A kind of jasmine flower oil and its extraction method and application
Through freeze-drying, and combined with technical means of microwave extraction, reduced pressure distillation and subcritical water extraction, the problems of organic solvent residue and high production costs in existing jasmine flower oil extraction are solved, and high efficiency and low-cost jasmine flower are achieved. Flower oil extraction.
Patent Information
- Application Number
- CN202311113034.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-08-31
- Publication Date
- 2025-02-07
- Estimated Expiration
- 2043-08-31
AI Technical Summary
There are problems in the existing jasmine flower oil extraction technology that are organic solvent residue and supercritical CO2 extraction production costs.
The jasmine was treated by freeze-drying, and then mixed with ethanol for microwave extraction. The ethanol was recovered by distillation under reduced pressure, and then the jasmine flower oil was obtained by subcritical water extraction.
It effectively reduces organic residues, improves extraction rate, reduces extraction costs, and retains the quality of volatile components.
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Abstract
Description
Technical Field
[0001] The invention relates to the technical field of flower oil extraction, in particular to jasmine flower oil and an extraction method and application thereof. Background Art
[0002] Jasmine is a plant of the Oleaceae family, an evergreen shrub, and a high-grade spice plant. The leaves, flowers, and roots of Mirabilis jalapa have medicinal value. Jasmine also has a strong aroma, which is not possessed by many flowers. The main active ingredients of jasmine flower oil are volatile oils, mainly linalool, cis-3-hexenyl acetate, nerol, cis-3-hexenol, and geraniol. Jasmine flower oil is known as the "king of essential oils." Jasmine flower oil is very expensive because of its very low production. It has an elegant smell, can soothe depression, invigorate the spirit, and enhance self-confidence. At the same time, it can care for and improve dry, dehydrated, overly oily and sensitive skin conditions, fade stretch marks and scars, increase skin elasticity, and make the skin feel soft and tender.
[0003] In the existing technology of extracting jasmine flower oil, jasmine extract is obtained by leaching jasmine flowers with organic solvents or extracting jasmine flowers with supercritical CO2, and the jasmine extract is further purified to obtain jasmine flower oil. The use of organic solvents such as petroleum ether and n-hexane to extract jasmine flowers is likely to cause the residue of toxic solvents in the jasmine flower oil, and the degradation of volatile components is likely to occur during the extraction process due to the effects of solvents and heat. The use of supercritical CO2 to extract jasmine flowers requires the equipment to operate under high pressure conditions, which consumes a lot of energy and has high production costs. The shortcomings of the existing jasmine flower oil production technology are mainly the residue of organic solvents and the high production cost of supercritical CO2 extraction. Summary of the invention
[0004] The invention aims to provide a method for extracting jasmine flower oil, which has small organic residue, high extraction rate, can effectively reduce the decomposition of aromatic substances in the extraction process and has low extraction cost.
[0005] In order to achieve the above-mentioned object of the invention, the present invention provides the following technical solutions:
[0006] The invention provides a method for extracting jasmine flower oil, comprising the following steps:
[0007] S1. Freeze, grind and freeze-dry jasmine flowers to obtain jasmine powder;
[0008] S2. The jasmine powder was mixed with ethanol at a ratio of 1 g: 2 to 5 mL, and the mixture was extracted to obtain an extract;
[0009] S3. The extract was filtered, ethanol was recovered by vacuum distillation, and the ethanol volume content was 10 to 20% to obtain a crude extract;
[0010] S4. subjecting the crude extract to subcritical water extraction, centrifuging and filtering the extract to obtain jasmine flower oil.
[0011] Preferably, the freezing temperature is -25 to -20°C, and the freezing time is 20 to 30 minutes.
[0012] Preferably, the freeze-drying temperature is -55 to -50°C.
[0013] Preferably, the extraction in step S2 is microwave extraction, and the time of the microwave extraction is 30 to 60 minutes.
[0014] Preferably, the microwave extraction is intermittent, the microwave treatment time is 3 to 5 min / time, the next microwave treatment is performed 10 to 15 min after a single microwave treatment, the number of microwave treatments is 2 to 6 times, and the microwave power is 400 to 500 W.
[0015] Preferably, the vacuum degree of the reduced pressure distillation is -0.08~-0.09Mpa, and the temperature of the reduced pressure distillation is 68~80°C.
[0016] Preferably, the temperature of the subcritical water extraction is 30-40° C., the pressure is 1.5-2.5 MPa, and the solution flow rate is 2.5-4.5 mL / min; and the time of the subcritical water extraction is 40-70 min.
[0017] The invention also provides jasmine flower oil extracted by the method.
[0018] The invention also provides application of the jasmine flower oil in preparing skin care products and spices.
[0019] The present invention also provides a moisturizing and soothing essential oil, comprising the following components in parts by weight: 0.4-1 parts of jasmine flower oil, 45-50 parts of squalane, 35-40 parts of camellia seed oil, 8-15 parts of ascorbyl tetraisopalmitate, 1-3 parts of vitamin E, and 0.5-1.5 parts of ubiquinone.
[0020] By adopting the above technical solution, the present invention has the following beneficial effects:
[0021] The present invention freeze-dries jasmine flowers to better preserve the volatile components of jasmine flowers, then uses ethanol as a solvent for microwave extraction, obtains an extract, and then recovers the ethanol by vacuum distillation to obtain a crude extract of jasmine flower oil; the crude extract is subjected to subcritical water extraction for 40 to 70 minutes at a temperature of 70 to 105° C., a pressure of 1.5 to 2.5 MPa, and a solution flow rate of 2.5 to 4.5 mL / min, and the extract is centrifuged and filtered to obtain jasmine flower oil. The jasmine flower oil obtained by the present invention has a maximum yield of 7.45%, a maximum content of linalool, an effective ingredient, of 6.8 wt%, and little toxic solvent residue. The extraction method of the present invention has a simple process, low energy consumption, and is suitable for large-scale production and application. The jasmine flower essential oil prepared by the present invention has the effect of moisturizing and moisturizing, can also resist aging and reduce fine lines, make the skin smooth and delicate, and has a calming fragrance. DETAILED DESCRIPTION
[0022] The invention provides a method for extracting jasmine flower oil, comprising the following steps:
[0023] S1. Freeze, grind and freeze-dry jasmine flowers to obtain jasmine powder;
[0024] S2. The jasmine powder was mixed with ethanol at a ratio of 1 g: 2 to 5 mL, and the mixture was extracted to obtain an extract;
[0025] S3. The extract was filtered and ethanol was recovered by distillation under reduced pressure to obtain a crude extract;
[0026] S4. subjecting the crude extract to subcritical water extraction, centrifuging and filtering the extract to obtain jasmine flower oil.
[0027] In the present invention, first, jasmine flowers are picked, preferably in the afternoon of a sunny day, fresh jasmine buds with large buds, high yield and good quality are picked, and fresh jasmine flowers are washed with water, and the surface water is drained for standby use. Then the jasmine flowers are freeze-dried, and the jasmine flowers are frozen, ground and freeze-dried to obtain jasmine powder. The freezing temperature of the present invention is preferably -25~-20°C, more preferably -24~-22°C, and more preferably -23°C; the freezing time is preferably 20~30min, more preferably 22~28min, and more preferably 25min; the grinding is preferably frozen shear grinding to obtain jasmine powder, and the frozen shear grinding is preferably carried out in a grinder; the jasmine powder is naturally thawed at room temperature; then the thawed jasmine powder is vacuum freeze-dried, and the freeze-drying temperature is preferably -55~-50°C, more preferably -54~-52°C, and more preferably -53°C; the freeze-drying time is preferably 40~55min, more preferably 45~50min, and more preferably 47min. Freeze-drying jasmine flowers can better preserve the volatile components of jasmine flowers, and jasmine flower oil can be extracted during the non-flowering period of jasmine flowers.
[0028] In the present invention, jasmine powder is mixed with ethanol and extracted to obtain an extract; the ratio of jasmine powder to ethanol in the present invention is preferably 1g:2~5mL, more preferably 1g:3~4mL, more preferably 1g:3.5mL; the extraction is preferably microwave extraction, and the time of the microwave extraction is preferably 30~60min, more preferably 40~50min, more preferably 45min; during the microwave extraction, the use time of the microwave is preferably 3~5min / time, more preferably 4min / time, and after a single microwave is finished, the next microwave is preferably carried out for 10~15min, more preferably 12~14min, more preferably 13min; the number of microwave treatments is preferably 2~6 times, more preferably 3~5 times, more preferably 4 times; the power of the microwave is preferably 400~500W, more preferably 420~470W, more preferably 450W. The volume percentage of ethanol in the present invention is preferably 50~70%, more preferably 55~60%, more preferably 65%. Microwave heating is different from traditional heating methods. It does not require heat conduction. It can make the heated material itself a heating body. Therefore, even materials with poor thermal conductivity can reach the heating temperature in a very short time. During the microwave extraction process, high-frequency electromagnetic waves penetrate the extraction medium to the cells inside the jasmine powder. Due to the absorption of microwave energy, the temperature inside the cells rises rapidly, causing the pressure inside the cells to exceed the capacity of the cell wall expansion, causing the cells to rupture, and the effective ingredients in the cells flow out freely and dissolve in ethanol at a lower temperature to obtain an extract.
[0029] After obtaining the extract, the extract is filtered, and the filtration is preferably filtered with a microporous filter membrane to obtain a filtrate. The filtrate is subjected to vacuum distillation to obtain a crude extract; the vacuum degree of the vacuum distillation is preferably -0.07~-0.09Mpa, more preferably -0.08Mpa, and the temperature of the vacuum distillation is preferably 68~80°C, further preferably 62~77°C, and more preferably 74°C; preferably concentrated to an ethanol volume content of 10~20%, further preferably 12~18%, and more preferably 15%. Since ethanol has a high boiling point and its molecules contain polar hydroxyl groups and non-polar alkyl groups, when the ethanol content in the distilled concentrate drops to a certain level, further distillation to remove ethanol will cause a large loss of the aroma components of jasmine flower oil, and since ethanol forms an azeotropic reaction with aroma components such as alcohols and esters in the flower oil, it is also difficult to remove ethanol. In order to avoid the loss of jasmine flower oil components caused by long distillation time and azeotropic phenomenon, when the residual ethanol content in the obtained crude extract is 10-20%, subcritical water extraction is performed to further remove ethanol. The temperature of the subcritical water extraction of the present invention is preferably 30-40 ° C, more preferably 32-37 ° C, more preferably 35 ° C; the pressure of the subcritical water extraction is preferably 1.5-2.5 MPa, more preferably 1.7-2.2 MPa, more preferably 2.0 MPa; the solution flow rate of the subcritical water extraction is preferably 2.5-4.5 mL / min, more preferably 3-4 mL / min, more preferably 3.5 mL / min; the time of the subcritical water extraction is 40-70 min, more preferably 50-60 min, more preferably 55 min. The subcritical water extraction method is used to extract the flower oil from the pretreated jasmine flowers. The subcritical water extraction technology has low temperature, low pressure, low energy consumption and high extraction efficiency during the extraction process, and can effectively remove ethanol. The extraction liquid used is water, which is more environmentally friendly and will not change the performance and structure of the flower oil.
[0030] After obtaining the extract, the present invention centrifuges and filters to obtain jasmine flower oil. The centrifugal speed of the present invention is preferably 2500-3500 rpm, more preferably 2700-3300 rpm, and more preferably 3000 rpm; the centrifugal time is preferably 10-20 min, more preferably 12-18 min, and more preferably 15 min. The purpose of centrifugation is to further remove impurities in the jasmine flower oil.
[0031] The invention also provides application of the jasmine flower oil in preparing skin care products and spices.
[0032] The present invention also provides a moisturizing and soothing essential oil, comprising the following components in parts by weight: 0.4-1 parts of jasmine flower oil, 45-50 parts of squalane, 35-40 parts of camellia seed oil, 8-15 parts of ascorbyl tetraisopalmitate, 1-3 parts of vitamin E, and 0.5-1.5 parts of ubiquinone.
[0033] The weight proportion of the jasmine flower oil of the present invention is preferably 0.4-1 part, more preferably 0.6-0.8 part, and more preferably 0.7 part; the jasmine flower oil has soothing and moisturizing effects, the fragrance of the jasmine flower oil has a calming and soothing effect, and can also avoid the use of essences in skin care products.
[0034] The weight proportion of the squalane in the present invention is preferably 45-50 parts, more preferably 47-49 parts, and even more preferably 48 parts; the function of squalane is to repair the skin barrier and promote the penetration of other ingredients in the essence oil into the skin.
[0035] The weight proportion of the camellia seed oil of the present invention is preferably 35 to 40 parts, more preferably 36 to 38 parts, and more preferably 37 parts; the camellia seed oil has the effects of anti-oxidation and nourishment.
[0036] The weight proportion of ascorbyl tetraisopalmitate of the present invention is preferably 8 to 15 parts, more preferably 10 to 13 parts, and more preferably 12 parts; ascorbyl tetraisopalmitate is a vitamin C derivative, which can inhibit the activity of tyrosinase and play an antioxidant and moisturizing role.
[0037] The weight proportion of the vitamin E in the present invention is preferably 1 to 3 parts, preferably 1.5 to 2.5 parts, and more preferably 2.0 parts; vitamin E can help repair and strengthen the skin's natural protective barrier, lock in moisture in the skin, and provide deep nourishment from the inside out.
[0038] The weight proportion of the ubiquinone of the present invention is preferably 0.5 to 1.5 parts, more preferably 0.8 to 1.2 parts, and more preferably 1.0 part; ubiquinone has the effects of moisturizing and removing wrinkles.
[0039] The invention prepares an essential oil by compounding lily oil, squalane, camellia seed oil, ascorbyl tetraisopalmitate, vitamin E and ubiquinone, which has the effects of moisturizing and anti-oxidation, and can also resist aging and reduce fine lines, and has a soothing and calming fragrance.
[0040] The freeze dryer used in the present invention is a FD-1A-50 freeze dryer, the microwave extractor used in the present invention is an AL-IMC1 intelligent microwave extractor, and the subcritical extractor used in the present invention is a SD-Helix subcritical extractor.
[0041] The technical solutions provided by the present invention are described in detail below in conjunction with the embodiments, but they should not be construed as limiting the protection scope of the present invention. Example 1
[0042] (1) Picking jasmine flowers: Pick fresh jasmine buds with large buds, high yield and good quality on a sunny afternoon. Wash the fresh jasmine flowers with water and drain the surface water for later use.
[0043] (2) Freeze drying: Freeze the jasmine flowers at -25°C and grind them into powder. Thaw the quick-frozen jasmine powder at room temperature. After thawing, freeze-dry the powder at -55°C for 40 minutes to obtain jasmine powder.
[0044] (3) Microwave extraction: 1000 g of jasmine powder was mixed with 2000 mL of 50% ethanol by volume for microwave extraction. The microwave was used for 3 min / time. The next microwave was carried out 10 min after the end of a single microwave. The microwave power was 400 W. The total extraction time was 30 min to obtain the extract.
[0045] (4) Vacuum distillation: The extract obtained in step (3) is filtered through a microporous filter membrane, and the filtrate is subjected to vacuum distillation at -0.07 MPa and 48° C. (heating temperature) until the ethanol content is 10% by weight, thereby obtaining a crude extract.
[0046] (5) Subcritical water extraction: The crude extract was extracted at a temperature of 60°C, a pressure of 1.5 MPa, and a water flow rate of 2.4 mL / min for 40 min to obtain an extract. The extract was centrifuged at 2500 rpm for 10 min and filtered to obtain jasmine flower oil. Example 2
[0047] (1) Picking jasmine flowers: Pick fresh jasmine buds with large buds, high yield and good quality on a sunny afternoon. Wash the fresh jasmine flowers with water and drain the surface water for later use.
[0048] (2) Freeze drying: Freeze the jasmine flowers at -20°C and grind them into powder. Then, thaw the quick-frozen jasmine powder at room temperature. After thawing, freeze-dry the powder at -50°C for 55 minutes to obtain jasmine powder.
[0049] (3) Microwave extraction: 1000 g of jasmine powder was mixed with 5000 mL of 70% ethanol for microwave extraction. The microwave was used for 5 min / time. The next microwave was carried out 15 min after the end of a single microwave. The microwave power was 500 W. The total extraction time was 60 min to obtain the extract.
[0050] (4) Vacuum distillation: The extract obtained in step (3) is filtered through a microporous filter membrane, and the filtrate is subjected to vacuum distillation at -0.09 MPa and 60° C. (heating temperature) until the ethanol weight content is 20%, thereby obtaining a crude extract.
[0051] (5) Subcritical water extraction: The crude extract was extracted at a temperature of 70°C, a pressure of 2.5 MPa, and a water flow rate of 4.5 mL / min for 70 min to obtain an extract. The extract was centrifuged at 3500 rpm for 20 min and filtered to obtain jasmine flower oil. Example 3
[0052] (1) Picking jasmine flowers: Pick fresh jasmine buds with large buds, high yield and good quality on a sunny afternoon. Wash the fresh jasmine flowers with water and drain the surface water for later use.
[0053] (2) Freeze drying: Freeze the jasmine flowers at -22°C and grind them into powder. Thaw the quick-frozen jasmine powder at room temperature. After thawing, freeze-dry the powder at -52°C for 45 minutes to obtain jasmine powder.
[0054] (3) Microwave extraction: 1000 g of jasmine powder was mixed with 3000 mL of 55% ethanol for microwave extraction. The microwave was used for 4 min / time. The next microwave was carried out 12 min after the end of a single microwave. The microwave power was 430 W. The total extraction time was 40 min to obtain the extract.
[0055] (4) Vacuum distillation: The extract obtained in step (3) is filtered through a microporous filter membrane, and the filtrate is subjected to vacuum distillation at -0.08 MPa and 52° C. (heating temperature) until the ethanol content by weight is 15%, thereby obtaining a crude extract.
[0056] (5) Subcritical water extraction: The crude extract was extracted at a temperature of 64°C, a pressure of 2.0 MPa, and a water flow rate of 3.5 mL / min for 50 min to obtain an extract. The extract was centrifuged at 2800 rpm for 15 min and filtered to obtain jasmine flower oil. Example 4
[0057] (1) Picking jasmine flowers: Pick fresh jasmine buds with large buds, high yield and good quality on a sunny afternoon. Wash the fresh jasmine flowers with water and drain the surface water for later use.
[0058] (2) Freeze drying: Freeze the jasmine flowers at -23°C and grind them into powder. Thaw the quick-frozen jasmine powder at room temperature. After thawing, freeze-dry the powder at -54°C for 50 minutes to obtain jasmine powder.
[0059] (3) Microwave extraction: 1000 g of jasmine powder was mixed with 4000 mL of 60% ethanol for microwave extraction. The microwave was used for 3 min / time. The next microwave was carried out 15 min after the end of a single microwave. The microwave power was 470 W. The total extraction time was 50 min to obtain the extract.
[0060] (4) Vacuum distillation: The extract obtained in step (3) is filtered through a microporous filter membrane, and the filtrate is subjected to vacuum distillation at -0.09 MPa and 56° C. (heating temperature) until the ethanol weight content is 18%, thereby obtaining a crude extract.
[0061] (5) Subcritical water extraction: The crude extract was extracted for 60 min at a temperature of 66°C, a pressure of 2.2 MPa, and a water flow rate of 4.0 mL / min to obtain an extract. The extract was centrifuged at 3000 rpm for 18 min and filtered to obtain jasmine flower oil. Example 5
[0062] A moisturizing and soothing essential oil: comprising 0.4g of jasmine flower oil prepared in Example 1, 45g of squalane, 35g of camellia seed oil, 8g of ascorbyl tetraisopalmitate, 1g of vitamin E, and 0.5g of ubiquinone. Add jasmine flower oil, camellia seed oil, ascorbyl tetraisopalmitate, and vitamin E into an emulsifying pot, heat to 85°C, homogenize at 1500rpm for 3min, keep warm for 30min, stir at 20rpm for 30min, cool down to 45°C for 20min under stirring at 15rpm, add squalane and ubiquinone, and cool down to 40°C for 15min to obtain a moisturizing and soothing essential oil. Example 6
[0063] A moisturizing and soothing essential oil: comprising 1 g of jasmine flower oil prepared in Example 2, 50 g of squalane, 40 g of camellia seed oil, 15 g of ascorbyl tetraisopalmitate, 3 g of vitamin E, and 1.5 g of ubiquinone, and the preparation method is the same as that of Example 5. Example 7
[0064] A moisturizing and soothing essential oil: comprising 0.6 g of jasmine flower oil prepared in Example 3, 47 g of squalane, 37 g of camellia seed oil, 10 g of ascorbyl tetraisopalmitate, 1.5 g of vitamin E, and 0.8 g of ubiquinone, and the preparation method is the same as that of Example 5. Example 8
[0065] A moisturizing and soothing essential oil: comprising 0.8 g of jasmine flower oil prepared in Example 4, 49 g of squalane, 38 g of camellia seed oil, 13 g of ascorbyl tetraisopalmitate, 2.0 g of vitamin E, and 1.2 g of ubiquinone, and the preparation method is the same as that of Example 5. Comparative Example 1
[0066] The difference from Example 3 is that petroleum ether is used to replace ethanol, and the other preparation methods and parameters are the same as those of Example 3. Comparative Example 2
[0067] The difference from Example 3 is that the microwave power is 600 W, and the other preparation methods and parameters are the same as those of Example 3. Comparative Example 3
[0068] The difference from Example 3 is that the reduced pressure is used to concentrate until the ethanol weight content is 5%. Other preparation methods and parameters are the same as those in Example 3. Comparative Example 4
[0069] The difference from Example 3 is that the solution flow rate of subcritical water extraction is 6 mL / min, and the other preparation methods and parameters are the same as those of Example 3. Comparative Example 5
[0070] Different from Example 5, the essential oil does not contain jasmine flower oil. Comparative Example 6
[0071] Different from Example 5, the essential oil does not contain squalane. Comparative Example 7
[0072] Different from Example 5, the essential oil does not contain camellia seed oil.
[0073] Experimental Example 1 Determination of the yield of jasmine flower oil
[0074] The jasmine flower oil obtained in Examples 1 to 4 and Comparative Examples 1 to 4 was weighed and the yield was calculated. The results are shown in Table 1.
[0075]
[0076] As can be seen from Table 1, the yields of jasmine flower oil in Examples 1 to 4 are 6.25%, 6.73%, 7.39% and 7.54% respectively; the yield of jasmine flower oil in Comparative Example 1 is 6.58%. Although the yield is relatively high, there is toxic solvent residue in the jasmine flower oil extracted by petroleum ether; the yield of jasmine flower oil in Comparative Example 2 is 5.31%, which is lower than that in Example 3; the yield of jasmine flower oil in Comparative Example 3 is only 4.60%, indicating that too long distillation time will cause jasmine flower oil loss; the yield of jasmine flower oil in Comparative Example 4 is 5.27, which is lower than that in Example 3.
[0077] Experimental Example 2 Determination of linalool content in jasmine flower oil
[0078] The GC-MC determination of jasmine flower oil was performed using a Shanghai Instrument GC126N gas chromatograph to determine the linalool content. Chromatographic conditions: column temperature was initially 45°C, and the temperature was increased to 75°C at 10°C per minute and maintained for 13 minutes; injection port temperature was 220°C; detector temperature was 220°C, FID detection; carrier gas was nitrogen, flow rate was 2.0 mL / min; split injection, split ratio was 16:1. The determination results are shown in Table 2.
[0079]
[0080] As can be seen from Table 2, the linalool contents in the jasmine flower oils of Examples 1 to 4 are 5.8wt%, 6.2wt%, 6.5wt%, and 6.8wt%, respectively, and the linalool contents in the jasmine flower oils of Comparative Examples 1 to 4 are 6.0wt%, 4.6wt%, 3.7wt%, and 5.0wt%, respectively, indicating that higher power is not conducive to the extraction of volatile substances in jasmine flower oil, and too long distillation time will destroy the effective ingredients in jasmine flower oil.
[0081] Experimental Example 3 Determination of organic residues in jasmine flower oil
[0082] According to the residual solvent determination method (General Rules 0861 Second Method of the 2020 Edition of the Chinese Pharmacopoeia), the ethanol residue in Examples 1 to 4 and Comparative Examples 2 to 4 and the hydrocarbon organic solvent residue in Comparative Example 1 were determined, and the results are shown in Table 3.
[0083]
[0084] As shown in Table 3, the ethanol residues in the jasmine flower oils of Examples 1 to 4 are 1.2ppm, 1.1ppm, 0.8ppm, and 1.0ppm, respectively, and the organic residues are relatively low. The hydrocarbon organic solvent residues in the jasmine flower oil of Comparative Example 1 are 10.2ppm, and the organic residues are relatively high; the ethanol residues in the jasmine flower oils of Comparative Examples 2 and 3 are 0.8ppm and 0.7ppm, respectively; the ethanol residue in the jasmine flower oil of Comparative Example 4 is 3.4ppm, indicating that too high a water flow rate is not conducive to the removal of ethanol.
[0085] Experimental Example 4 Determination of moisturizing effect of essence oil
[0086] 35 healthy volunteers aged 18 to 50 were selected, half male and half female. According to QB / T4256-2011 Cosmetic Moisturizing Efficacy Evaluation Guide, the test parts should not use any cosmetics for 2 to 3 days before the test, and should not be exposed to water for 2 hours. Before the experiment, the subjects need to clean the inner forearms of both hands. The cleaning method is to use a paper towel to clean it. The test sample is (2.0±0.1)mg / cm 2The amount of the sample was applied once and evenly applied to the test area. The moisture content was measured with a skin moisture tester (CorneometerCM825, Germany) at 0h, 0.5h, 1h, 2h, 3h, 4h after use and before using the essence oil. Different points were selected in the same area for measurement 3 times. Each essence oil sample was tried by 5 volunteers respectively. The measurement results at each time point were averaged from 5 parallel experiments to avoid the influence of personal skin quality level. The moisturizing effect of the essence oil is shown in Table 4.
[0087] Results judging criteria:
[0088] Skin moisture content <30% is very dry;
[0089] Skin moisture content of 30-40% is considered dry;
[0090] Skin with a water content of 40-50% is considered hydrated;
[0091] Skin with a water content of >50% is considered extremely hydrated.
[0092]
[0093] As shown in Table 4, the moisturizing and soothing essence oil prepared by compounding lily flower oil, squalane, camellia seed oil, ascorbyl tetraisopalmitate, vitamin E and ubiquinone has good moisturizing properties, high stability, and maintains its efficacy longer; the skin of the subjects was still fully hydrated 4 hours after using the essence oil product, while the skin moisture content values of the other experimental groups decreased significantly, and basically dropped to a medium level 3 hours after the use of the essence oil, and the moisturizing effect was shorter.
[0094] Experimental Example 5 Determination of the soothing properties of essential oil
[0095] Experimental principle: Hyaluronic acid is an important component of the extracellular matrix of the skin and plays an important role in maintaining the volume of the extracellular matrix and the normal physiological function of the skin. Hyaluronidase is an enzyme that can hydrolyze hyaluronic acid and is related to most IgE-mediated type I and T-cell-mediated type IV allergic reactions. In addition, the hydrolysis products of hyaluronic acid promote skin inflammatory reactions. Inhibiting the activity of hyaluronidase can ensure the normal content and function of hyaluronic acid in the skin.
[0096] This test method is an in vitro method, which characterizes the soothing effect by evaluating the inhibition rate of the test sample on hyaluronidase activity.
[0097] The hyaluronidase inhibition test was performed according to the Elson-Morgan modified method, and three parallel experiments were set for each essential oil, and the average value was taken. The test results are shown in Table 5:
[0098]
[0099]
[0100] As shown in Table 5, the moisturizing and soothing essence oil prepared by compounding lily flower oil, squalane, camellia seed oil, ascorbyl tetraisopalmitate, vitamin E and ubiquinone has a good hyaluronidase inhibition rate, indicating that the essence oil of the present invention has the ability to inhibit hyaluronidase activity and has a soothing effect.
[0101] Experimental Example 6 DPPH free radical scavenging experiment
[0102] Freshly prepare 200μmol / L DPPH ethanol solution, measure the light absorption value (A) at 517nm wavelength, record it as A0, and use it to prepare 1.0ml target concentration antioxidant (Examples 5-8, control group 8.0μg / ml Vc, comparative examples 5-7) and 9.0ml 200μmol / L DPPH ethanol mixed solution, each sample is repeated 3 times. Mix and immediately measure the light absorption value (A) at 517nm wavelength, and the absorbance value is recorded as A1. Incubate at 37℃ in the dark for 30min and measure the absorbance value, record it as A2, blank control test
[0103] is 10mL DPPH ethanol solution, and its absorbance is recorded as A0. The relative scavenging rate γ of the sample to DPPH is calculated according to formula (1).
[0104] γ = (1- )×100% Formula (1)
[0105] The DPPH free radical scavenging rate is shown in Table 6:
[0106]
[0107] The greater the clearance rate, the stronger the antioxidant capacity. It can be seen from Table 6 that the DPPH free radical clearance rates of the jasmine essential oils of Examples 5 to 6 are 85.3%, 86.5%, 83.2%, and 85.7%, respectively, the removal rate of Vc in the control group is 90.6%, and the removal rates of Comparative Examples 5 to 7 are 52.6%, 62.3%, and 57.5%, respectively, which proves that jasmine essential oil has a strong antioxidant capacity.
[0108] The above is only 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 principle of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.
Claims
1. A method for extracting jasmine flower oil, characterized in that: The following steps are involved: S1. Freeze, grind and freeze-dry jasmine flowers to obtain jasmine powder; S2. The jasmine powder was mixed with ethanol at a ratio of 1 g: 2 to 5 mL, and the mixture was extracted to obtain an extract; S3. The extract was filtered, ethanol was recovered by vacuum distillation, and the ethanol volume content was 10 to 20% to obtain a crude extract; S4. The crude extract is subjected to subcritical water extraction, and the extract is centrifuged and filtered to obtain jasmine flower oil; The extraction in step S2 is microwave extraction, and the time of microwave extraction is 30 to 60 minutes; The microwave extraction is intermittent, the microwave treatment time is 3-5 min / time, the next microwave is carried out 10-15 min after the single microwave treatment, the number of microwave treatments is 2-6 times, and the microwave power is 400-500 W; The temperature of the subcritical water extraction is 70-105° C., the pressure is 1.5-2.5 MPa, and the solution flow rate is 2.5-4.5 mL / min; the time of the subcritical water extraction is 40-70 min.
2. The extraction method according to claim 1, characterized in that The freezing temperature is -25 to -20°C, and the freezing time is 20 to 30 minutes.
3. The extraction method according to claim 1, characterized in that The freeze-drying temperature is -55~-50°C.
4. The extraction method according to claim 1, characterized in that The vacuum degree of the reduced pressure distillation is -0.08~-0.09Mpa, and the temperature of the reduced pressure distillation is 68~80°C.
5. The jasmine flower oil obtained by extracting according to any one of claims 1 to 4.
6. Use of the jasmine flower oil according to claim 5 in preparing skin care products and spices.
7. A moisturizing and soothing essential oil, characterized in that: Contains the following components in parts by weight: 0.4-1 parts of jasmine flower oil prepared according to claim 1, 45-50 parts of squalane, 35-40 parts of camellia seed oil, 8-15 parts of ascorbyl tetraisopalmitate, 1-3 parts of vitamin E, and 0.5-1.5 parts of ubiquinone.
Citation Information
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