Liquid functional fragrance capable of relieving emotion, helping sleep and soothing nerves and preparation method of liquid functional fragrance
By preparing fragrances containing composite stabilizers and modified antioxidants, the problems of limited fragrance functionality and short duration are solved, thereby enhancing the effects of mood soothing and sleep aid, and providing a safe and natural solution.
Patent Information
- Application Number
- CN202511510872.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-10-22
- Publication Date
- 2025-11-28
AI Technical Summary
Existing fragrance products have limited functions in soothing emotions and aiding sleep. Traditional sleep aids are addictive and have side effects, and the fragrance effect is short-lived.
By using compound stabilizers and modified antioxidants, and combining plant essential oils and stabilizers in a specific ratio, a soothing, sleep-inducing, and calming liquid functional fragrance is prepared. It utilizes aromatherapy to regulate emotions and enhance the stability and sleep-inducing effect of the fragrance.
It effectively prolongs the stability of the fragrance and enhances its sleep-aiding effect. Through the application of compound stabilizers and modified antioxidants, it improves the stability and mood-regulating ability of the fragrance and promotes deep sleep.
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Figure CN121015779A_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of fragrance preparation technology, specifically relating to a soothing, sleep-aiding, and calming liquid functional fragrance and its preparation method. Background Technology
[0002] In today's fast-paced, high-pressure society, insomnia and anxiety are becoming increasingly prominent, posing a significant threat to public health. People are constantly in a state of tension, leading to poor sleep quality, which not only results in daytime fatigue and reduced work efficiency but can also trigger a series of physiological and physical illnesses. Traditional sleep aids often rely on medication, which, while providing quick relief, can lead to dependence and drug tolerance with long-term use, and may cause side effects, failing to address the root causes of emotional and sleep problems. Ordinary fragrance products primarily focus on creating a pleasant scent environment, offering limited and singular functions in soothing emotions and promoting sleep and calming the mind. Therefore, a liquid functional fragrance for mood soothing, sleep aiding, and calming the mind has emerged. It integrates modern aromatherapy with natural plant extract technology, carefully selecting plant ingredients with calming and relaxing effects, such as lavender and chamomile. These essential elements are incorporated into liquid fragrances, which, through the diffusion of fragrance molecules in the air, act on the human olfactory system, thereby affecting the limbic system of the brain, regulating emotions, relieving stress, helping people relax their mind and body, and enter a state of deep sleep more quickly. This provides a safe, natural, and effective solution for people who pursue healthy, high-quality sleep. Summary of the Invention
[0003] The purpose of this invention is to provide a soothing, sleep-aiding, and calming liquid functional fragrance and its preparation method, in order to solve the technical problem of the short duration of fragrance in the prior art.
[0004] To achieve the above objectives, the present invention adopts the following technical solution: This invention provides a soothing, sleep-aiding, and calming liquid fragrance, composed of the following ingredients by weight: 50-60 parts deionized water, 30-45 parts anhydrous ethanol, 2-4 parts Schisandra chinensis essential oil, 2-4 parts Acorus tatarinowii essential oil, 1-3 parts Neroli essential oil, 1-3 parts Chamomile essential oil, 1-2 parts Lily essential oil, 1-2 parts compound stabilizer, and 0.2-0.5 parts modified antioxidant.
[0005] Preferably, the preparation method of the composite stabilizer includes the following steps: Q1: Under nitrogen atmosphere, a mixed solution of ethoxyacetylene and hexane was added to a container, followed by the addition of tetrahydrofuran. After stirring and dissolving, the mixture was cooled, and a hexane solution containing n-butyllithium was added dropwise. After stirring and reacting, p-dimethylquinone was added, and the reaction was continued. After the reaction was completed, a saturated ammonium chloride solution was added to quench the reaction. The mixture was separated, extracted, washed, dried, concentrated, and purified to obtain product 1. Q2: Put product 1 and pyridine-N-oxide into a container containing dichloroethane, stir evenly, then add triphenylphosphine trifluorimide gold, stir the reaction at room temperature, after the reaction is completed, add sodium hydroxide aqueous solution to quench the reaction, separate the liquid, extract, add hydrochloric acid, precipitate, dissolve, extract, wash, dry, concentrate, purify, and obtain product 2; Q3: Put product 2 and 12-hydroxystearic acid into a container, then add cyclohexane and p-toluenesulfonic acid, heat and stir to reflux the reaction, after the reaction is completed, wash, dry, concentrate, and purify to obtain a composite stabilizer.
[0006] In the above process, the synthesis reaction formula of the composite stabilizer is as follows:
[0007] The mass spectrum analysis result of product 1 is as follows: m / z: 206.09 (100.0%), 207.10 (13.3%), 208.10 (1.4%); the mass spectrum analysis result of product 2 is as follows: m / z: 222.09 (100.0%), 223.09 (13.1%); and the mass spectrum analysis result of the composite stabilizer is as follows: m / z: 504.35 (100.0%), 505.35 (33.2%), 506.35 (6.6%).
[0008] As preferred, in Q1, the amount ratio of ethoxyacetylene, tetrahydrofuran, n-butyllithium and p-dimethylquinone is (1.23-1.68) g:(17.5-22.3) mL:(3.11-3.53) g:(0.88-1.24) g, the temperature is reduced to -78~-80℃, the reaction is stirred for 1-2h, and the reaction is continuously stirred for 3-5h.
[0009] As preferred, in Q2, the amount ratio of product 1, pyridine-N-oxide, dichloroethane and triphenylphosphine trifluorimide gold is (1.11-1.54) g:(0.84-1.05) g:(10-16) mL:(0.111-0.125) mg, the reaction is stirred at room temperature for 3-5h, the concentration of sodium hydroxide aqueous solution is 0.5mol / L, and the concentration of hydrochloric acid is 1mol / L.
[0010] As preferred, in Q3, the molar ratio of product 2 and 12-hydroxystearic acid is (0.9-1.1):(1.2-1.5), the temperature is heated to 100-120℃, the reaction is stirred to reflux for 4-12h.
[0011] As preferred, the preparation method of the modified antioxidant comprises the following steps: S1: under low temperature environment, N, N-dimethylformamide, phosphorus oxychloride and acetonitrile are added into a container, after stirring and mixing, resveratrol is added and stirred, after stirring, filtration, washing, adding to distilled water, heating hydrolysis, filtration, washing, drying, obtaining organic matter a; S2: under low temperature environment, organic matter a, tert-butyl dimethyl chlorosilane and tetrahydrofuran are added into a container in turn, stirring, adding imidazole-containing tetrahydrofuran solution, stirring, rotary evaporation, purification, obtaining organic matter b; S3: organic matter b is added into a container containing tetrahydrofuran, then sodium borohydride is added, low temperature stirring, adding distilled water and continuing stirring, then adding ammonium chloride aqueous solution and stirring, adding tetrahydrofuran for dilution, filtration, concentration, purification and separation, obtaining organic matter c; S4: under low temperature environment, chlorogenic acid, DCC, p-dimethylaminopyridine and dichloromethane are mixed and stirred, then dichloromethane containing organic matter c is added, after low temperature stirring, room temperature stirring, washing, drying, filtration, concentration, purification, obtaining organic matter d; organic matter d is added into a container containing tetrahydrofuran, then trifluoroacetic acid is added, under nitrogen protection, low temperature stirring reaction, after reaction, concentration, purification, obtaining modified antioxidant.
[0012] In the above process, the synthesis reaction formula of the modified antioxidant is:
[0013] The mass spectrometry analysis results of the organic matter a are: m / z: 256.07 (100.0%), 257.08 (16.5%), 258.08 (2.1%); the mass spectrometry analysis results of the organic matter b are: m / z: 598.33 (100.0%), 599.34 (36.5%), 599.33 (15.2%), 600.34 (12.8%), 600.33 (10.8%), 601.33 (4.6%), 601.34 (2.5%); the mass spectrometry analysis results of the organic matter c are: m / z: 600.35 (100.0%), 601.35 (51.7%), 602.35 (17.2%), 602.36 (6.5%), 603.35 (6.0%), 604.35 (1.1%), 603.36 (1.1%); the mass spectrometry analysis results of the organic matter d are: m / z: 936.43 (100.0%), 937.44 (54.3%), 938.44 (25.2%), 937.43 (15.2%), 938.43 (10.8%), 939.44 (6.8%), 939.43 (6.4%), 940.44 (2.5%), 940.43 (1.2%); the mass spectrometry analysis results of the modified antioxidant are: m / z: 594.17 (100.0%), 595.18 (34.3%), 596.18 (8.2%), 597.18 (1.4%).
[0014] Preferably, in the S1, the low-temperature environment temperature is -3~ -6℃, the dosage ratio of N,N-dimethylformamide, phosphorus oxychloride, acetonitrile and white wine is (0.12-0.16) g: (0.28-0.37) g: (55-65) mL: (0.448-0.472) g, the stirring mixing time is 20-30 min, the stirring time is continued for 3-5 h, the hydrolysis temperature is 50-60℃, and the time is 3-4 h; in the S2, the low-temperature environment temperature is 0-1℃, the dosage ratio of the organic matter a, tert-butyl dimethyl chlorosilane and imidazole is (0.247-0.263) g: (1.423-1.521) g: (0.61-0.73) g, and the stirring time is 10-12 h.
[0015] As preferred, in the S3, the amount ratio of the organic matter b, sodium borohydride, distilled water and the aqueous solution of ammonium chloride is (0.112-0.214) g:(0.0071-0.0083) g:(0.1-0.15) mL:(0.28-0.32) mL, the concentration of the aqueous solution of ammonium chloride is 0.18 g / mL, the low-temperature stirring temperature is 0-1 DEG C, the time is 20-25 min, the continuous stirring time is 5-8 min, and the aqueous solution of ammonium chloride is stirred for 20-30 min.
[0016] As preferred, in the S4, the low-temperature environment temperature is 0-1 DEG C, the amount ratio of the chlorogenic acid, DCC, p-dimethylaminopyridine and the organic matter c is (0.342-0.358) g:(0.212-0.246) g:(0.011-0.013) g:(0.581-0.622) g, the mixing and stirring time is 10-20 min, the low-temperature stirring temperature is 0-1 DEG C, the time is 10-15 min, the room-temperature stirring time is 15-20 h, the amount ratio of the organic matter d, tetrahydrofuran and trifluoroacetic acid is (0.191-0.205) g:(3-5) mL:(0.45-0.55) mL, and the low-temperature stirring reaction temperature is 0-1 DEG C, and the time is 5-7 h.
[0017] As preferred, the preparation method of the mood relieving, sleep aiding and tranquilizing liquid functional fragrance comprises the following steps: Step one: deionized water is added into a reaction kettle, then a composite stabilizer is added, after stirring and mixing, a modified antioxidant is added, and stirring is performed until uniform dispersion is achieved, so as to obtain an aqueous phase; Step two: five kinds of essential oils, i.e., schisandra essential oil, acorus essential oil, orange flower essential oil, chamomile essential oil and lily flower essential oil, are mixed, then anhydrous ethanol is added, and after ultrasonic mixing, an oil phase is obtained; Step three: the oil phase is slowly added into the aqueous phase, mixing is performed, high-pressure homogenization treatment is performed, aging is performed, and filtering is performed, so as to obtain the mood relieving, sleep aiding and tranquilizing liquid functional fragrance.
[0018] As described above, due to the adoption of the above technical solutions, the mood relieving, sleep aiding and tranquilizing liquid functional fragrance has the following advantages: 1. The composite stabilizer and the modified antioxidant prepared in the present application are applied to the fragrance, so that the stability of the fragrance can be effectively improved, the sleep aiding effect can be enhanced, and the mood pressure can be adjusted.
[0019] 2. The obtained composite stabilizer is applied to the fragrance, which can effectively prolong the stability of the fragrance and enhance the sleep aid effect, regulate emotional stress, the structure of 12-hydroxystearate can form a steric hindrance effect, prevent volatile components in the fragrance from contacting oxygen, reduce the generation of free radicals, the introduced alkyl chain can enhance the intermolecular van der Waals force, improve the stability of the fragrance base oil, prevent component degradation caused by phase separation, the cycloheptatrienone structure contained has molecular recognition and inclusion ability for organic molecules, part of the structure of the fragrance molecule is combined with the surface of the cycloheptatrienone through pi-pi interaction and van der Waals force, and is surrounded by a hydrophobic environment formed by a long-chain alkyl group, which significantly reduces the volatility of the fragrance molecule and the contact opportunity with oxygen / light, prolongs the stability, so that the continuous stable nerve input can be that the fragrance molecule penetrates into the brain edge through the olfactory epithelium, and the concentration of the signal molecule of the system is maintained at an effective and stable video for a longer time, thereby enhancing the sleep aid effect.
[0020] 3. The prepared modified antioxidant is applied to the fragrance, which can effectively prolong the stability of the fragrance and enhance the sleep aid effect, the hydroxyl structure contained in resveratrol and chlorogenic acid can neutralize free radicals by providing hydrogen atoms or electrons, directly inhibit the oxidation chain reaction, and the esterification structure contained can also reduce the intermolecular oxidation contact through steric hindrance effect, thereby improving the stability performance; resveratrol, as a gamma-aminobutyric acid receptor agonist, can bind to the receptor benzodiazepine site, promote the opening of the chloride ion channel, inhibit the excitability of neurons, produce a sedative sleep aid effect, and chlorogenic acid can inhibit the activity of monoamine oxidase, reduce the degradation of 5-hydroxytryptamine and dopamine, increase the level thereof, and enhance the sleep aid effect. BRIEF DESCRIPTION OF DRAWINGS
[0021] In order to more clearly illustrate the technical solutions in the embodiments of the present application or the prior art, the drawings needed in the embodiments or the prior art description will be briefly introduced below. Obviously, the drawings in the following description are only some embodiments of the present application, and other drawings can also be obtained by those skilled in the art without creative labor.
[0022] Figure 1 is the antibacterial effect column chart of the sample prepared according to example 1; Figure 2 is the PC12 cell oxidative damage protection activity chart of the sample prepared according to example 1; Figure 3 is the antioxidant performance column chart of the sample prepared according to example 1. DETAILED DESCRIPTION
[0023] With reference to the accompanying drawings, the technical solutions in the embodiments of the present application will be clearly and completely described below. Obviously, the described embodiments are only a part of the embodiments of the present application, rather than all the embodiments of the present application. Based on the embodiments in the present application, all other embodiments obtained by those of ordinary skill in the art without creative work fall within the scope of the present application.
[0024] Embodiment 1: The present embodiment discloses a preparation method of a composite stabilizer, comprising the following steps: Q1: A mixed solution of 1.45g ethoxyacetylene and 3mL hexane is added to a container under a nitrogen environment, then 19.9mL tetrahydrofuran is added, after stirring and dissolving, the temperature is lowered to-78℃, 8mL of a hexane solution containing 3.32g n-butyllithium is added dropwise, after stirring for 2h, 1.01g p-dimethylquinone is added, and the stirring reaction is continued for 5h, after the reaction is completed, saturated ammonium chloride solution is added to quench the reaction, the liquid is separated, the organic phase is extracted, washed and dried, concentrated, purified, and the product 1 is obtained; Q2: 1.32g of product 1 and 0.94g of pyridine-N-oxide are added to a container containing 13mL dichloroethane, after stirring uniformly, 0.118mg of triphenylphosphine trifluoride imine gold is added, and the stirring reaction is carried out at room temperature for 5h, after the reaction is completed, 5mL of 0.5mol / L sodium hydroxide aqueous solution is added to quench the reaction, the liquid is separated, extracted, 5mL of 1mol / L hydrochloric acid is added, precipitated, dissolved, extracted, washed, dried, concentrated, and purified to obtain product 2; Q3: 0.735g of product 2 and 1.352g of 12-hydroxystearic acid are added to a container, then 2.42g of cyclohexane and 0.02g of p-toluenesulfonic acid are added, heated to 120℃ and stirred to reflux for 8h, after the reaction is completed, washed, dried, concentrated, and purified to obtain the composite stabilizer.
[0025] The present embodiment discloses a preparation method of a modified antioxidant, comprising the following steps: S1: 0.14g of N,N-dimethylformamide, 0.32g of phosphorus oxychloride and 60mL of acetonitrile are added to a container at-6℃, after stirring and mixing for 30min, 0.461g of white hederin is added and stirred for 5h, after the stirring is completed, filtered, washed, added to distilled water, heated to hydrolyze at 55℃ for 4h, filtered, washed, dried, and the organic matter a is obtained; S2: 0.255g of organic matter a, 1.482g of tert-butyl dimethylchlorosilane and 5mL of tetrahydrofuran are sequentially added to a container at 0℃, stirred, 4mL of a tetrahydrofuran solution containing 0.68g of imidazole is added, stirred for 12h, rotary evaporated, and purified to obtain the organic matter b; S3: 0.163g of organic matter b was added to a container containing 5mL of tetrahydrofuran, followed by 0.0076g of sodium borohydride, stirring at 0℃ for 25min, adding 0.12mL of distilled water and continuing to stir for 8min, then adding 0.3mL of 0.18g / mL ammonium chloride aqueous solution and stirring for 20min, adding tetrahydrofuran for dilution, filtering, concentrating, purifying and separating to obtain organic matter c; S4: 0.348g of chlorogenic acid, 0.234g of DCC, 0.012g of p-dimethylaminopyridine and 10mL of dichloromethane were mixed and stirred at 0℃ for 20min, then 5mL of dichloromethane containing 0.602g of organic matter c was added, stirred at 0℃ for 15min, then stirred at room temperature for 18h, washed, dried, filtered, concentrated and purified to obtain organic matter d; 0.198g of organic matter d was added to a container containing 4mL of tetrahydrofuran, followed by 0.5mL of trifluoroacetic acid, and stirred at 0℃ for 6h under nitrogen protection. After the reaction was completed, it was concentrated and purified to obtain a modified antioxidant.
[0026] The embodiment discloses a mood-relieving sleep-aiding and nerve-calming liquid functional fragrance, which is composed of the following components in parts by weight: 55 parts of deionized water, 37.5 parts of anhydrous ethanol, 3 parts of Schisandra chinensis essential oil, 3 parts of Acorus gramineus essential oil, 2 parts of orange flower essential oil, 2 parts of chamomile essential oil, 1.5 parts of lily flower essential oil, 1.5 parts of a composite stabilizer and 0.35 parts of a modified antioxidant.
[0027] The embodiment discloses a preparation method of a mood-relieving sleep-aiding and nerve-calming liquid functional fragrance, which comprises the following steps: Step one: deionized water was added to a reaction kettle, followed by the addition of a composite stabilizer, and then a modified antioxidant was added after stirring and mixing to obtain an aqueous phase; Step two: Schisandra chinensis essential oil, Acorus gramineus essential oil, orange flower essential oil, chamomile essential oil and lily flower essential oil were mixed, and then anhydrous ethanol was added, and after ultrasonic mixing, an oil phase was obtained; Step three: the oil phase was slowly added to the aqueous phase, mixed, high-pressure homogenized, aged, filtered, and a mood-relieving sleep-aiding and nerve-calming liquid functional fragrance was obtained.
[0028] Embodiment 2: The embodiment discloses a preparation method of a composite stabilizer, which comprises the following steps: Q1: A mixture solution of 1.23g of ethoxyacetylene and 3mL of hexane was added to a container, followed by the addition of 17.5mL of tetrahydrofuran, and after stirring and dissolving, the temperature was lowered to-78℃, 8mL of a hexane solution containing 3.11g of n-butyllithium was added dropwise, and after stirring for 2h, 0.88g of p-dimethylquinone was added, and the stirring was continued for 5h. After the reaction was completed, saturated ammonium chloride solution was added to quench the reaction, and then the mixture was separated, extracted, the organic phase was washed and dried, concentrated, and purified to obtain product 1. Q2: 1.11 g of product 1 and 0.84 g of pyridine-N-oxide were added to a container containing 10 mL of dichloroethane, stirred uniformly, then 0.111 mg of triphenylphosphine trifluorimide gold was added, stirred at room temperature for 5 h, after the reaction was completed, 5 mL of 0.5 mol / L sodium hydroxide aqueous solution was added to quench the reaction, separated, extracted, 5 mL of 1 mol / L hydrochloric acid was added, precipitated, dissolved, extracted, washed, dried, concentrated, purified to obtain product 2; Q3: 0.666 g of product 2 and 1.201 g of 12-hydroxystearic acid were added to a container, then 2.42 g of cyclohexane and 0.02 g of p-toluenesulfonic acid were added, heated to 120°C and stirred to reflux for 8 h, after the reaction was completed, washed, dried, concentrated, purified to obtain a composite stabilizer.
[0029] The embodiment discloses a preparation method of a modified antioxidant, comprising the following steps: S1: 0.12 g of N,N-dimethylformamide, 0.28 g of phosphorus oxychloride and 55 mL of acetonitrile were added to a container at -6°C, stirred and mixed for 30 min, then 0.448 g of white pigweed alcohol was added and stirred for 5 h, after stirring was completed, filtration, washing, adding to distilled water, heating hydrolysis at 55°C for 4 h, filtration, washing, drying to obtain organic matter a; S2: 0.247 g of organic matter a, 1.423 g of tert-butyl dimethyl chlorosilane and 5 mL of tetrahydrofuran were sequentially added to a container at 0°C, stirring, adding 4 mL of tetrahydrofuran containing 0.61 g of imidazole, stirring for 12 h, rotary evaporation, purification to obtain organic matter b; S3: 0.112 g of organic matter b was added to a container containing 5 mL of tetrahydrofuran, then 0.0071 g of sodium borohydride was added, stirred at 0°C for 25 min, 0.1 mL of distilled water was added and stirred for 8 min, then 0.28 mL of 0.18 g / mL ammonium chloride aqueous solution was added and stirred for 20 min, tetrahydrofuran was added for dilution, filtration, concentration, purification and separation to obtain organic matter c; S4: 0.342 g of chlorogenic acid, 0.212 g of DCC, 0.011 g of p-dimethylaminopyridine and 10 mL of dichloromethane were mixed and stirred at 0°C for 20 min, then 5 mL of dichloromethane containing 0.581 g of organic matter c was added, stirred at 0°C for 15 min, then stirred at room temperature for 18 h, washed, dried, filtered, concentrated, purified to obtain organic matter d; 0.191 g of organic matter d was added to a container containing 3 mL of tetrahydrofuran, then 0.55 mL of trifluoroacetic acid was added, stirred at 0°C for 6 h under nitrogen protection, after the reaction was completed, concentrated, purified to obtain a modified antioxidant.
[0030] The embodiment discloses a mood-relieving sleep-aiding tranquilizing liquid functional fragrance, which is composed of the following components in parts by weight: 50 parts of deionized water, 30 parts of anhydrous ethanol, 2 parts of Schisandra chinensis essential oil, 2 parts of Acorus gramineus essential oil, 1 part of orange flower essential oil, 1 part of chamomile essential oil, 1 part of lily flower essential oil, 1 part of a composite stabilizer and 0.2 parts of a modified antioxidant.
[0031] The embodiment discloses a preparation method of a mood-relieving sleep-aiding tranquilizing liquid functional fragrance, which comprises the following steps: Step one: deionized water is added into a reaction kettle, then a composite stabilizer is added, after stirring and mixing, a modified antioxidant is added, stirring is conducted until uniform dispersion is achieved, and a water phase is obtained; Step two: Schisandra chinensis essential oil, Acorus gramineus essential oil, orange flower essential oil, chamomile essential oil and lily flower essential oil are mixed, then anhydrous ethanol is added, ultrasonic mixing is conducted, and an oil phase is obtained; Step three: the oil phase is slowly added into the water phase, mixing is conducted, high-pressure homogenization treatment is conducted, aging is conducted, filtration is conducted, and the mood-relieving sleep-aiding tranquilizing liquid functional fragrance is obtained.
[0032] The embodiment discloses a preparation method of a composite stabilizer, which comprises the following steps: Q1: a mixed solution of 1.68g ethoxyacetylene and 3mL hexane is added into a container under a nitrogen environment, then 22.3mL tetrahydrofuran is added, after stirring and dissolving, the temperature is lowered to-78℃, 8mL of a hexane solution containing 3.53g n-butyllithium is added dropwise, stirring is conducted for 2h, then 1.24g p-dimethylquinone is added, stirring is continuously conducted for 5h, after the reaction is completed, a saturated ammonium chloride solution is added to quench the reaction, liquid separation is conducted, extraction is conducted, the organic phase is washed, drying is conducted, concentration is conducted, purification is conducted, and product 1 is obtained; Q2: 1.54g product 1 and 1.05g pyridine-N-oxide are added into a container containing 16mL dichloroethane, after stirring and uniform mixing, 0.125mg triphenylphosphine trifluoride imidate gold is added, stirring is conducted at room temperature for 5h, after the reaction is completed, 5mL of a 0.5mol / L sodium hydroxide aqueous solution is added to quench the reaction, liquid separation is conducted, extraction is conducted, 5mL of 1mol / L hydrochloric acid is added, precipitation is conducted, dissolution is conducted, extraction is conducted, washing is conducted, drying is conducted, concentration is conducted, and purification is conducted, and product 2 is obtained; Q3: 0.814g product 2 and 1.502g 12-hydroxystearic acid are added into a container, then 2.42g cyclohexane and 0.02g p-toluenesulfonic acid are added, heating is conducted to 120℃, stirring is conducted to reflux for 8h, after the reaction is completed, washing is conducted, drying is conducted, concentration is conducted, and purification is conducted, and the composite stabilizer is obtained.
[0033] The embodiment discloses a preparation method of a modified antioxidant, which comprises the following steps: S1: 0.16 g of N,N-dimethylformamide, 0.37 g of phosphorus oxychloride and 65 mL of acetonitrile were added into a container at -6°C, after stirring the mixture for 30 min, 0.472 g of Ziyuol was added and stirred for 5 h, after stirring, it was filtered, washed, added into distilled water, hydrolyzed at 55°C for 4 h, filtered, washed, dried, and the organic matter a was obtained; S2: 0.263 g of organic matter a, 1.521 g of tert-butyl dimethyl chlorosilane and 5 mL of tetrahydrofuran were sequentially added into a container at 0°C, stirred, 4 mL of tetrahydrofuran solution containing 0.73 g of imidazole was added, stirred for 12 h, rotary evaporated, and purified to obtain organic matter b; S3: 0.214 g of organic matter b was added into a container containing 5 mL of tetrahydrofuran, then 0.0083 g of sodium borohydride was added, stirred at 0°C for 25 min, 0.15 mL of distilled water was added and stirred for 8 min, then 0.32 mL of 0.18 g / mL of ammonium chloride aqueous solution was added and stirred for 20 min, diluted with tetrahydrofuran, filtered, concentrated, purified and separated to obtain organic matter c; S4: 0.358 g of chlorogenic acid, 0.246 g of DCC, 0.013 g of p-dimethylaminopyridine and 10 mL of dichloromethane were mixed and stirred at 0°C for 20 min, then 5 mL of dichloromethane containing 0.622 g of organic matter c was added, stirred at 0°C for 15 min, then stirred at room temperature for 18 h, washed, dried, filtered, concentrated, purified to obtain organic matter d; 0.205 g of organic matter d was added into a container containing 5 mL of tetrahydrofuran, then 0.45 mL of trifluoroacetic acid was added, stirred at 0°C for 6 h under nitrogen protection, after the reaction was completed, concentrated, purified to obtain the modified antioxidant.
[0034] The embodiment discloses a mood-relieving sleep-aiding and tranquilizing liquid functional fragrance, which is composed of the following components in parts by weight: 60 parts of deionized water, 45 parts of anhydrous ethanol, 4 parts of Schisandra chinensis essential oil, 4 parts of Acorus gramineus essential oil, 3 parts of orange flower essential oil, 3 parts of chamomile essential oil, 2 parts of lily flower essential oil, 2 parts of a composite stabilizer and 0.5 part of a modified antioxidant.
[0035] The embodiment discloses a preparation method of a mood-relieving sleep-aiding and tranquilizing liquid functional fragrance, which comprises the following steps: Step one: deionized water was added into a reaction kettle, then a composite stabilizer was added, after stirring and mixing, a modified antioxidant was added, and stirring was performed until uniform dispersion was achieved, to obtain an aqueous phase; Step two: Schisandra chinensis essential oil, Acorus gramineus essential oil, orange flower essential oil, chamomile essential oil and lily flower essential oil were mixed, then anhydrous ethanol was added, after ultrasonic mixing, an oil phase was obtained; Step three: slowly add the oil phase into the water phase, mix, high pressure homogenization treatment, aging, filter, get the mood soothing sleep and tranquilizing liquid functional fragrance.
[0036] Example 4: The present embodiment discloses a preparation method of a composite stabilizer, comprising the following steps: Q1: under nitrogen environment, add a mixed solution of 1.37g ethoxyacetylene and 3mL hexane into a container, then add 18.5mL tetrahydrofuran, after stirring and dissolving, cool to-78℃, drop 8mL n-butyllithium solution containing 3.21g n-butyllithium, after stirring for 2h, add 0.96g p-dimethylquinone, continue to stir for 5h, after the reaction is completed, add saturated ammonium chloride solution to quench the reaction, separate, extract, wash the organic phase, dry, concentrate, purify to obtain product 1; Q2: add 1.26g product 1 and 0.92g pyridine-N-oxide into a container containing 12mL dichloroethane, after stirring uniformly, add 0.116mg triphenylphosphine trifluorimide gold, stir at room temperature for 5h, after the reaction is completed, add 5mL 0.5mol / L sodium hydroxide aqueous solution to quench the reaction, separate, extract, add 5mL 1mol / L hydrochloric acid, precipitate, dissolve, extract, wash, dry, concentrate, purify to obtain product 2; Q3: add 0.692g product 2 and 1.257g 12-hydroxystearic acid into a container, then add 2.42g cyclohexane and 0.02g p-toluenesulfonic acid, heat to 120℃ and stir to reflux for 8h, after the reaction is completed, wash, dry, concentrate, purify to obtain the composite stabilizer.
[0037] The present embodiment discloses a preparation method of a modified antioxidant, comprising the following steps: S1: under-6℃, add 0.13g N,N-dimethylformamide, 0.31g phosphorus oxychloride and 62mL acetonitrile into a container, after stirring and mixing for 30min, add 0.453g white vitex alcohol and continue to stir for 5h, after the stirring is completed, filter, wash, add into distilled water, heat to hydrolyze at 55℃ for 4h, filter, wash, dry to obtain organic matter a; S2: under 0℃, add 0.251g organic matter a, 1.452g tert-butyl dimethylchlorosilane and 5mL tetrahydrofuran into a container in sequence, stir, add 4mL imidazole solution containing 0.64g imidazole in tetrahydrofuran, stir for 12h, rotary evaporation, purify to obtain organic matter b; S3: 0.138 g of organic matter b was added to a container containing 5 mL of tetrahydrofuran, followed by 0.0073 g of sodium borohydride, stirring at 0°C for 25 min, adding 0.11 mL of distilled water and continuing to stir for 8 min, then adding 0.29 mL of 0.18 g / mL concentration of ammonium chloride aqueous solution and stirring for 20 min, adding tetrahydrofuran for dilution, filtering, concentrating, purifying and separating to obtain organic matter c; S4: 0.345 g of chlorogenic acid, 0.221 g of DCC, 0.011 g of p-dimethylaminopyridine and 10 mL of dichloromethane were mixed and stirred at 0°C for 20 min, then 5 mL of dichloromethane containing 0.593 g of organic matter c was added, stirred at 0°C for 15 min, then stirred at room temperature for 18 h, washed, dried, filtered, concentrated and purified to obtain organic matter d; 0.196 g of organic matter d was added to a container containing 3.5 mL of tetrahydrofuran, followed by 0.48 mL of trifluoroacetic acid, and the reaction was stirred at 0°C for 6 h under nitrogen protection. After the reaction was completed, it was concentrated and purified to obtain a modified antioxidant.
[0038] The embodiment discloses a mood-relieving sleep-aiding and tranquilizing liquid functional fragrance, which is composed of the following components in parts by weight: 52 parts of deionized water, 32 parts of anhydrous ethanol, 2.5 parts of Schisandra chinensis essential oil, 2.5 parts of Acorus gramineus essential oil, 1.5 parts of orange flower essential oil, 1.8 parts of chamomile essential oil, 1.8 parts of lily flower essential oil, 1.2 parts of a composite stabilizer and 0.3 parts of a modified antioxidant.
[0039] The embodiment discloses a preparation method of a mood-relieving sleep-aiding and tranquilizing liquid functional fragrance, which comprises the following steps: Step one: deionized water was added to a reaction kettle, followed by the addition of a composite stabilizer, and then a modified antioxidant was added after stirring and mixing, and stirring was performed until uniform dispersion was achieved to obtain an aqueous phase; Step two: Schisandra chinensis essential oil, Acorus gramineus essential oil, orange flower essential oil, chamomile essential oil and lily flower essential oil were mixed, and then anhydrous ethanol was added, and ultrasonic mixing was performed to obtain an oil phase; Step three: the oil phase was slowly added to the aqueous phase, mixed, subjected to high-pressure homogenization treatment, aged, filtered and then a mood-relieving sleep-aiding and tranquilizing liquid functional fragrance was obtained.
[0040] Comparative Example 1: Comparative Example 1 is compared with Example 1. In the preparation process of the mood-relieving sleep-aiding and tranquilizing liquid functional fragrance, no composite stabilizer is added, and other conditions remain unchanged.
[0041] Comparative Example 2: Comparative Example 2 is compared with Example 1. In the preparation process of the mood-relieving sleep-aiding and tranquilizing liquid functional fragrance, no modified antioxidant is added, and other conditions remain unchanged.
[0042] Performance test: I. Cell test Mouse L929 fibroblasts were inoculated into a 96-well plate, 37°C, 5% CO2, and cultured for 24 h to adhere to the wall, then the fragrance diluent prepared according to Example 1 was added, the fragrance diluent concentration was 0.1%, 1%, 5%, and incubated for 24-72 h, and the cell culture solution was set as a control group, 10 μL of CCK-8 reagent was added to each well, and incubated for 2-4 h, then the absorbance at 450 nm was measured by a microplate reader, and the cell survival rate was calculated, and the test results are shown in Table 1: Table 1
[0043] According to the above data, it can be found that the prepared fragrance is non-toxic.
[0044] II. Human patch test The fragrance diluent (1%) prepared according to Example 1 was dropped into 4 layers of gauze, and was attached to the healthy skin on the inner side of the forearm of the test subject (age 20-50 years old, no history of skin disease, no history of allergy, no use of antihistamines or glucocorticoids in the recent period), with a spacing of ≥4 cm, covered with transparent glass paper and fixed with a non-allergic tape, during the test period, avoid strenuous exercise, sweating or water, 72 h after the test, 30 min after the patch was removed, 48 h, 72 h, respectively, evaluate the skin reaction, see if there are erythema, edema, papules and blisters, set up normal saline as a control group, and the experimental results are shown in Table 2: Table 2
[0045] III. Fragrance stability test The fragrance prepared according to Example 1 was placed in different environments, and the changes in appearance and odor were detected, and the test results are shown in Table 3: Table 3
[0046] As can be seen from the test results in Table 3, the prepared fragrance has excellent stability.
[0047] The above is only a preferred specific embodiment of the present application, but the protection scope of the present application is not limited thereto, any person skilled in the art can make equivalent substitutions or changes within the technical scope disclosed in the present application according to the technical solution and inventive concept of the present application, which should be covered within the protection scope of the present application.
[0048] The preferred embodiments of the application disclosed above are only to facilitate the elucidation of the application. The preferred embodiments do not describe all the details of the application and limit the application to the specific embodiments. Obviously, many modifications and variations can be made in light of the teachings above. The description is chosen and described in order to provide the best illustration of the application and its practical application to those skilled in the art and to enable those skilled in the art to utilize the application in its best mode. The application is only limited by the claims and their full scope and equivalents.
Claims
1. A soothing, sleep-inducing, and calming liquid fragrance, characterized in that, It consists of the following components by weight: 50-60 parts deionized water, 30-45 parts anhydrous ethanol, 2-4 parts Schisandra chinensis essential oil, 2-4 parts Acorus tatarinowii essential oil, 1-3 parts Neroli essential oil, 1-3 parts Chamomile essential oil, 1-2 parts Lilium brownii essential oil, 1-2 parts compound stabilizer, and 0.2-0.5 parts modified antioxidant.
2. The mood-soothing, sleep-aiding, and calming liquid fragrance according to claim 1, characterized in that, The preparation method of the composite stabilizer includes the following steps: Q1: Under nitrogen atmosphere, a mixed solution of ethoxyacetylene and hexane was added to a container, followed by the addition of tetrahydrofuran. After stirring and dissolving, the mixture was cooled, and a hexane solution containing n-butyllithium was added dropwise. After stirring and reacting, p-dimethylquinone was added, and the reaction was continued. After the reaction was completed, a saturated ammonium chloride solution was added to quench the reaction. The mixture was separated, extracted, washed, dried, concentrated, and purified to obtain product 1. Q2: Add product 1 and pyridine-N-oxide to a container containing dichloroethane, stir well, add triphenylphosphine trifluoroformamide gold, stir the reaction at room temperature, after the reaction is complete, add sodium hydroxide aqueous solution to quench the reaction, separate the liquid, extract, add hydrochloric acid, precipitate, dissolve, extract, wash, dry, concentrate, purify, and obtain product 2. Q3: Add product 2 and 12-hydroxystearic acid to a container, then add cyclohexane and p-toluenesulfonic acid, heat and stir under reflux, and after the reaction is complete, wash, dry, concentrate and purify to obtain the composite stabilizer.
3. The mood-soothing, sleep-aiding, and calming liquid fragrance according to claim 2, characterized in that, In Q1, the ratio of the amounts of ethoxyacetylene, tetrahydrofuran, n-butyllithium and p-dimethylquinone is (1.23-1.68) g : (17.5-22.3) mL : (3.11-3.53) g : (0.88-1.24) g.
4. The mood-soothing, sleep-aiding, and calming liquid fragrance according to claim 2, characterized in that, In Q2, the ratio of product 1, pyridine-N-oxide, dichloroethane, and triphenylphosphine trifluoroformamide gold is (1.11-1.54) g : (0.84-1.05) g : (10-16) mL : (0.111-0.125) mg.
5. The mood-soothing, sleep-aiding, and calming liquid fragrance according to claim 2, characterized in that, In Q3, the molar ratio of product 2 and 12-hydroxystearic acid is (0.9-1.1):(1.2-1.5).
6. The mood-soothing, sleep-aiding, and calming liquid fragrance according to claim 1, characterized in that, The method for preparing the modified antioxidant includes the following steps: S1: Under low temperature conditions, N,N-dimethylformamide, phosphorus oxychloride and acetonitrile were added to a container and stirred. After mixing, resveratrol was added and stirring was continued. After stirring was completed, the mixture was filtered, washed, added to distilled water, heated and hydrolyzed, filtered, washed and dried to obtain organic compound a. S2: Under low temperature conditions, organic compound a, tert-butyldimethylchlorosilane and tetrahydrofuran were added to a container in sequence, stirred, and a tetrahydrofuran solution containing imidazole was added. The mixture was stirred, rotary evaporated, and purified to obtain organic compound b. S3: Add organic compound b to a container containing tetrahydrofuran, then add sodium borohydride, stir at low temperature, add distilled water and continue stirring, then add ammonium chloride aqueous solution and stir, add tetrahydrofuran for dilution, filter, concentrate, purify and separate to obtain organic compound c; S4: Under low temperature conditions, chlorogenic acid, DCC, p-dimethylaminopyridine, and dichloromethane were mixed and stirred. Then, dichloromethane containing organic compound c was added. After stirring at low temperature, the mixture was stirred at room temperature, washed, dried, filtered, concentrated, and purified to obtain organic compound d. Organic compound d was added to a container containing tetrahydrofuran, followed by the addition of trifluoroacetic acid. Under nitrogen protection, the mixture was stirred at low temperature. After the reaction was completed, the mixture was concentrated and purified to obtain the modified antioxidant.
7. The mood-soothing, sleep-aiding, and calming liquid fragrance according to claim 6, characterized in that, In S1, the ratio of N,N-dimethylformamide, phosphorus oxychloride, acetonitrile, and resveratrol is (0.12-0.16) g : (0.28-0.37) g : (55-65) mL : (0.448-0.472) g; in S2, the ratio of organic compound a, tert-butyldimethylchlorosilane, and imidazole is (0.247-0.263) g : (1.423-1.521) g : (0.61-0.73) g.
8. The mood-soothing, sleep-aiding, and calming liquid fragrance according to claim 6, characterized in that, In S3, the ratio of organic matter b, sodium borohydride, distilled water and ammonium chloride aqueous solution is (0.112-0.214) g : (0.0071-0.0083) g : (0.1-0.15) mL : (0.28-0.32) mL.
9. A soothing, sleep-aiding, and calming liquid fragrance according to claim 6, characterized in that, In S4, the ratio of chlorogenic acid, DCC, p-dimethylaminopyridine and organic compound c is (0.342-0.358) g : (0.212-0.246) g : (0.011-0.013) g : (0.581-0.622) g; the ratio of organic compound d, tetrahydrofuran and trifluoroacetic acid is (0.191-0.205) g : (3-5) mL : (0.45-0.55) mL.
10. A method for preparing a mood-soothing, sleep-aiding, and calming liquid functional fragrance as described in any one of claims 1-9, comprising the following steps: Step 1: Add deionized water to the reactor, then add the composite stabilizer, stir and mix, then add the modified antioxidant and stir until uniformly dispersed to obtain the aqueous phase; Step 2: Mix the essential oils of Schisandra chinensis, Acorus calamus, Neroli, Chamomile, and Lily, then add anhydrous ethanol and sonicate to obtain the oil phase. Step 3: Slowly add the oil phase to the aqueous phase, mix, homogenize under high pressure, age, and filter to obtain a soothing, sleep-inducing, and calming liquid functional fragrance.