CN119258144B - Composition for improving sleep quality and preparation method and application thereof - Google Patents
Composition for improving sleep quality and preparation method and application thereof Download PDFInfo
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- CN119258144B CN119258144B CN202411794330.2A CN202411794330A CN119258144B CN 119258144 B CN119258144 B CN 119258144B CN 202411794330 A CN202411794330 A CN 202411794330A CN 119258144 B CN119258144 B CN 119258144B
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Classifications
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- C07D213/02—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members
- C07D213/04—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D213/60—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
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- C07D213/803—Processes of preparation
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- C11B1/108—Production of fats or fatty oils from raw materials by extracting after-treatment, e.g. of miscellae
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- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/001—Refining fats or fatty oils by a combination of two or more of the means hereafter
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- C11B3/00—Refining fats or fatty oils
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Abstract
本发明提出了一种提高睡眠质量的组合物及其制备方法和应用，属于医药技术领域。将薰衣草、紫罗兰、玫瑰、沉香经过超临界流体萃取得到萃取油，固体酶解，固定化离子液体萃取，解吸附，得到提取油，与萃取油、促透剂混合均匀，制得提高睡眠质量的组合物。本发明将制得的萃取油和提取油混合，加入促透剂，制得的提高睡眠质量的组合物通过皮肤吸收进入人体，达到调节脏腑气机，调和机体阴阳的作用，具有安神助眠、延长睡眠时间、提高睡眠功效、舒缓紧张情绪的功效，具有广阔的应用前景。The present invention proposes a composition for improving sleep quality, a preparation method and an application thereof, and belongs to the field of medical technology. Lavender, violet, rose and agarwood are subjected to supercritical fluid extraction to obtain an extracted oil, solid enzymatic hydrolysis, immobilized ionic liquid extraction, desorption, and extraction oil. The extracted oil is mixed evenly with the extracted oil and a penetration enhancer to obtain a composition for improving sleep quality. The present invention mixes the obtained extracted oil and the extracted oil, adds a penetration enhancer, and the obtained composition for improving sleep quality is absorbed into the human body through the skin, achieving the effect of regulating the qi of the internal organs and harmonizing the yin and yang of the body, having the effects of calming the mind and helping sleep, prolonging sleep time, improving sleep efficacy, and relieving tension, and has broad application prospects.
Description
Technical Field
The invention relates to the technical field of medicines, in particular to a composition for improving sleep quality, a preparation method and application thereof.
Background
One third of the life of a person spends in sleep, and high-quality sleep is a basis for ensuring that people finish daily work and life and keep healthy. Sleep is generally divided into two stages, non-rapid eye movement sleep and rapid eye movement sleep or deep sleep, according to changes of electroencephalogram, eyeball movement, electromyography, etc. Studies have shown that the light sleep period and the light sleep period, which account for about 55% of the entire sleep time, have little effect on relieving fatigue, whereas only the middle sleep period, the deep sleep period, and the rapid eye movement sleep period, which enter the deep sleep state, have a great effect on relieving fatigue. Because the cerebral cortex cells are in a full resting state in a deep sleep state, the cerebral cortex cells have important effects on eliminating fatigue, restoring energy, immune disease resistance and the like. However, this deep sleep takes only 25% of the total sleep time. If the human body cannot get effective deep sleep for a long time, people are easy to insomnia, and a series of pathological reactions of the human body are caused.
At present, the commercial essential oil has various types, generally single essential oil, and most consumers are unfamiliar with the blended essential oil, the application range is narrow, or the preparation method is complex, the price is high, and the sleep promoting effect is poor, so that the consumer compliance is poor.
Disclosure of Invention
The invention aims to provide a composition for improving sleep quality, a preparation method and application thereof, which can promote uric acid excretion, inhibit sodium urate crystallization, improve antioxidation, repair intestinal barriers, reduce inflammation, inhibit Xanthine Oxidase (XOD) activity and expression, reduce blood uric acid level, have good uric acid reducing effect and have wide application prospect.
The technical scheme of the invention is realized as follows:
The invention provides a preparation method of a composition for improving sleep quality, which comprises the steps of extracting lavender, violet, rose and agilawood through supercritical fluid to obtain extract oil, carrying out solid enzymolysis, extracting and desorbing by using immobilized ionic liquid to obtain the extract oil, and uniformly mixing the extract oil, the extract oil and a permeation enhancer to obtain the composition for improving sleep quality.
As a further improvement of the invention, the method comprises the following steps:
S1, freeze-drying lavender, violet, rose and agilawood, crushing, extracting by supercritical fluid, and collecting solid and extracted oil;
s2, adding the solid into water, adding complex enzyme for enzymolysis, inactivating enzyme, filtering, and removing the solvent from the filtrate under reduced pressure to obtain an extract;
S3, adding immobilized ionic liquid into the extract, performing ultrasonic stirring adsorption, filtering, adding the solid into ethanol, performing thermal desorption, filtering, washing the solid, recycling, and recovering the ethanol from the filtrate to obtain extract oil;
s4, uniformly mixing the extracted oil, the extracted oil and the permeation enhancer to prepare the composition for improving sleep quality.
As a further improvement of the invention, in the step S1, the mass ratio of the lavender to the violet to the rose to the agilawood is 10-12:7-9:3-5:2-4, the condition of supercritical fluid extraction is that the extraction pressure is 20-25MPa, the extraction temperature is 35-45 ℃, the flow rate of CO 2 is 5-10L/h, the extraction time is 1-3h, the addition amount of the entrainer is 1-2wt%, and the entrainer is ethanol.
As a further improvement of the invention, in the step S2, the mass ratio of the solid to the compound enzyme is 10:1-2, the mass ratio of the compound enzyme is 4-6:3, the enzymolysis temperature is 40-50 ℃ and the enzymolysis time is 2-4h.
As a further improvement of the invention, the mass ratio of the extract to the immobilized ionic liquid in the step S3 is 10:3-4, the ultrasonic stirring adsorption time is 0.5-1.5h, the power is 500-1000W, the heating temperature is 45-55 ℃, and the preparation method of the immobilized ionic liquid comprises the following steps:
t1, adding silica gel powder into ethanol, adding a silane coupling agent with double bonds, heating, stirring, reacting, filtering, washing and drying to obtain modified silica gel powder;
T2 adding the modified silica gel powder and N-vinyl imidazole into dichloromethane, adding an initiator, heating and stirring for reaction to obtain imidazole modified silica gel powder;
Adding the imidazole modified silica gel powder and the chloro-n-butane into acetone, heating and refluxing for reaction, filtering, washing and drying to obtain the substituted imidazole modified silica gel powder;
And T4, adding the substituted imidazole modified silica gel powder and the 2-sodium naphthalene sulfonate into water, stirring at room temperature, filtering, washing and drying to obtain the immobilized ionic liquid.
As a further improvement of the invention, the mass ratio of the silica gel powder to the silane coupling agent with double bonds in the step T1 is 10:3-5, the silane coupling agent with double bonds is selected from at least one of KH570, A151 and A171, the temperature of the heating and stirring reaction is 40-50 ℃ for 2-4h, the mass ratio of the modified silica gel powder to the N-vinylimidazole to the initiator in the step T2 is 15-20:7-10:0.01-0.02, the initiator is selected from at least one of potassium persulfate, sodium persulfate and ammonium persulfate, the temperature of the heating and stirring reaction is 45-55 ℃ for 3-5h, the mass ratio of the imidazole modified silica gel powder to the chloro-N-butane in the step T3 is 10:3-4, the time of the heating and reflux reaction is 20-24h, the mass ratio of the substituted imidazole modified silica gel powder to the 2-sodium naphthalene sulfonate in the step T4 is 12-15:4-7, and the time of stirring at room temperature is 7-9h.
As a further improvement of the invention, in the step S4, the mass ratio of the extracted oil to the permeation enhancer is 10:7-10:0.01-0.02, the permeation enhancer is a mixture of laurocapram and a permeation enhancer compound, the mass ratio is 10:3-5, and the structure of the permeation enhancer compound is shown as a formula I:
The preparation method of the penetration-promoting compound comprises the following steps:
U1. reacting salicylic acid with carveol under the action of a catalyst to prepare an intermediate, wherein the structure is as follows:
U2. reacting the intermediate with nicotinic acid under the action of a catalyst to obtain the penetration-promoting compound.
As a further improvement of the invention, the molar ratio of salicylic acid to carvacrol in the step U1 is 1-1.1:1, the catalyst is concentrated sulfuric acid, the addition amount is 2-3wt% of salicylic acid, the reaction temperature is 100-110 ℃ and the time is 4-6h, the molar ratio of the intermediate to nicotinic acid in the step U2 is 1:1-1.1, the catalyst is concentrated sulfuric acid, the addition amount is 2-3wt% of the intermediate, the reaction temperature is 100-110 ℃ and the time is 3-5h.
The invention further provides the composition for improving sleep quality prepared by the preparation method.
The invention further protects application of the composition for improving sleep quality in preparing medicaments for improving sleep, improving sleep quality and prolonging sleep time.
The invention has the following beneficial effects:
the aromatherapy is to make natural plants with aromatic smell into proper dosage form, act on local or whole body to achieve the medical care effects of preventing and treating diseases and promoting health, and utilize the aromatic smell of Chinese herbal medicines or extract aromatic essential oil to act on human body by oral administration, inhalation, skin absorption, etc. to achieve the effects of regulating viscera qi movement and harmonizing yin and yang of organism.
The main chemical components of the lavender essential oil are linalool, linalool acetate, lavender acetate and the like, wherein linalool can stimulate parasympathetic nervous system, has tranquilization effect, linalool acetate has tranquilization, relaxation and hypnotic effects, and the lavender essential oil is used for aromatherapy to effectively prevent sleep disorder, and the action mechanism of the lavender essential oil can be increased with the level of 5-hydroxytryptamine (5-HT) in vivo. Violet essential oils contain a large amount of monoterpenes and sesquiterpenes. Linalool (a monoterpene alcohol) is the main component of common violet essential oil, and can be used as antioxidant and neuroprotectant. The rose essential oil is a natural essential oil derived from rose petals, and has various effects including antioxidation, antibiosis, relaxation, emotion regulation and the like. The agilawood has multiple medicinal values, has multiple effects of clearing away heart fire, soothing nerves, tonifying qi, nourishing essence, detoxifying, preventing epidemic and the like, and the agilawood essential oil has volatile components such as linalool, linalool acetate, santalool and the like, and is considered to have the effects of soothing nerves, aiding sleep and relieving tension emotion. The compound extracted oil obtained by the supercritical fluid extraction method contains rich active components, has better effects of adjusting emotion and aiding sleep, but the active components of the product obtained by direct extraction are not completely extracted, so that the utilization rate of raw materials is reduced.
The invention further carries out enzymolysis on the extracted solid by compound enzyme (comprising cellulase and pectase), thereby promoting the wall breaking of plant cell walls, dissolving out a large amount of active components, and simultaneously, entering a large amount of impurities into the solution. The immobilized ionic liquid prepared and added in the invention has higher enrichment efficiency and adsorption capacity, so that the immobilized ionic liquid can effectively extract active molecules from a sample in solid phase extraction, is convenient for separation and desorption, and greatly improves the purification effect of active components.
The immobilized ionic liquid takes silica gel as a carrier, the surface of the immobilized ionic liquid is modified by a silane coupling agent with double bonds and then can be copolymerized with N-vinylimidazole, and then anion exchange and the like are carried out for further reaction, so that the immobilized ionic liquid is prepared, has the characteristics of good stability, strong dissolving capacity, easiness in separation and the like, can reduce the loss of the ionic liquid in the operation process, reduces the cost and reduces the environmental pollution, and has no residual anxiety of the ionic liquid.
The prepared composition for improving sleep quality is absorbed into human body through skin to achieve the effects of regulating viscera qi movement and harmonizing yin and yang of the organism, has the effects of soothing nerves, helping sleep, prolonging sleep time, improving sleep efficacy and relieving tension emotion, and has wide application prospect.
The intermediate is prepared by the esterification reaction of carveol and salicylic acid, the problem of stronger skin irritation when the carveol and the salicylic acid are used independently is solved, the combined intermediate can break and fuse the arrangement mode of fatty acid between cells or directly extract the fatty acid of the epidermis layer, so that the barrier function of skin is weakened, the permeability of chemical substances is increased, the intermediate further reacts with nicotinic acid, the problems that skin allergy is easily caused, the pH value of the skin is changed and the like when the nicotinic acid is directly used are solved, the anti-inflammatory, antibacterial and antioxidant properties of the skin are improved, the penetration-promoting effect on other substances is further improved, the preparation method of the penetration-promoting compound is simple, the condition is mild, the yield is high, the prepared product has good effect, the unexpected synergistic effect with laurocapram is achieved, the essential oil has better penetration promoting property, and the penetration-promoting effect is further improved after the penetration-promoting agent is added, and the drug effect is enhanced.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Silica gel powder with 150-250 μm and specific surface area of 600-800m2/g.
Cellulase, 5 ten thousand U/g, pectase, 5 ten thousand U/g, purchased from Shanghai Yuan Ye Biotechnology Co.
Preparation example 1 preparation of immobilized ionic liquid
The method comprises the following steps:
T1, adding 10g of silica gel powder into 200mL of ethanol, adding 3g of silane coupling agent A151, heating to 40 ℃, stirring and reacting for 2h, filtering, washing and drying to obtain modified silica gel powder;
T2 adding 15g of modified silica gel powder and 7g N-vinylimidazole into 500mL of dichloromethane, adding 0.01g of sodium persulfate, heating to 45 ℃, and stirring for reaction for 3 hours to obtain imidazole modified silica gel powder;
t3 adding 10g of imidazole modified silica gel powder and 3g of n-butyl chloride into 200mL of acetone, heating and refluxing for reaction for 20h, filtering, washing and drying to obtain the substituted imidazole modified silica gel powder;
t4 adding 12g of the substituted imidazole modified silica gel powder and 4g of 2-naphthalene sodium sulfonate into 200mL of water, stirring for 7h at room temperature, filtering, washing and drying to obtain the immobilized ionic liquid.
Preparation example 2 preparation of immobilized ionic liquid
The method comprises the following steps:
t1, adding 10g of silica gel powder into 200mL of ethanol, adding 5g of silane coupling agent A171, heating to 50 ℃, stirring for reaction for 4 hours, filtering, washing and drying to obtain modified silica gel powder;
t2 adding 20g of modified silica gel powder and 10g N-vinylimidazole into 500mL of dichloromethane, adding 0.02g of potassium persulfate, heating to 55 ℃, and stirring for reaction for 5 hours to obtain imidazole modified silica gel powder;
T3 adding 10g of imidazole modified silica gel powder and 4g of n-butyl chloride into 200mL of acetone, heating and refluxing for reaction for 24h, filtering, washing and drying to obtain substituted imidazole modified silica gel powder;
T4 adding 15g of the substituted imidazole modified silica gel powder and 7g of the 2-naphthalene sodium sulfonate into 200mL of water, stirring for 9h at room temperature, filtering, washing and drying to obtain the immobilized ionic liquid.
Preparation example 3 preparation of immobilized ionic liquid
The method comprises the following steps:
t1 adding 10g of silica gel powder into 200mL of ethanol, adding 4g of silane coupling agent KH570, heating to 45 ℃, stirring for reaction for 3h, filtering, washing and drying to obtain modified silica gel powder;
T2 adding 17g of modified silica gel powder and 8g N-vinylimidazole into 500mL of dichloromethane, adding 0.015g of ammonium persulfate, heating to 50 ℃, and stirring for reaction for 4 hours to obtain imidazole modified silica gel powder;
t3 adding 10g of imidazole modified silica gel powder and 3.5g of n-butyl chloride into 200mL of acetone, heating and refluxing for reaction for 22h, filtering, washing and drying to obtain the substituted imidazole modified silica gel powder;
and T4. Adding 13g of the substituted imidazole modified silica gel powder and 5g of the 2-naphthalene sodium sulfonate into 200mL of water, stirring for 8h at room temperature, filtering, washing and drying to obtain the immobilized ionic liquid.
Comparative preparation example 1
In comparison with preparation example 3, the difference is that step S4 is not performed.
Test example 1
The specific surface area and the total pore volume of the immobilized ionic liquid prepared in preparation examples 1-3 are measured by a 3-FLEX 3500 multi-station high-flux gas adsorber.
The results are shown in Table 1.
TABLE 1
| Group of | Specific surface area (m 2/g) | Total pore volume (cm 3/g) |
| Preparation example 1 | 856.7 | 0.52 |
| Preparation example 2 | 859.2 | 0.54 |
| Preparation example 3 | 863.4 | 0.55 |
| Comparative preparation example 1 | 821.4 | 0.49 |
As shown in the table above, the immobilized ionic liquid prepared in preparation examples 1-3 of the invention has a relatively high specific surface area.
Preparation example 4 preparation of penetration enhancing Compounds
The synthetic route is as follows:
The method comprises the following steps:
U1. dissolving 10mmol of salicylic acid and 10mmol of carvacrol in 200mL of toluene, adding concentrated sulfuric acid, wherein the addition amount is 3wt% of the salicylic acid, heating and refluxing for reaction for 5h, removing the solvent under reduced pressure, washing with water, drying, recrystallizing with acetone to obtain an intermediate, wherein the calculated value of ESI-MS is C 17H21O3(M+H)+ 243.14, the measured value is 243.1, and the yield is 78%.
Nuclear magnetic results ：1H NMR(300MHz,CDCl3)δ7.8(d,J＝6.5Hz,1H),7.3(m,1H),6.89-6.92(m,2H),5.37(t,1H),5.0(br,1H),4.85(d,J＝4.2Hz,1H),4.65(d,J＝4.4Hz,1H),4.42(t,1H),2.33(m,1H),1.89-2.2(m,4H),1.72(s,6H).
U2. dissolving 10mmol of the intermediate and 10mmol of nicotinic acid in 200mL of toluene, adding concentrated sulfuric acid with the addition amount of 2wt% of the intermediate, heating and refluxing for reaction for 4h, washing with water, drying, and recrystallizing with acetone to obtain the penetration-promoting compound. ESI-MS calculated C 23H24NO4(M+H)+ 378.16, found 378.2, yield 72%.
Nuclear magnetic results ：1H NMR(300MHz,CDCl3)δ9.05(s,1H),8.72(d,J＝6.7Hz,1H),8.17(d,J＝6.2Hz,1H),7.92(d,J＝6.0Hz,1H),7.54(m,1H),7.42(m,1H),7.19(m,2H),5.37(t,1H),4.82(d,1H),4.62(d,1H),4.41(t,1H),2.32(m,1H),1.82-2.05(m,4H),1.75(s,6H).
Example 1
The embodiment provides a preparation method of a composition for improving sleep quality, which comprises the following steps:
s1, freeze-drying 10g of lavender, 7g of violet, 3g of rose and 2g of agilawood, crushing, extracting by supercritical fluid, and collecting solid and extracted oil;
The supercritical fluid extraction conditions comprise extraction pressure of 20MPa, extraction temperature of 35 ℃, CO 2 flow rate of 5L/h, extraction time of 1h, the addition amount of the entrainer of 1wt%, and the entrainer of ethanol;
S2, adding 10g of solid into 200mL of water, adding 1g of complex enzyme, carrying out enzymolysis for 2 hours at 40 ℃, inactivating enzyme, filtering, and removing solvent from filtrate under reduced pressure to obtain an extract;
the compound enzyme is cellulase and pectase, and the mass ratio is 4:3;
S3, adding 3g of the immobilized ionic liquid prepared in the preparation example 1 into 10g of the extract, carrying out ultrasonic stirring and adsorption for 0.5h at 500W, filtering, adding the solid into 50mL of ethanol, heating to 45 ℃, desorbing for 30min, filtering, washing the solid, recycling the filtrate, and recycling the ethanol to prepare extract oil;
s4, uniformly mixing 10g of extract oil, 7g of extract oil and 0.01g of penetration enhancer to prepare a composition for improving sleep quality;
the penetration enhancer is a mixture of laurocapram and the penetration enhancer compound prepared in preparation example 4, and the mass ratio is 10:3.
Example 2
The embodiment provides a preparation method of a composition for improving sleep quality, which comprises the following steps:
s1, freeze-drying 12g of lavender, 9g of violet, 5g of rose and 4g of agilawood, crushing, extracting by supercritical fluid, and collecting solid and extracted oil;
The supercritical fluid extraction conditions comprise extraction pressure of 25MPa, extraction temperature of 45 ℃, CO 2 flow rate of 10L/h, extraction time of 3h, the addition amount of the entrainer is 2wt%, and the entrainer is ethanol;
s2, adding 10g of solid into 200mL of water, adding 2g of complex enzyme, carrying out enzymolysis for 4 hours at 50 ℃, inactivating enzyme, filtering, and removing solvent from filtrate under reduced pressure to obtain an extract;
the compound enzyme is cellulase and pectase, and the mass ratio is 6:3;
S3, adding 4g of the immobilized ionic liquid prepared in the preparation example 2 into 10g of the extract, carrying out 1000W ultrasonic stirring and adsorption for 1.5h, filtering, adding the solid into 50mL of ethanol, heating to 55 ℃, desorbing for 30min, filtering, washing the solid, recycling the filtrate, and recycling the ethanol to prepare extract oil;
s4, uniformly mixing 10g of extract oil, 10g of extract oil and 0.02g of penetration enhancer to prepare a composition for improving sleep quality;
the penetration enhancer is a mixture of laurocapram and the penetration enhancer compound prepared in preparation example 4, and the mass ratio is 10:5.
Example 3
The embodiment provides a preparation method of a composition for improving sleep quality, which comprises the following steps:
s1, freeze-drying 11g of lavender, 8g of violet, 4g of rose and 3g of agilawood, crushing, extracting by supercritical fluid, and collecting solid and extracted oil;
The supercritical fluid extraction conditions comprise extraction pressure of 22MPa, extraction temperature of 40 ℃, CO 2 flow rate of 7L/h, extraction time of 2h, the addition amount of the entrainer is 1.5wt%, and the entrainer is ethanol;
S2, adding 10g of solid into 200mL of water, adding 1.5g of complex enzyme, carrying out enzymolysis for 3 hours at 45 ℃, inactivating enzyme, filtering, and removing the solvent from the filtrate under reduced pressure to obtain an extract;
The compound enzyme is cellulase and pectase, and the mass ratio is 5:3;
S3, adding 3.5g of the immobilized ionic liquid prepared in the preparation example 1 into 10g of the extract, carrying out ultrasonic stirring and adsorption for 1h at 700W, filtering, adding the solid into 50mL of ethanol, heating to 50 ℃, desorbing for 30min, filtering, washing the solid, recycling the filtrate, and recycling the ethanol to prepare extract oil;
S4, uniformly mixing 10g of extract oil, 8g of extract oil and 0.015g of penetration enhancer to prepare a composition for improving sleep quality;
the penetration enhancer is a mixture of laurocapram and the penetration enhancer compound prepared in preparation example 4, and the mass ratio is 10:4.
Example 4
The difference compared to example 3 is that the permeation enhancer is a single laurocapram.
Example 5
The difference compared to example 3 is that the permeation enhancer is a single permeation enhancer compound prepared in preparation example 4.
Example 6
The difference compared to example 3 is that the complex enzyme is a single cellulase.
Example 7
The difference compared to example 3 is that the complex enzyme is a single pectase.
Comparative example 1
The difference compared to example 3 is that no permeation enhancer was added.
The method comprises the following steps:
s4, uniformly mixing 10g of extract oil and 8g of extract oil to prepare the composition for improving sleep quality.
Comparative example 2
In comparison with example 3, the difference is that no complex enzyme was added.
The method comprises the following steps:
s2, adding 10g of solid into 200mL of water, heating, boiling and extracting for 3h, filtering, and removing the solvent from the filtrate under reduced pressure to obtain an extract.
Comparative example 3
In comparison with example 3, the difference is that step S3 is not performed.
The method comprises the following steps:
s1, freeze-drying 11g of lavender, 8g of violet, 4g of rose and 3g of agilawood, crushing, extracting by supercritical fluid, and collecting solid and extracted oil;
The supercritical fluid extraction conditions comprise extraction pressure of 22MPa, extraction temperature of 40 ℃, CO 2 flow rate of 7L/h, extraction time of 2h, the addition amount of the entrainer is 1.5wt%, and the entrainer is ethanol;
S2, adding 10g of solid into 200mL of water, adding 1.5g of complex enzyme, carrying out enzymolysis for 3 hours at 45 ℃, inactivating enzyme, filtering, and removing the solvent from the filtrate under reduced pressure to obtain an extract;
The compound enzyme is cellulase and pectase, and the mass ratio is 5:3;
S3, uniformly mixing 10g of extract oil, 8g of extract and 0.015g of penetration enhancer to prepare a composition for improving sleep quality;
the penetration enhancer is a mixture of laurocapram and the penetration enhancer compound prepared in preparation example 4, and the mass ratio is 10:4.
Comparative example 4
The difference from example 3 is that no extraction oil was added in step S4.
The method comprises the following steps:
s4, uniformly mixing 18g of extracted oil and 0.015g of penetration enhancer to prepare a composition for improving sleep quality;
the penetration enhancer is a mixture of laurocapram and the penetration enhancer compound prepared in preparation example 4, and the mass ratio is 10:4.
Comparative example 5
The difference from example 3 is that no extracted oil was added in step S4.
The method comprises the following steps:
s4, uniformly mixing 18g of extract oil and 0.015g of penetration enhancer to prepare a composition for improving sleep quality;
the penetration enhancer is a mixture of laurocapram and the penetration enhancer compound prepared in preparation example 4, and the mass ratio is 10:4.
Comparative example 6
The difference compared to example 3 is that an immobilized ionic liquid was prepared from comparative preparation 1.
Test example 2
150 Healthy ICR mice (male and female halves) were randomly divided into 15 groups, 10 mice in each group were respectively the example 1-7 groups, the comparative example 1-6 groups, the control group, the levolinalool groups, the example 1-7 groups, the comparative example 1-6 groups, and 1 mL/one of the corresponding prepared sleep quality improving composition was uniformly coated on the bellyband, the levolinalool group was given 5mg/kg of levolinalool, then each group of mice was intraperitoneally injected with 50mg/kg of pentobarbital sodium, and after administration, the mice lost for 1min after the eversion of the positive reflection, indicating that they had fallen to sleep. The time between injection of sodium pentobarbital and disappearance of the mouse eversion is taken as a sleep latency period, and the time between disappearance of the mouse eversion and restoration of the mouse eversion is taken as a sleep period. The time of injection of sodium pentobarbital, the time of disappearance of the specular reflection and the time of recovery of the specular reflection were recorded for each group of mice, and sleep latency and sleep time were calculated. The results are shown in Table 2.
TABLE 2
Note that P <0.05 compared to the control group.
From the above table, the compositions for improving sleep quality prepared in examples 1 to 3 of the present invention can obviously prolong the sleep time of mice and shorten the sleep latency.
Test example 3
150 Healthy ICR mice (male and female halves) are randomly divided into 15 groups, 10 mice in each group are respectively an example 1-7 group, a comparative example 1-6 group, a control group and a left-handed linalool group, 1 mL/corresponding prepared composition for improving sleep quality is uniformly coated on bellyband of the mice in the examples 1-7 group and the comparative examples 1-6 group, 5mg/kg of the left-handed linalool group is given to the left-handed linalool group, 30mg/kg of pentobarbital sodium is injected into abdominal cavities of the mice in each group, the mice in each group are subjected to over-reflection disappearance for more than 1min within 30min as a sleep index, the number of sleep in each group of mice within 30min is recorded, and the sleep rate of each group of mice is calculated. The results are shown in Table 3.
TABLE 3 Table 3
| Group of | Sleep Rate (%) |
| Control group | 10 |
| L-linalool group | 40 |
| Example 1 | 90 |
| Example 2 | 90 |
| Example 3 | 100 |
| Example 4 | 60 |
| Example 5 | 50 |
| Example 6 | 70 |
| Example 7 | 70 |
| Comparative example 1 | 40 |
| Comparative example 2 | 50 |
| Comparative example 3 | 60 |
| Comparative example 4 | 50 |
| Comparative example 5 | 40 |
| Comparative example 6 | 80 |
As is clear from the above table, the sleep quality improving compositions prepared in examples 1 to 3 of the present invention are capable of remarkably improving the sleep rate of mice.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.
Claims (9)
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