Long-lasting fragrance and method for preparing the same

Abstract

This invention relates to a long-lasting fragrance perfume and its preparation method, belonging to the field of daily chemical technology. The perfume is alcohol-free and consists of a complex fragrance oil, modified chitosan microcapsules, a polymeric sustained-release carrier, a stabilizer, a fermentation extract, and deionized water. The complex fragrance oil is obtained through supercritical CO2 extraction. The modified chitosan microcapsules are made by loading volatile precursor fragrances onto quaternized modified chitosan. The polymeric sustained-release carrier is a compound of polylactic acid-glycolic acid copolymer and sodium carboxymethyl cellulose. The fermentation extract is derived from bergamot and other raw materials through fermentation with Saccharomyces cerevisiae. Through a dual sustained-release mechanism of "microcapsule targeted release + slow degradation by polymeric carrier," combined with small-molecule fermentation extract, it solves the problems of short-lasting fragrance, poor stability, and insufficient gentleness in existing alcohol-free perfumes. It has the advantages of long-lasting fragrance, uniform fragrance evaporation, stable system, gentle and non-irritating properties, and suitability for all skin types. The preparation process is simple and easy for industrial production.

Description

Technical Field

[0001] This invention belongs to the field of daily chemical technology and relates to a long-lasting fragrance perfume and its preparation method. Background Technology

[0002] As a common daily beauty product, perfume's core function is to release fragrance through evaporation, enhancing the user's personal charm. With increasing consumer health awareness, alcohol-free perfumes, avoiding skin irritation and respiratory discomfort caused by alcohol, are gradually becoming a mainstream market demand. However, existing alcohol-free perfumes generally face two major technical bottlenecks: First, short lasting power. Due to the lack of alcohol's solubilizing and evaporation-regulating effects on fragrance components, the fragrance evaporates quickly, typically lasting only 4-8 hours, failing to meet consumers' demand for long-lasting fragrance. Second, it's difficult to balance stability and gentleness. Some products add high concentrations of polymers to prolong fragrance, resulting in a viscous system that easily separates and may increase the risk of skin sensitization. Furthermore, traditional perfume essential oils are often prepared using methods such as distillation and solvent extraction, leading to significant loss of fragrance components. Direct addition of extracts results in large molecular weights and poor compatibility with other components, easily causing uneven evaporation and problems such as an initially strong fragrance that fades later.

[0003] Therefore, developing an alcohol-free perfume that combines long-lasting fragrance, gentleness, non-irritation, uniform fragrance evaporation, and system stability has become a pressing technical problem for the industry. This invention successfully solves the technical contradictions of short-lasting fragrance, poor stability, and insufficient gentleness in alcohol-free perfumes by employing a dual sustained-release mechanism of "targeted release from modified chitosan microcapsules + slow degradation by a polymer composite sustained-release carrier," combined with the synergistic effect of small-molecule extracts fermented with specific microbial strains. Summary of the Invention

[0004] The purpose of this invention is to provide a long-lasting fragrance perfume and its preparation method. The perfume is alcohol-free, has a long-lasting fragrance, is gentle and non-irritating, suitable for all skin types, and has uniform fragrance evaporation, high system stability, and a simple preparation process that is easy to industrialize.

[0005] The objective of this invention can be achieved through the following technical solutions:

[0006] A long-lasting fragrance, comprising the following components in parts by weight: 5-15 parts of complex essential oil, 8-20 parts of modified chitosan microcapsules, 10-25 parts of polymeric sustained-release carrier, 2-8 parts of stabilizer, 3-10 parts of fermentation extract, and deionized water to make up to 100 parts.

[0007] The compound essential oil was prepared by supercritical CO2 extraction.

[0008] The modified chitosan microcapsules are made of quaternized modified chitosan loaded with volatile precursor fragrances, with a particle size of 50-200 nm.

[0009] The fermented extract is obtained by mixing bergamot, ylang-ylang, cassia and lily of the valley in a mass ratio of (1-3):(0.5-2):(0.5-2):(0.5-2), fermenting with brewer's yeast, and then extracting by ethanol reflux.

[0010] The polymeric sustained-release carrier is a compound of polylactic acid-hydroxyacetic acid copolymer and sodium carboxymethyl cellulose in a mass ratio of (2-5):1.

[0011] As a preferred technical solution of the present invention, the raw materials of the compound essential oil include rose petals, jasmine petals, lavender and lemon peel, and the mass ratio of the four is (3-5):(2-4):(1-3):(1-2).

[0012] As a preferred embodiment of the present invention, the process parameters for supercritical CO2 extraction are: extraction pressure 35-45 MPa, extraction temperature 38-45℃, CO2 flow rate 15-25 L / h, and extraction time 2-4 h.

[0013] As a preferred embodiment of the present invention, the method for preparing the quaternized modified chitosan is as follows: chitosan is dissolved in a 1% acetic acid solution, 3-chloro-2-hydroxypropyltrimethylammonium chloride is added, the mass ratio of chitosan to 3-chloro-2-hydroxypropyltrimethylammonium chloride is 1:(0.8-1.2), the reaction is carried out at 60-70℃ for 4-6 hours, the pH is adjusted to 7-8, and the mixture is filtered, washed and dried to obtain the quaternized modified chitosan.

[0014] As a preferred embodiment of the present invention, the volatile precursor fragrance is one or more of citral, citronellol, and geraniol, and the mass ratio of modified chitosan to volatile precursor fragrance is (3-5):1.

[0015] As a preferred embodiment of the present invention, the preparation conditions of the fermentation extract are as follows: the inoculation amount of brewer's yeast is 3-5% of the mass of the mixed raw materials, the fermentation temperature is 29-31℃, the fermentation time is 50-60h, and the fermentation pH is 5.0-6.0; the process parameters for ethanol reflux extraction are as follows: ethanol concentration is 70-80%, the material-to-liquid ratio is 1:15-20, the reflux temperature is 80-85℃, and the reflux time is 2-3h.

[0016] As a preferred embodiment of the present invention, the stabilizer is a mixture of vitamin E and triethyl citrate in a mass ratio of (1-2):1.

[0017] As a preferred embodiment of the present invention, the polylactic acid-glycolic acid copolymer has a molecular weight of 5000-10000 Da and the sodium carboxymethyl cellulose has a degree of substitution of 0.6-0.8.

[0018] A method for preparing a long-lasting fragrance as described above includes the following steps:

[0019] S1: Preparation of compound essential oil: Weigh rose petals, jasmine petals, lavender and lemon peel according to the mass ratio, crush them to 20-40 mesh, add them to a supercritical extraction vessel, set the extraction pressure to 35-45MPa, the extraction temperature to 38-45℃, and the CO2 flow rate to 15-25L / h, extract for 2-4h, collect the extract, and dry it with anhydrous sodium sulfate to obtain compound essential oil for later use;

[0020] S2: Preparation of modified chitosan microcapsules:

[0021] S2.1: Preparation of quaternized modified chitosan: Chitosan was dissolved in 1% acetic acid solution and stirred until completely dissolved. 3-chloro-2-hydroxypropyltrimethylammonium chloride was added and reacted at a constant temperature of 60-70℃ for 4-6 hours. After the reaction was completed, the pH was adjusted to 7-8 with 10% NaOH solution. The precipitate was collected by filtration and washed with deionized water until the washing solution was neutral. The precipitate was then dried under vacuum at 60℃ for 8 hours to obtain quaternized modified chitosan.

[0022] S2.2: Preparation of microcapsules: Weigh the modified chitosan and volatile precursor fragrance according to the mass ratio, add deionized water (the mass ratio of modified chitosan to deionized water is 1:10-15), stir and emulsify at 8000-10000 rpm at 50-60℃ for 30-40 min, add glutaraldehyde crosslinking agent, react at 40-50℃ for 2-3 h, cool to room temperature, centrifuge at 8000 rpm for 15 min, collect the precipitate, wash 3 times with deionized water, and vacuum dry at 50℃ for 6 h to obtain modified chitosan microcapsules for later use;

[0023] S3: Preparation of fermentation extract:

[0024] S3.1: Raw material pretreatment: Take bergamot peel, ylang-ylang flowers, cassia leaves and lily of the valley flowers respectively, wash and dry them, then grind them to 40-60 mesh, mix them according to the set mass ratio to obtain mixed raw materials;

[0025] S3.2: Fermentation treatment: Mix the mixed raw materials with deionized water at a mass ratio of 1:5, add brewing yeast (inoculation amount is 3-5% of the mass of mixed raw materials), adjust the pH to 5.0-6.0, and ferment at 29-31℃ for 50-60 hours. Stir once every 8 hours for 10 minutes each time during the fermentation process.

[0026] S3.3: Extraction and purification: After fermentation, filter the fermentation broth, take the filter residue, add 70-80% ethanol solution (material-liquid ratio 1:15-20), reflux at 80-85℃ for 2-3 hours, filter, collect the filtrate, and recover the ethanol by vacuum distillation to obtain the fermentation extract for later use.

[0027] S4: Preparation of mixed matrix solution: Weigh out the polymer slow-release carrier (PLGA and CMC-Na), stabilizer (vitamin E and triethyl citrate), and deionized water according to the mass ratio, add them to the reaction vessel, and stir at 350-450 rpm for 1-2 hours at 35-40℃ until all components are completely dissolved to obtain the mixed matrix solution.

[0028] S5: Dispersing microcapsules: Add the modified chitosan microcapsules prepared in step S2 to the mixed matrix liquid, turn on the ultrasonic disperser, set the ultrasonic power to 300-400W and the ultrasonic time to 15-25min, so that the microcapsules are evenly dispersed to obtain a microcapsule dispersion.

[0029] S6: Mixing aroma components: Add the compound essential oil prepared in step S1 and the fermented extract prepared in step S3 to the microcapsule dispersion, and stir at 400-500 rpm for 30-60 min at 30-35℃ to fully mix the aroma components with the matrix liquid.

[0030] S7: Post-treatment: Cool the mixture to room temperature, let it stand for 12-24 hours, filter it through a 0.22μm organic phase filter membrane to remove impurities and undispersed particles, and obtain a long-lasting fragrance.

[0031] As a preferred technical solution of the present invention, the preparation of modified chitosan microcapsules in step S2 includes: mixing modified chitosan with volatile precursor fragrance, adding deionized water, stirring and emulsifying at 8000-10000 rpm for 30-40 min at 50-60℃, adding 5-10% of glutaraldehyde crosslinking agent by weight of modified chitosan, reacting at 40-50℃ for 2-3 h, cooling, centrifuging, washing until neutral, and drying to obtain modified chitosan microcapsules.

[0032] The beneficial effects of this invention are:

[0033] (1) Significant long-lasting fragrance effect: This invention uses a dual slow-release mechanism of "targeted release of modified chitosan microcapsules + slow degradation of polymer composite slow-release carrier" and combines fermented small molecule extracts to synergistically regulate the evaporation rate, effectively extending the fragrance time of perfume.

[0034] (2) This invention does not contain alcohol, and the molecular weight of the fermented extract is reduced after fermentation with brewer's yeast, which improves its compatibility with the system and makes it mild and suitable for sensitive skin.

[0035] (3) The preparation process of the present invention uses conventional equipment, the steps are clear, it is easy to industrialize, and all components are food-grade or cosmetic-grade raw materials, which are highly safe and have broad market application prospects. Detailed Implementation

[0036] To further illustrate the technical means and effects of the present invention in achieving its intended purpose, the following detailed description of the specific implementation methods, structures, features, and effects of the present invention, in conjunction with embodiments, is provided below.

[0037] Example 1

[0038] A long-lasting fragrance, with the following components in parts by weight:

[0039] 8 parts blended essential oil (3 parts rose petals, 2 parts jasmine petals, 2 parts lavender, 1 part lemon peel)

[0040] 12 parts of modified chitosan microcapsules (9.6 parts of quaternized modified chitosan and 2.4 parts of citral)

[0041] 15 parts of polymeric sustained-release carrier (12 parts PLGA, 3 parts CMC-Na, PLGA molecular weight 8000 Da, CMC-Na degree of substitution 0.7)

[0042] Stabilizer 4 parts (Vitamin E 2.7 parts, Triethyl Citrate 1.3 parts)

[0043] Five portions of fermented extracts (2 portions of bergamot, 1 portion of ylang-ylang, 1 portion of cassia, and 1 portion of lily of the valley).

[0044] 56 portions of deionized water

[0045] The preparation method is as follows:

[0046] S1: Preparation of compound essential oil: Crush 3kg of rose petals, 2kg of jasmine petals, 2kg of lavender and 1kg of lemon peel to 30 mesh, add to a supercritical extraction vessel, set the extraction pressure to 40MPa, extraction temperature to 42℃ and CO2 flow rate to 20L / h, extract for 3h, collect the extract, dry with anhydrous sodium sulfate to obtain 8kg of compound essential oil for later use.

[0047] S2: Preparation of modified chitosan microcapsules:

[0048] S2.1: Preparation of quaternized modified chitosan: 10 kg of chitosan (Xi'an Aosai Biotechnology Co., Ltd.) was dissolved in 1000 L of 1% acetic acid solution and stirred until completely dissolved. 10 kg of 3-chloro-2-hydroxypropyltrimethylammonium chloride was added and reacted at 65℃ for 5 h. The pH was adjusted to 7.5 with 10% NaOH solution. The precipitate was collected by filtration and washed with deionized water until the washing solution was neutral. The precipitate was vacuum dried at 60℃ for 8 h to obtain 12 kg of quaternized modified chitosan.

[0049] S2.2: Preparation of microcapsules: Weigh 9.6 kg of modified chitosan and 2.4 kg of citral, add 96 L of deionized water, and emulsify at 9000 rpm at 55 °C for 35 min. Add 0.77 kg of glutaraldehyde crosslinking agent (8% of the mass of modified chitosan), react at 45 °C for 2.5 h, cool to room temperature, centrifuge at 8000 rpm for 15 min, collect the precipitate, wash 3 times with deionized water, and vacuum dry at 50 °C for 6 h to obtain 12 kg of modified chitosan microcapsules for later use.

[0050] S3: Preparation of fermentation extract:

[0051] S3.1: Take 2kg of bergamot peel, 1kg of ylang-ylang flowers, 1kg of cassia leaves, and 1kg of lily of the valley flowers, wash and dry them, then grind them to 50 mesh and mix them to obtain 5kg of mixed raw materials;

[0052] S3.2: Mix 5 kg of the mixed raw material with 25 L of deionized water, and add 0.2 kg of activated water until the concentration reaches 1 × 10⁻⁶. 8 Inoculate with CFU / mL of Saccharomyces cerevisiae (CICC®1392) (4% of the mass of the mixed raw materials), adjust the pH to 5.5, and ferment at 30°C for 55 hours. Stir for 10 minutes every 8 hours during the fermentation process.

[0053] S3.3: After fermentation, filter the fermentation broth, take the filter residue, add 90L of 75% ethanol solution (material-to-liquid ratio 1:18), reflux extract at 82℃ for 2.5h, filter, collect the filtrate, and recover the ethanol by vacuum distillation to obtain 5kg of fermentation extract for later use.

[0054] S4: Weigh 12kg PLGA, 3kg CMC-Na, 2.7kg Vitamin E, 1.3kg Triethyl Citrate, and 56L Deionized Water, add them to the reaction vessel, and stir at 400rpm for 1.5h at 38℃ until all components are completely dissolved to obtain a mixed matrix solution.

[0055] S5: Add 12 kg of modified chitosan microcapsules to the mixed matrix solution, turn on the ultrasonic disperser, set the ultrasonic power to 350 W and the ultrasonic time to 20 min, so that the microcapsules are evenly dispersed to obtain a microcapsule dispersion.

[0056] S6: Add 8 kg of compound essential oil and 5 kg of fermented extract to the microcapsule dispersion, and stir at 450 rpm for 45 min at 32℃ to fully mix the aroma components with the matrix liquid;

[0057] S7: Cool the mixture to room temperature, let it stand for 18 hours, and filter it through a 0.22μm organic phase filter membrane to obtain a long-lasting fragrance perfume.

[0058] Example 2

[0059] A long-lasting fragrance, with the following components in parts by weight:

[0060] 10 parts blended essential oil (4 parts rose petals, 3 parts jasmine petals, 2 parts lavender, 1 part lemon peel)

[0061] 15 parts of modified chitosan microcapsules (12 parts of quaternized modified chitosan and 3 parts of citronellol).

[0062] 18 parts of polymeric sustained-release carrier (14 parts PLGA, 4 parts CMC-Na, PLGA molecular weight 10000 Da, CMC-Na degree of substitution 0.8)

[0063] Stabilizer 5 parts (Vitamin E 3.3 parts, Triethyl Citrate 1.7 parts)

[0064] Fermented extracts (3 parts bergamot, 2 parts ylang-ylang, 1 part cassia, 1 part lily of the valley)

[0065] 45 parts deionized water

[0066] The preparation method is as follows:

[0067] S1: Preparation of compound essential oil: 4 kg of rose petals, 3 kg of jasmine petals, 2 kg of lavender and 1 kg of lemon peel are crushed to 35 mesh and added to a supercritical extraction vessel. The extraction pressure is set to 42 MPa, the extraction temperature to 43℃ and the CO2 flow rate to 22 L / h. The extraction is carried out for 3.5 h. The extract is collected and dried with anhydrous sodium sulfate to obtain 10 kg of compound essential oil for later use.

[0068] S2: Preparation of modified chitosan microcapsules:

[0069] S2.1: Preparation of quaternized modified chitosan: Dissolve 15 kg of chitosan in 1500 L of 1% acetic acid solution and stir until completely dissolved. Add 18 kg of 3-chloro-2-hydroxypropyltrimethylammonium chloride (mass ratio 1:1.2) and react at 68 °C for 5.5 h. Adjust the pH to 7.8 with 10% NaOH solution, filter and collect the precipitate, wash with deionized water until neutral, and vacuum dry at 60 °C for 8 h to obtain 18 kg of quaternized modified chitosan.

[0070] S2.2: Preparation of microcapsules: Weigh 12 kg of modified chitosan and 3 kg of citronellol, add 144 L of deionized water, stir and emulsify at 9500 rpm at 58 °C for 38 min, add 1.2 kg of glutaraldehyde crosslinking agent (10% of the mass of modified chitosan), react at 48 °C for 2.8 h, cool, centrifuge at 8000 rpm for 15 min, wash 3 times, vacuum dry at 50 °C for 6 h to obtain 15 kg of modified chitosan microcapsules for later use;

[0071] S3: Preparation of fermentation extract:

[0072] S3.1: Take 3kg of bergamot peel, 2kg of ylang-ylang flowers, 1kg of cassia leaves, and 1kg of lily of the valley flowers, grind them to 55 mesh, and mix them to obtain 7kg of mixed raw materials;

[0073] S3.2: Mix 7 kg of the mixed raw materials with 35 L of deionized water, and add 0.35 kg of activated water to a concentration of 1 × 10⁻⁶. 8 Inoculate with 5% CFU / mL of Saccharomyces cerevisiae, adjust pH to 5.8, ferment at 31℃ for 58 hours, stirring for 10 minutes every 8 hours;

[0074] S3.3: Filter the fermentation broth, take the filter residue, add 126L of 78% ethanol solution (solid-liquid ratio 1:18), reflux at 84℃ for 2.8h, filter, and recover the ethanol by vacuum distillation to obtain 7kg of fermentation extract for later use.

[0075] S4: Weigh 14kg PLGA, 4kg CMC-Na, 3.3kg Vitamin E, 1.7kg Triethyl Citrate, and 45L Deionized Water, and stir at 39℃ and 420rpm for 1.8h to obtain a mixed matrix solution;

[0076] S5: Add 15kg of modified chitosan microcapsules, sonicate at 380W for 22min to obtain microcapsule dispersion;

[0077] S6: Add 10kg of compound essential oil and 7kg of fermented extract, stir at 480rpm for 50min at 34℃ until well mixed;

[0078] S7: Cool to room temperature, stand for 20 hours, filter through a 0.22μm filter membrane to obtain a long-lasting fragrance perfume.

[0079] Example 3

[0080] A long-lasting fragrance, with the following components in parts by weight:

[0081] 6 parts blended essential oil (2 parts rose petals, 2 parts jasmine petals, 1 part lavender, 1 part lemon peel)

[0082] 10 parts of modified chitosan microcapsules (8 parts of quaternized modified chitosan and 2 parts of geraniol)

[0083] 12 polymeric sustained-release carriers (9 parts PLGA, 3 parts CMC-Na; PLGA molecular weight 6000 Da, CMC-Na degree of substitution 0.6)

[0084] Stabilizer 3 parts (2 parts Vitamin E, 1 part Triethyl Citrate)

[0085] Four parts of fermented extract (1.5 parts bergamot, 1 part ylang-ylang, 0.5 parts cassia, and 1 part lily of the valley).

[0086] 65 parts deionized water

[0087] The preparation method is as follows:

[0088] S1: Preparation of compound essential oil: Crush 2kg of rose petals, 2kg of jasmine petals, 1kg of lavender and 1kg of lemon peel to 25 mesh, add to a supercritical extraction vessel, set the extraction pressure to 38MPa, extraction temperature to 40℃ and CO2 flow rate to 18L / h, extract for 2.5h, collect the extract, dry with anhydrous sodium sulfate to obtain 6kg of compound essential oil for later use;

[0089] S2: Preparation of modified chitosan microcapsules:

[0090] S2.1: Preparation of quaternized modified chitosan: Dissolve 8 kg of chitosan in 800 L of 1% acetic acid solution, add 6.4 kg of 3-chloro-2-hydroxypropyltrimethylammonium chloride (mass ratio 1:0.8), react at 62℃ for 4.5 h, adjust the pH to 7.2 with 10% NaOH solution, filter and wash, and vacuum dry at 60℃ for 8 h to obtain 8 kg of quaternized modified chitosan;

[0091] S2.2: Preparation of microcapsules: Weigh 8 kg of modified chitosan and 2 kg of geraniol, add 80 L of deionized water, stir and emulsify at 8500 rpm for 32 min at 52 °C, add 0.4 kg of glutaraldehyde crosslinking agent (5% of the mass of modified chitosan), react at 42 °C for 2.2 h, cool, centrifuge at 8000 rpm for 15 min, wash 3 times, vacuum dry at 50 °C for 6 h to obtain 10 kg of modified chitosan microcapsules for later use;

[0092] S3: Preparation of fermentation extract:

[0093] S3.1: Take 1.5 kg of bergamot peel, 1 kg of ylang-ylang flowers, 0.5 kg of cassia leaves, and 1 kg of lily of the valley flowers, grind them to 45 mesh, and mix them to obtain 4 kg of mixed raw materials;

[0094] S3.2: Mix 4 kg of the mixed raw material with 20 L of deionized water, and add 0.12 kg of activated water to a concentration of 1 × 10⁻⁶.8 Inoculate with 3% CFU / mL of Saccharomyces cerevisiae (pH adjusted to 5.2) and ferment at 29°C for 52 hours, stirring for 10 minutes every 8 hours.

[0095] S3.3: Filter the fermentation broth, take the filter residue, add 60L of 72% ethanol solution (solid-liquid ratio 1:15), reflux at 81℃ for 2.2h, filter, and recover the ethanol by vacuum distillation to obtain 4kg of fermentation extract for later use.

[0096] S4: Weigh 9kg PLGA, 3kg CMC-Na, 2kg Vitamin E, 1kg Triethyl Citrate, and 65L Deionized Water, and stir at 380rpm for 1.2h at 36℃ to obtain a mixed matrix solution;

[0097] S5: Add 10 kg of modified chitosan microcapsules, sonicate at 320 W for 18 min to obtain microcapsule dispersion;

[0098] S6: Add 6kg of compound essential oil and 4kg of fermented extract, stir at 420rpm for 35min at 31℃ until well mixed;

[0099] S7: Cool to room temperature, stand for 15 hours, filter through a 0.22μm filter membrane to obtain a long-lasting fragrance perfume.

[0100] Comparative Example 1

[0101] A perfume, the mass fractions of its components are as follows:

[0102] 8 parts of compound essential oil

[0103] 15 portions of polymeric sustained-release carrier

[0104] stabilizer 4 parts

[0105] 5 parts of fermentation extract

[0106] 68 parts of deionized water

[0107] The preparation method is the same as in Example 1, except that steps S2 (preparation of modified chitosan microcapsules) and S5 (dispersion of microcapsules) are omitted.

[0108] Comparative Example 2

[0109] A perfume, the mass fractions of its components are as follows:

[0110] 8 parts of compound essential oil

[0111] 12 portions of modified chitosan microcapsules

[0112] stabilizer 4 parts

[0113] 5 parts of fermentation extract

[0114] 71 parts deionized water

[0115] The preparation method is the same as in Example 1, except that step S4 does not include the polymeric sustained-release carrier (PLGA and CMC-Na).

[0116] Comparative Example 3

[0117] A perfume, with the same mass fractions of each component as in Example 1, except that the preparation method of the fermentation extract is changed: the mixed raw materials obtained after step S3.1 are directly extracted by reflux with 75% ethanol without fermentation with brewer's yeast, and the remaining preparation steps are the same as in Example 1.

[0118] Comparative Example 4

[0119] A perfume, with the same mass percentages of each component as in Example 1, except that the chitosan was not quaternized, and the remaining preparation steps were the same as in Example 1.

[0120] Comparative Example 5

[0121] A perfume, the mass fractions of its components are as follows:

[0122] 8 parts of compound essential oil

[0123] 12 portions of modified chitosan microcapsules

[0124] 15 portions of polymeric sustained-release carrier

[0125] stabilizer 4 parts

[0126] Three portions of fermented extracts (1 portion of ylang-ylang, 1 portion of cassia, and 1 portion of lily of the valley).

[0127] 58 portions of deionized water

[0128] The preparation method is the same as in Example 1.

[0129] Comparative Example 6

[0130] A perfume, the mass fractions of its components are as follows:

[0131] 8 parts of compound essential oil

[0132] 12 portions of modified chitosan microcapsules

[0133] 15 portions of polymeric sustained-release carrier

[0134] stabilizer 4 parts

[0135] 5 parts of fermentation extract

[0136] 5 parts alcohol

[0137] 51 parts deionized water

[0138] The preparation method is the same as in Example 1.

[0139] Comparative Example 7

[0140] A perfume, with the same mass fractions of each component as in Example 1, except that the preparation method of the compound essential oil is changed to: using steam distillation at a temperature of 100°C for 5 hours, and the remaining preparation steps are the same as in Example 1.

[0141] Comparative Example 8

[0142] A perfume, with the same mass percentages of each component as in Example 1, except that citral (a volatile precursor fragrance) was not added in the preparation of the modified chitosan microcapsules, and the rest of the preparation steps were the same as in Example 1.

[0143] Performance testing

[0144] Detection methods

[0145] Scent retention time test: Ten perfumers (5 males and 5 females, aged 25-45) were selected. The perfumes of each example and comparative example were evenly applied to the evaluation paper (area 2cm×5cm) with an application amount of 0.2mL. The paper was placed in an environment with a temperature of 25℃ and a relative humidity of 50%. The fragrance intensity was scored at 1h, 4h, 8h, 12h, 24h, 30h, 36h, and 48h (0 points: no fragrance; 1 point: faint fragrance, can only be smelled at close range; 2 points: slight fragrance, can be smelled at normal distance; 3 points: obvious fragrance; 4 points: strong fragrance). The duration of fragrance intensity ≥1 point was recorded as the scent retention time, and the average value of the 10 perfumers was taken.

[0146] Mildness test: Thirty volunteers (15 males and 15 females, aged 18-50 years, without skin diseases) were selected. 0.1 mL of perfume was applied to the inner forearm of each volunteer, covering an area of ​​3cm × 3cm. The area was covered and fixed with gauze. The application was removed after 24 hours. Skin reactions were observed at 1 hour, 24 hours, and 48 hours after removal and scored according to the following criteria: 0 points: no reaction; 1 point: mild erythema; 2 points: obvious erythema and mild edema; 3 points: severe erythema, edema, and papules; 4 points: erythema, edema, papules, and vesicles. The average score of the 30 volunteers was taken.

[0147] System stability testing: Accelerated stability test: Each perfume sample was sealed and placed in a 45℃ constant temperature chamber for 3 months. The samples were observed to see if there were any phenomena such as layering, discoloration, or precipitation. At the same time, the fragrance retention time before and after the placement was measured, and the change rate of fragrance retention time was calculated (change rate = (fragrance retention time before placement - fragrance retention time after placement) / fragrance retention time before placement × 100%).

[0148] Evaporation rate test: Weighing method: Take 20mL of perfume sample and place it in a dry and clean weighing bottle, weigh it accurately (m1), place it in an environment with a temperature of 25℃ and a relative humidity of 50% for 24h, and weigh it accurately again (m2). Evaporation rate = (m1-m2) / m1×100%, and take the average value of 3 parallel tests.

[0149] The performance test data of each embodiment and comparative example are shown in Table 1 below.

[0150] Table 1 Summary of performance test data for examples and comparative examples

[0151] Sample number Scent lasting time (h) Mildness rating (points) Stability (after 3 months) Persistence time change rate (%) Evaporation rate (% / 24h) Example 1 36.2 0.0 No layering, no color change 2.8 4.6 Example 2 38.5 0.0 No layering, no color change 2.3 4.2 Example 3 34.8 0.0 No layering, no color change 3.2 4.9 Comparative Example 1 11.8 0.0 No layering, no color change 4.9 17.8 Comparative Example 2 9.6 0.0 No layering, no color change 5.8 19.5 Comparative Example 3 18.3 0.0 Slight layering, no discoloration 11.5 11.7 Comparative Example 4 22.5 0.0 No layering, slight discoloration 8.7 9.2 Comparative Example 5 25.7 0.0 No layering, no color change 6.3 7.8 Comparative Example 6 20.4 2.1 No layering, no color change 3.5 7.5 Comparative Example 7 28.6 0.0 No layering, no color change 4.2 6.8 Comparative Example 8 23.1 0.0 No layering, no color change 7.9 8.9

[0152] The above description is merely a preferred embodiment of the present invention and is not intended to limit the present invention in any way. Although the present invention has been disclosed above with reference to preferred embodiments, it is not intended to limit the present invention. Any person skilled in the art can make some modifications or alterations to the above-disclosed technical content to create equivalent embodiments without departing from the scope of the present invention. Any simple modifications, equivalent changes and alterations made to the above embodiments based on the technical essence of the present invention without departing from the scope of the present invention shall still fall within the scope of the present invention.

Claims

1. A long-lasting fragrance, characterized in that, It is composed of the following components in parts by weight: 5-15 parts of compound essential oil, 8-20 parts of modified chitosan microcapsules, 10-25 parts of polymeric sustained-release carrier, 2-8 parts of stabilizer, 3-10 parts of fermentation extract, and deionized water to make up to 100 parts. The raw materials of the compound essential oil include rose petals, jasmine petals, lavender, and lemon peel, and the mass ratio of the four is (3-5):(2-4):(1-3):(1-2); The compound essential oil was prepared by supercritical CO2 extraction. The process parameters for supercritical CO2 extraction are: extraction pressure 35-45 MPa, extraction temperature 38-45℃, CO2 flow rate 15-25 L / h, and extraction time 2-4 h. The modified chitosan microcapsules are made of quaternized modified chitosan loaded with volatile precursor fragrances, with a particle size of 50-200 nm. The preparation of the modified chitosan microcapsules includes: mixing quaternized modified chitosan with volatile precursor fragrance, adding deionized water, stirring and emulsifying at 8000-10000 rpm for 30-40 min at 50-60℃, adding 5-10% of glutaraldehyde crosslinking agent by weight of quaternized modified chitosan, reacting at 40-50℃ for 2-3 h, cooling, centrifuging, washing until neutral, and drying to obtain modified chitosan microcapsules; The preparation method of the quaternized modified chitosan is as follows: chitosan is dissolved in 1% acetic acid solution, 3-chloro-2-hydroxypropyltrimethylammonium chloride is added, the mass ratio of chitosan to 3-chloro-2-hydroxypropyltrimethylammonium chloride is 1:(0.8-1.2), the reaction is carried out at 60-70℃ for 4-6 hours, the pH is adjusted to 7-8, and the mixture is filtered, washed and dried to obtain quaternized modified chitosan; The volatile precursor fragrance is one or more of citral, citronellol, and geraniol, and the mass ratio of quaternized modified chitosan to volatile precursor fragrance is (3-5):

1. The fermented extract is obtained by mixing bergamot peel, ylang-ylang flower, cassia leaf and lily of the valley flower in a mass ratio of (1-3):(0.5-2):(0.5-2):(0.5-2), fermenting with brewer's yeast, and then extracting by ethanol reflux. The polymeric sustained-release carrier is a compound of polylactic acid-glycolic acid copolymer and sodium carboxymethyl cellulose in a mass ratio of (2-5):1; The preparation conditions for the fermented extract are as follows: the inoculation amount of brewer's yeast is 3-5% of the mass of the mixed raw materials, the fermentation temperature is 29-31℃, the fermentation time is 50-60h, and the fermentation pH is 5.0-6.0; the process parameters for ethanol reflux extraction are as follows: ethanol concentration is 70-80%, the material-liquid ratio is 1:15-20, the reflux temperature is 80-85℃, and the reflux time is 2-3h. The stabilizer is a mixture of vitamin E and triethyl citrate in a mass ratio of (1-2):

1.

2. The long-lasting fragrance according to claim 1, characterized in that, The polylactic acid-glycolic acid copolymer has a molecular weight of 5000-10000 Da and a degree of substitution of sodium carboxymethyl cellulose of 0.6-0.

8.

3. A method for preparing a long-lasting fragrance as described in any one of claims 1-2, characterized in that, Includes the following steps: S1: Weigh rose petals, jasmine petals, lavender, and lemon peel according to the mass ratio, crush them, and extract them by supercritical CO2 to obtain a compound essential oil; S2: Prepare quaternized modified chitosan, mix it with volatile precursor fragrance, and obtain modified chitosan microcapsules through emulsification, crosslinking, centrifugation and drying; S3: The bergamot peel, ylang-ylang flower, cassia leaf, and lily of the valley flower are mixed and crushed, fermented with brewer's yeast, and extracted by ethanol reflux to obtain the fermented extract; S4: Mix the polymer slow-release carrier, stabilizer and deionized water, heat and stir to dissolve to obtain a mixed matrix solution; S5: Add modified chitosan microcapsules to the mixed matrix solution and disperse by ultrasonication to obtain a microcapsule dispersion; S6: Add the compound essential oil and fermented extract to the microcapsule dispersion and stir to mix evenly; S7: Cool, let stand, and filter to obtain a long-lasting fragrance.