A kind of extraction process of freeze-dried rose water and rose cosmetics

Abstract

The present application relates to the field of rose processing technology. The present application discloses a freeze-dried rose water extraction process and rose cosmetics. The freeze-dried rose water extraction process comprises the following steps: S1, pretreatment, quick freezing the rose for 5-8 hours; S2, vacuum freeze-drying the quick-frozen rose; S3, using a cold hydrazine device to capture the gas generated by sublimation in step S2, and quickly condense it into a solid ice-like substance; S4, repeating steps S2-S3 1-3 times; S5, melting the solid ice-like substance to obtain freeze-dried rose water. The present application discloses freeze-dried rose water prepared by the above freeze-dried rose water extraction process. The present application also discloses the application of the above freeze-dried rose water in cosmetics. The freeze-dried rose water extraction process of the present application is in an ultra-low temperature environment throughout the process, without high temperature damage, and the freeze-drying process is vacuum-sealed throughout the process, which can effectively retain the rose aroma and active ingredients.

Description

Technical Field

[0001] The present application relates to the technical field of rose processing, and in particular to an extraction process of freeze-dried rose water and rose cosmetics. Background Art

[0002] Rose, commonly known as beach eggplant and beach pear, is a deciduous shrub of the family Rosaceae. Rose branches have many thorns, odd-pinnate compound leaves, elliptical; the branches are relatively weak and drooping with dense thorns, and the flowering period is only once a year; the stems are thick and clustered. The petals are obovate, double or semi-double, and the flowers are purple-red or white. The fruiting period is from August to September, and the shape of the oblate sphere.

[0003] Rose water has a long history of application in the field of beauty. As early as in ancient times, there were records of using rose water for skin care. With the development of science and technology, people's understanding and research on rose water have become more and more in-depth. Modern research shows that roses are rich in active ingredients, such as citronellol, geraniol and nerol, which have a good protective effect on the skin. Citronellol is one of the main components of rose fragrance. It has antibacterial effects and can inhibit the activity of Staphylococcus aureus and Salmonella typhi. It may also have antiviral and anti-free radical damage properties, which can strengthen skin cells and regenerate skin tissue. Geraniol has antioxidant and anti-cancer effects, which can help resist oxidative stress and prevent skin damage and signs of aging, such as wrinkles, dark spots, dryness, etc. Nerol can promote metabolism, repair cells, reduce inflammation and kill bacteria, soothe emotions, regulate endocrine, beautify and nourish the skin, prevent and treat gynecological diseases, etc.

[0004] Therefore, rose water is a natural skin care product with high value, which is widely used in skin care, beauty, fragrance and other fields. Rose water has a unique aroma and beauty effect, which can help fade fine lines, improve skin tone, moisturize and nourish. Rose water also has antibacterial, anti-inflammatory and antioxidant effects, which can help protect the skin from external environmental damage. At the same time, the aroma components of rose water can soothe the body and mind, improve sleep, etc.

[0005] The existing methods for preparing rose water include traditional leaching, distillation and supercritical fluid extraction, but these preparation methods all have their limitations. The traditional leaching method has low extraction efficiency and unstable extraction effect; the distillation method has limited output and some raw materials will be lost during the distillation process; the supercritical fluid extraction method has high requirements for equipment and is difficult to operate.

[0006] Therefore, it is urgent to develop an extraction process for rose water that does not cause high-temperature damage, retains the rose aroma and active ingredients, and has a high content of active ingredients. Summary of the invention

[0007] In order to solve at least one of the above technical problems, a rose water extraction process is developed that does not cause high temperature damage, retains rose aroma and active ingredients, and has a high content of active ingredients. The present application provides a freeze-dried rose water extraction process and rose cosmetics.

[0008] On the one hand, the present application provides a freeze-dried rose water extraction process, comprising the following steps:

[0009] S1. Pretreatment: quick-freeze the roses for 5 to 8 hours;

[0010] S2, subjecting the quick-frozen roses to vacuum freeze-drying treatment;

[0011] S3, using a cold hydrazine device to capture the gas sublimated in step S2, and quickly condense it into a solid ice-like substance;

[0012] S4, repeat steps S2 to S3 1 to 3 times;

[0013] S5. Melt the solid ice to obtain freeze-dried rose water.

[0014] By adopting the above technical scheme, the extraction process of freeze-dried rose water of the present application is in an ultra-low temperature environment throughout the process, without high temperature damage, and the freeze-drying process is vacuum-sealed throughout the process, which can effectively retain the rose aroma and active ingredients. The obtained freeze-dried rose water has a fresh and natural taste, evaporates quickly, and retains the most rose top aroma components.

[0015] The low-temperature quick freezing of the present application helps to maintain the integrity of the cell structure and prevent the loss of aroma and nutrients; the vacuum freeze-drying process further prevents the destruction of the cell structure and retains more aroma and active ingredients.

[0016] Optionally, in step S1, the pretreatment includes: selecting fresh roses free of pests and diseases, removing branches and leaves of the roses, and removing impurities and damaged parts of petals.

[0017] By adopting the above technical solution, the present application pre-treats roses to remove undesirable flavors or impurities that may be present in the branches and leaves, thereby ensuring the purity and quality of the final product. Removing damaged parts helps maintain the stability and consistency of the product.

[0018] Optionally, in step S1, the quick freezing is performed in a quick freezing tunnel, and the temperature in the quick freezing tunnel is -50 to -41°C.

[0019] By adopting the above technical solution, the quick freezing temperature of the present application can ensure that the roses are frozen quickly and evenly, avoiding the formation of large ice crystals, thereby protecting the cell structure and tissue integrity of the roses.

[0020] Optionally, when quick freezing, the flowers are spread flat on a tray with the center facing upwards, and the tray is then placed in a quick freezing tunnel for quick freezing.

[0021] By adopting the above technical solution, the present application adopts a flat laying method with the center of the flower facing upward, which helps to freeze the roses more evenly during the quick freezing process, thereby maintaining their shape and texture.

[0022] Optionally, in step S2, the vacuum degree is 20-30Pa.

[0023] By adopting the above technical solution, the vacuum degree of the present application can reduce the impact of moisture and oxygen in the air on roses, ensure the stability and quality of roses during the vacuum freeze-drying process, and also help to accelerate the extraction process of active ingredients.

[0024] Optionally, in step S2, the freeze-drying temperature is -25 to -15°C.

[0025] By adopting the above technical solution, the freeze-drying temperature of the present application can balance the drying speed and the drying degree, ensuring that the roses remain in the best state during the drying process and avoiding damage to the active ingredients.

[0026] Optionally, in step S5, the pH value of the freeze-dried rose water is 6 to 6.5.

[0027] Optionally, after quick freezing in step S1, ultrasonic treatment is further included, with an ultrasonic frequency of 20 to 25 kHz and an ultrasonic time of 15 to 20 minutes.

[0028] By adopting the above technical solution, the present application also adopts ultrasonic treatment, which can improve the tissue structure of the rose, make the ice crystal distribution more uniform, and retain more aroma components and active ingredients.

[0029] In a second aspect, the present application provides freeze-dried rose water prepared by the above-mentioned freeze-dried rose water extraction process.

[0030] By adopting the above technical scheme, the freeze-dried rose water prepared in the present application can effectively retain the rose aroma and active ingredients, has a fresh and natural taste, has a unique fresh floral flavor, evaporates quickly, and retains more rose top aroma components.

[0031] Optionally, the freeze-dried rose water comprises the following components in relative percentages: 40.12-77.20% citronellol, 0.65-5.24% geraniol, 3.03-4.12% nerol, and 3.52-6.27% methyl eugenol.

[0032] By adopting the above technical scheme, the ingredients in the freeze-dried rose water of the present application give the freeze-dried rose water a unique aroma with a strong rose fragrance. Ingredients such as citronellol, geraniol and nerol have antioxidant effects, can resist the damage of free radicals, and protect the skin from the damage of oxidative stress reactions. Methyl eugenol is a substance with sensitizing effects, and the less the content, the better.

[0033] In a third aspect, the present application provides the use of the freeze-dried rose water in cosmetics, wherein the content of the freeze-dried rose water in the cosmetics is 3 to 8 wt %.

[0034] By adopting the above technical scheme, the freeze-dried rose water of the present application can be used in cosmetics to make moisturizing sprays, facial masks, creams and lotions, etc. The prepared rose cosmetics can replenish skin moisture, improve skin spots, delay skin aging, and have the effects of rapid anti-inflammatory, antibacterial and anti-itching. It can soothe the liver, relieve depression, regulate menstruation, and relieve tension.

[0035] The freeze-dried rose water in cosmetics contains 3-8 wt % of the water, which can effectively exert its fragrance, anti-oxidation and skin-soothing effects without negatively affecting other ingredients of the product.

[0036] In summary, the present invention includes at least one of the following beneficial technical effects:

[0037] 1. The extraction process of freeze-dried rose water of the present application is in an ultra-low temperature environment throughout the process, without high temperature damage, and the freeze-drying process is vacuum-sealed throughout the process, which can effectively retain the rose aroma and active ingredients.

[0038] 2. The freeze-dried rose water prepared in the present application can effectively retain the rose aroma and active ingredients, has a fresh and natural taste, has a unique fresh floral flavor, evaporates quickly, and retains more rose top aroma components.

[0039] 3. The freeze-dried rose water of the present application can be used in cosmetics to make rose cosmetics such as moisturizing sprays, facial masks, creams and lotions. DETAILED DESCRIPTION

[0040] The present application is further described in detail below with reference to the embodiments.

[0041] The present application designs a freeze-dried rose water extraction process, comprising the following steps:

[0042] S1. Pretreatment: quick-freeze the roses for 5 to 8 hours;

[0043] S2, subjecting the quick-frozen roses to vacuum freeze-drying treatment;

[0044] S3, using a cold hydrazine device to capture the gas sublimated in step S2, and quickly condense it into a solid ice-like substance;

[0045] S4, repeat steps S2 to S3 1 to 3 times;

[0046] S5. Melt the solid ice to obtain freeze-dried rose water.

[0047] The present application provides freeze-dried rose water prepared by the above-mentioned freeze-dried rose water extraction process.

[0048] The freeze-dried rose water of the present application can be used in cosmetics, and the content of the freeze-dried rose water in the cosmetics is 3-8wt%.

[0049] The freeze-dried rose water extraction process of the present application is in an ultra-low temperature environment throughout the process, without high temperature damage, and the freeze-drying process is vacuum-sealed throughout the process, which can effectively retain the rose aroma and active ingredients. The prepared freeze-dried rose water tastes fresh and natural, has a unique fresh floral flavor, evaporates quickly, and retains more rose top aroma components. Specific embodiments

[0051] The roses used in this application are Pingyin double-petal red roses.

[0052] Examples 1 to 3

[0053] Example 1

[0054] This embodiment provides a freeze-dried rose water extraction process, comprising the following steps:

[0055] S1. Select fresh roses without diseases and insect pests, remove the branches and leaves of the roses, remove impurities and damaged parts of the petals, lay them flat on a tray with the center of the flower facing upward, place the tray in a quick-freezing tunnel, and quick-freeze at -50°C for 8 hours;

[0056] S2, placing the low-temperature quick-frozen roses into a vacuum freeze-drying device for vacuum freeze-drying, with a vacuum degree of 30 Pa, a freeze-drying temperature of -25°C, and a freeze-drying time of 30 h;

[0057] S3, using a cold hydrazine device to capture the gas sublimated in step S2, and quickly condense it into a solid ice-like substance;

[0058] S4, repeat steps S2 to S3 once;

[0059] S5. Melt the solid ice to obtain freeze-dried rose water.

[0060] The pH value of freeze-dried rose water was detected to be 6.5.

[0061] Example 2

[0062] This embodiment provides a freeze-dried rose water extraction process, comprising the following steps:

[0063] S1. Select fresh roses without diseases and insect pests, remove the branches and leaves of the roses, remove impurities and damaged parts of the petals, lay them flat on a tray with the center of the flower facing upward, place the tray in a quick freezing tunnel, and quick freeze at -50°C for 6.5 hours;

[0064] S2, placing the low-temperature quick-frozen roses into a vacuum freeze-drying device for vacuum freeze-drying, with a vacuum degree of 30 Pa, a freeze-drying temperature of -25°C, and a freeze-drying time of 30 h;

[0065] S3, using a cold hydrazine device to capture the gas sublimated in step S2, and quickly condense it into a solid ice-like substance;

[0066] S4, repeat steps S2 to S3 three times;

[0067] S5. Melt the solid ice to obtain freeze-dried rose water.

[0068] The pH value of freeze-dried rose water was detected to be 6.3.

[0069] Example 3

[0070] This embodiment provides a freeze-dried rose water extraction process, comprising the following steps:

[0071] S1. Select fresh roses without diseases and insect pests, remove the branches and leaves of the roses, remove impurities and damaged parts of the petals, lay them flat on a tray with the center of the flower facing upward, place the tray in a quick-freezing tunnel, and quick-freeze at -50°C for 5 hours;

[0072] S2, placing the low-temperature quick-frozen roses into a vacuum freeze-drying device for vacuum freeze-drying, with a vacuum degree of 30 Pa, a freeze-drying temperature of -25°C, and a freeze-drying time of 30 h;

[0073] S3, using a cold hydrazine device to capture the gas sublimated in step S2, and quickly condense it into a solid ice-like substance;

[0074] S4, repeat steps S2 to S3 twice;

[0075] S5. Melt the solid ice to obtain freeze-dried rose water.

[0076] The pH value of freeze-dried rose water was detected to be 6.0.

[0077] Comparative Examples 1 to 3

[0078] Comparative Example 1

[0079] The difference between Comparative Example 1 and Example 2 is that Comparative Example 1 does not have the quick freezing process of step S1, and the roses are directly subjected to vacuum freeze-drying.

[0080] Comparative Example 2

[0081] The difference between Comparative Example 2 and Example 2 is that Comparative Example 2 does not have the repeated process of step S4, and the solid ice is directly melted after being obtained to obtain freeze-dried rose water.

[0082] Comparative Example 3

[0083] The difference between Comparative Example 3 and Example 2 is that Comparative Example 3 adopts a traditional extraction method to prepare rose water, and the steps include: putting roses into water, heating to 95° C., boiling for 20 minutes, filtering out the extract; and distilling the extract to obtain rose water.

[0084] Experimental testing

[0085] Test items and test methods

[0086] Relative percentage content detection of citronellol, geraniol, nerol and methyl eugenol: SPME method GC-MS detection, the detection conditions are as follows:

[0087] Instrument: Agilent 7890B-5977A gas chromatograph-mass spectrometer (GC-MS);

[0088] Chromatographic column: DB-WAX (30m×250μm×0.25μm);

[0089] Carrier gas: helium (99.999%);

[0090] Column temperature: from 65°C to 120°C at 2°C / min, then to 136.5°C at 1°C / min, then to 145°C at 0.5°C / min, and finally to 230°C at 2°C / min, and hold for 2 min;

[0091] Inlet: 230℃;

[0092] Ion source: 230℃;

[0093] Quadrupole: 150℃;

[0094] Ionization mode: EI+, 70eV;

[0095] Detector voltage: 2047V;

[0096] Scan mode: full scan;

[0097] Carrier gas flow rate: 1.1 mL / min;

[0098] Take 20mL sample and adsorb it in a 60℃ constant temperature water bath for 30min;

[0099] Injection volume: 1 μL;

[0100] Split ratio: 30 / 1.

[0101] The rose water prepared in Examples 1 to 3 and Comparative Examples 1 to 3 was tested for relative percentage contents of citronellol, geraniol, nerol and methyl eugenol. The test results are shown in Table 1.

[0102] Table 1

[0103] Citronellol / % Geraniol / % Nerolidol / % Methyl eugenol / % Example 1 60.24 3.80 3.54 5.37 Example 2 65.08 4.25 3.72 5.18 Example 3 53.61 3.12 3.35 5.06 Comparative Example 1 49.55 3.05 3.03 6.30 Comparative Example 2 59.04 3.59 2.53 4.61 Comparative Example 3 39.12 4.32 2.96 9.05

[0104] From the test results in Table 1, it can be seen that the rose water obtained by the extraction process of freeze-dried rose water in Examples 1 to 3 has a high relative percentage content of the active ingredients citronellol, geraniol and nerol, and effectively retains the rose aroma.

[0105] Comparative Example 1 does not have a low-temperature quick-freezing process, and Comparative Example 2 does not have a repeated process of step S4. In the prepared rose water, the relative percentages of the active ingredients citronellol and geraniol are significantly reduced.

[0106] Comparative Example 3 is a rose water prepared by traditional extraction method, in which the relative percentages of citronellol and nerol are much lower than those in Example 2, and the content of methyl eugenol is increased.

[0107] Embodiments 4 to 9

[0108] Example 4

[0109] The difference between Example 4 and Example 2 is that in step S1 of Example 4, the temperature in the quick-freezing tunnel is -45°C.

[0110] Example 5

[0111] The difference between Example 5 and Example 2 is that in step S1 of Example 5, the temperature in the quick-freezing tunnel is -41°C.

[0112] Example 6

[0113] The difference between Example 6 and Example 4 is that in step S2 of Example 6, the vacuum degree is 25Pa.

[0114] Example 7

[0115] The difference between Example 7 and Example 4 is that in step S2 of Example 7, the vacuum degree is 20Pa.

[0116] Example 8

[0117] The difference between Example 8 and Example 6 is that in step S2 of Example 8, the freeze-drying temperature is -20°C.

[0118] Example 9

[0119] The difference between Example 9 and Example 6 is that in step S2 of Example 9, the freeze-drying temperature is -15°C.

[0120] The rose water prepared in Examples 4 to 9 was tested for relative percentage contents of citronellol, geraniol, nerol and methyl eugenol. The test results are shown in Table 2.

[0121] Table 2

[0122] Citronellol / % Geraniol / % Nerolidol / % Methyl eugenol / % Example 4 67.32 4.57 3.80 5.26 Example 5 61.03 4.08 3.45 5.22 Example 6 69.15 5.04 3.92 5.11 Example 7 64.60 3.96 3.56 5.61 Example 8 72.21 5.10 4.03 5.17 Example 9 65.39 4.86 3.77 5.32

[0123] From the test results in Table 2, it can be seen that the low-temperature quick-freezing temperatures of Examples 4 and 5 are different from those of Example 2. Among them, the relative percentage contents of the active ingredients citronellol, geraniol and nerol in the rose water prepared in Example 4 are the highest.

[0124] The vacuum degrees of Example 6 and Example 7 are different from those of Example 4. In the rose water prepared in Example 6, the relative percentage contents of the active ingredients citronellol, geraniol and nerol are the highest.

[0125] The freeze-drying temperatures of Examples 8 and 9 are different from those of Example 6. In the rose water prepared in Example 8, the relative percentage contents of the active ingredients citronellol, geraniol and nerol are the highest.

[0126] Embodiments 10 to 12

[0127] Example 10

[0128] The difference between Example 10 and Example 8 is that after the low-temperature quick freezing in step S1 of Example 10, ultrasonic treatment is also included, and the ultrasonic frequency is 20 kHz and the ultrasonic time is 20 min.

[0129] Embodiment 11

[0130] The difference between Example 11 and Example 10 is that the ultrasonic frequency of Example 11 is 23 kHz and the ultrasonic time is 18 min.

[0131] Example 12

[0132] The difference between Example 12 and Example 10 is that the ultrasonic frequency of Example 12 is 25 kHz and the ultrasonic time is 15 min.

[0133] The rose water prepared in Examples 10 to 12 was tested for relative percentage contents of citronellol, geraniol, nerol and methyl eugenol. The test results are shown in Table 3.

[0134] Table 3

[0135] Citronellol / % Geraniol / % Nerolidol / % Methyl eugenol / % Example 10 75.04 5.19 4.07 5.25 Embodiment 11 77.20 5.23 4.12 5.09 Example 12 75.18 5.20 3.68 5.39

[0136] From the test results in Table 3, it can be seen that the extraction process of freeze-dried rose water in Example 10 also includes ultrasonic treatment, and the relative percentage content of active ingredients citronellol, geraniol and nerol in the obtained rose water is higher than that in Example 8.

[0137] In Examples 10 to 12, the rose water obtained by the extraction process of freeze-dried rose water in Example 11 has the highest relative percentage content of the active ingredients citronellol, geraniol and nerol.

[0138] Application Examples 1 to 3

[0139] Application Example 1

[0140] Application Example 1 provides a rose cosmetic, which is a moisturizing cream.

[0141] The ingredients are: 5% of freeze-dried rose water prepared in Example 2, 30% of glycerol, 20% of hyaluronic acid, 5% of vaseline, and 40% of water.

[0142] Application Example 2

[0143] Application Example 2 provides a rose cosmetic, which is a moisturizing cream.

[0144] The ingredients are: 5% of the freeze-dried rose water prepared in Example 4, 30% of glycerol, 20% of hyaluronic acid, 5% of vaseline, and 40% of water.

[0145] Application Example 3

[0146] Application Example 3 provides a rose cosmetic, which is a moisturizing cream.

[0147] The ingredients are: 5% of freeze-dried rose water prepared in Example 7, 30% of glycerol, 20% of hyaluronic acid, 5% of vaseline, and 40% of water.

[0148] The blank composition is as follows: 30% glycerin, 20% hyaluronic acid, 5% vaseline, and 45% water.

[0149] Moisture retention test method: 3 volunteers participated in the test. The test area was the flexor side of the forearm. The corresponding test sample was applied to the test area. Each test area was 3cmx4cm, and the application amount was 2.0±0.1mg / cm 2 . After use, the skin was continuously monitored for 48 hours, and the change rate of skin moisture content at each stage before and after use was measured, and the average value of the three volunteers was taken.

[0150] The moisturizing properties of the blank group and the moisturizing creams of Application Examples 1 to 3 were tested, and the test results are shown in Table 4.

[0151] Table 4

[0152] Moisture content change rate after 24 hours of use / % Moisture content change rate after 48 hours of use / % Blank group 4 2 Application Example 1 20 12 Application Example 2 22 15 Application Example 3 19 10

[0153] From the test results in Table 4, it can be seen that the moisturizing cream containing the freeze-dried rose water prepared in the present application has strong moisturizing ability and long lasting effect. The freeze-dried rose water prepared by the freeze-dried rose water extraction process of the present application can be used in cosmetics. Among Application Examples 1 to 3, the moisturizing cream containing the freeze-dried rose water prepared in Application Example 2 has the strongest moisturizing ability.

[0154] The above are all preferred embodiments of the present application, and the protection scope of the present application is not limited thereto. Therefore, any equivalent changes made according to the structure, shape, and principle of the present application should be included in the protection scope of the present application.

Claims

1. A freeze-dried rose water extraction process, characterized in that: The following steps are involved: S1, pretreatment, quick freezing the roses for 5-8 hours; the quick freezing is quick freezing in a quick freezing tunnel, and the temperature in the quick freezing tunnel is -50--41°C; S2, vacuum freeze drying the quick-frozen roses; S3, using a cold hydrazine device to capture the gas sublimated in step S2, and quickly condense it into a solid ice-like substance; S4, repeating steps S2-S3 1-3 times; S5, melting the solid ice-like substance to obtain freeze-dried rose water; after the quick freezing in step S1, ultrasonic treatment is also included, the ultrasonic frequency is 20-25kHz, and the ultrasonic time is 15-20min; in step S2, the vacuum degree is 20-30Pa.

2. The extraction process of freeze-dried rose water according to claim 1, characterized in that: In step S1, the pretreatment includes: selecting fresh roses without diseases and insect pests, removing branches and leaves of the roses, and removing impurities and damaged parts of petals.

3. The extraction process of freeze-dried rose water according to claim 1, characterized in that: In step S2, the freeze-drying temperature is -25 to -15°C.

4. The extraction process of freeze-dried rose water according to claim 1, characterized in that: In step S5, the pH value of the freeze-dried rose water is 6-6.

5.

5. A freeze-dried rose water, characterized in that: The rose water is prepared by the extraction process of freeze-dried rose water according to any one of claims 1 to 4.

6. The freeze-dried rose water according to claim 5, characterized in that: It includes the following ingredients in relative percentage: citronellol 40.12~77.20%, geraniol 0.65~5.24%, nerol 3.03~4.12%, and methyl eugenol 3.52~6.27%.

7. Use of the freeze-dried rose water according to claim 6 in preparing cosmetics, characterized in that: The content of the freeze-dried rose water in the cosmetics is 3-8wt%.