lotion, a skin essence or a moisturizing spray.

10. The use according to claim 9, characterized in that: The mass percentage of the green coffee seed oil in the cosmetics is 0.001 to 20%.

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