Sleep-aiding plant essential oil composition and preparation method thereof

Abstract

The invention relates to the technical field of sleep-aiding essential oil, in particular to a sleep-aiding plant essential oil composition and a preparation method thereof. The plant essential oil composition is prepared from the following raw material components: plant essential oil, modified mannose and modified carbomer, the preparation raw materials of the plant essential oil comprise a plant mixture. The plant mixture consists of the following components in parts by weight: 15-20 parts of lavender, 8-12 parts of valerian, 5-8 parts of michelia figo, 4-6 parts of garden balsam stem, 4-6 parts of semiliquidambar cathayensis, 5-9 parts of permanent flower and 4-7 parts of swertia. According to the invention, the modified mannose and the modified carbomer are adopted to prepare the double-layer micro-capsule for wrapping the plant essential oil, so that the prepared plant essential oil composition is good in sleep aiding effect and strong in slow release property and stability.

Description

Technical Field

[0001] The invention relates to the technical field of sleep-aiding essential oils, and in particular to a sleep-aiding plant essential oil composition and a preparation method thereof. Background Art

[0002] Sleep disorders and insomnia have become a common phenomenon, with the main symptoms being difficulty falling asleep, poor sleep quality, and short sleep time. Long-term insomnia can cause physiological dysfunction, fatigue, memory loss, and in severe cases may cause some adverse symptoms, inducing physical and mental illnesses, etc. Existing methods include the use of essential oil therapy, also known as aromatherapy, for conditioning treatment, which is considered an effective intervention measure in improving sleep problems. At present, the existing natural plant essential oil preparation technology mainly has the following problems: due to the irritation of the ingredients, applying it on the skin will cause skin allergies, redness, swelling, itching and other symptoms; through breathing, the volatilized essential oil comes into contact with the respiratory mucosa, causing poisoning in the body, damaging the liver and kidneys, causing dizziness, chest tightness, shortness of breath, and loss of appetite; the quality is uneven, the fragrance is strong and has a peculiar smell, it evaporates too quickly, and it is poorly absorbed when applied to the skin, and the product contains many impurities; it contains a large amount of additives, and uses volatile organic solvents to extract the ingredients in the plant raw materials. The organic solvent residue is toxic, the extraction time is long and the efficiency is low, resulting in a large amount of waste of raw materials, etc. Summary of the invention

[0003] In view of the deficiencies in the prior art, the present invention provides a sleep-aiding plant essential oil composition and a preparation method thereof.

[0004] The present invention is achieved through the following technical solutions: A sleep-aiding plant essential oil composition, the preparation raw materials of which include the following components in parts by weight: 3-5 parts of plant essential oil, 1-1.5 parts of modified mannose, and 2-3 parts of modified carbomer.

[0005] Furthermore, the raw materials for preparing the plant essential oil include a plant mixture; the plant mixture consists of the following components in parts by weight: 15-20 parts of lavender, 8-12 parts of valerian, 5-8 parts of Michelia, 4-6 parts of Herba Polygoni Multiflori, 4-6 parts of Helichrysum, 5-9 parts of Helichrysum, and 4-7 parts of Swertia paniculata.

[0006] Furthermore, the method for preparing the plant essential oil comprises the following steps: A1: Add citric acid and tartaric acid to deionized water and mix well to obtain a mixed acid solution, freeze-dry the plant mixture at -20°C, crush through a 40-mesh sieve, immerse completely in the mixed acid solution, stir at 200-300 rpm, keep warm at 60-70°C for 2-3 hours, filter, wash with deionized water, add to a honey aqueous solution and immerse completely, stir at 200 rpm, keep warm at 50-60°C for 2-3 hours, filter, wash with deionized water to obtain pretreated plants; A2: Add the pretreated plant obtained in step A1 into distilled water, add 1-ethyl-3-methylimidazolium tetrafluoroborate ionic liquid into the distilled water, heat to boiling, and maintain a slight boiling at normal pressure, distill for 4 hours, collect the condensate, let it stand for stratification, take the upper oil phase, and dry it with anhydrous sodium sulfate to obtain the plant essential oil.

[0007] Furthermore, in step A1, the mass concentrations of citric acid and tartaric acid in deionized water are 80-100 g / L and 12-15 g / L, respectively.

[0008] Furthermore, in step A1, the mass concentration of the honey aqueous solution is 12-18wt%.

[0009] Furthermore, in step A2, the ratio of the pretreated plant to distilled water is 1 g: 6-9 mL.

[0010] Furthermore, in step A2, the concentration of the 1-ethyl-3-methylimidazolium tetrafluoroborate ionic liquid in distilled water is 0.8-1.2 vol%.

[0011] Furthermore, the raw materials for preparing the modified mannose include the following components in parts by weight: 7-9 parts of fumaric acid, 10-14 parts of 1-amino-1-deoxy-β-D-pyranose, and 13-18 parts of resveratrol.

[0012] Furthermore, the preparation method of the modified mannose comprises the following steps: B1: Add fumaric acid to DMF and mix well, heat to 50°C, add EDC and NHS, stir at 150-200 rpm for 2-3h, add 1-amino-1-deoxy-β-D-pyranose, react at 50-60°C and 500-600 rpm for 10-12h, cool to room temperature, centrifuge at 8000 rpm for 15-20 min, wash the precipitate with DMF and acetone, and dry at 80°C to obtain fumaric acid-mannose; B2: The fumarate-mannose obtained in step B1 is dissolved in formamide to obtain a fumarate-mannose solution, resveratrol is added to thionyl chloride, reacted at 70°C for 1 h, added to the fumarate-mannose solution, 4-dimethylaminopyridine (DMAP) is added, stirred at 600-700 rpm at 50-60°C for 2 h, allowed to stand at 4°C for 2-3 h, centrifuged at 5000 rpm for 15-20 min, the precipitate is washed with anhydrous ethanol and deionized water, and dried in vacuo at 40-50°C to obtain modified mannose.

[0013] Furthermore, in step B1, the mass concentration of fumaric acid in DMF is 10 mg / mL.

[0014] Furthermore, in step B1, the mass ratio of fumaric acid, EDC and NHS is 1:1.6:0.9.

[0015] Furthermore, in step B2, the mass concentration of fumarate-mannose in formamide is 15-20 mg / mL.

[0016] Furthermore, in step B2, the ratio of resveratrol to thionyl chloride is 2 g: 6-9 mL.

[0017] Furthermore, in step B2, the mass ratio of resveratrol to DMAP is 10:1.

[0018] Furthermore, the raw materials for preparing the modified carbomer include the following components in parts by weight: 4-6 parts of carbomer and 3-5 parts of citric acid.

[0019] Furthermore, the preparation method of the modified carbomer comprises the following steps: C1: Add carbomer, DCC and NHS to DMSO, stir at 200-300 rpm for 5-6 h, filter, wash the filter cake with deionized water, freeze-dry at -20°C, add to 0.1 g / mL citric acid solution, stir at 50-60°C and 200-300 rpm for 3-4 h; C2: After the reaction of step C1 is completed, stand at 4°C for 3 h, centrifuge at 5000 rpm for 20-30 min, wash the precipitate with deionized water, and freeze-dry at -40°C to obtain modified carbomer.

[0020] Furthermore, in step C1, the mass ratio of carbomer, DCC and NHS is 1:1.2:0.8.

[0021] Furthermore, in step C1, the mass concentration of DCC in DMSO is 6 mg / mL.

[0022] Furthermore, the present invention also provides a method for preparing the sleep-aiding plant essential oil composition, comprising the following steps: S1: Take modified carbomer and add it to distilled water and mix well to obtain a modified carbomer solution, add modified mannose and plant essential oil into deionized water, emulsify at 1300-1500 rpm for 20-30 min, and drip into the modified carbomer solution at a rate of 1-1.5 mL / min; S2: After the step S1 is added dropwise, stir at 40-50°C and 500-600 r / min for 30-40 min, cool to room temperature, centrifuge at 4000 r / min for 30 min, wash the precipitate with anhydrous ethanol, and dry in vacuo at 25°C to obtain a sleep-aiding plant essential oil composition.

[0023] Furthermore, in step S1, the mass concentration of the modified carbomer in distilled water is 0.1-0.2 g / mL.

[0024] Furthermore, in step S1, the mass concentration of the modified mannose in deionized water is 0.04-0.06 g / mL.

[0025] Compared with the prior art, the present invention has the following beneficial effects: The present invention provides a sleep-aiding plant essential oil composition, with plant essential oil as core material, and modified mannose and modified carbomer are used to coat the plant essential oil to form microcapsules, which avoid the defects of fast volatilization of plant essential oil and poor solubility in aqueous phase system, broaden its application field, and the coating layer encapsulates the plant essential oil, effectively protects the active substance, improves stability, and the encapsulated plant essential oil has the advantages of sustained release and long-term effect. The plant essential oil of the present invention is extracted and prepared by using a plant mixture of lavender, valerian, Michelia, Herba scutellariae, Helichrysum, and Swertia japonica, and each component is reasonably compatible, synergistic, and can effectively improve sleep quality. Soaking the plant mixture in tartaric acid, citric acid and honey aqueous solution can moisten and soften the plant cell wall, disperse the fiber structure, be conducive to the release of active ingredients, improve the extraction rate, and at the same time not to contact the oil component in the deep cell, and avoid the loss during the distillation process. Resveratrol has certain antioxidant and antibacterial properties, can enhance the stability of plant essential oils, effectively avoid the use of fungicides, and is safe and environmentally friendly. At the same time, resveratrol can provide hydrophobic groups and covalently link with hydrophilic 1-amino-1-deoxy-β-D-pyranose through fumaric acid to obtain modified mannose with one hydrophilic end and the other hydrophobic end. In water, the hydrophilic end faces outward and the hydrophobic end faces inward, and can self-assemble and coat hydrophobic plant essential oils. The hydrophobic interaction between resveratrol and plant essential oils is strong, and the coating rate is high. At the same time, the phenyl group of resveratrol is also easy to form π-π conjugation with the aromatic groups in the active substances in the essential oils, thereby stably fixing them inside the microcapsules, increasing the loading capacity of the active substances in the essential oils, improving stability and dispersibility, and enhancing the sustained-release effect. Carbomer is a water-soluble high molecular polymer. In the present invention, the carboxyl group of carbomer and the hydroxyl group of citric acid are subjected to esterification reaction in an EDC and NHS catalytic system to obtain modified carbomer. The carboxyl group content of the carbomer modified by citric acid grafting is increased, thereby improving the hydrophilicity. After the essential oil is wrapped with modified mannose, the hydrophilic 1-amino-1-deoxy-β-D-pyranose end faces outward, and the modified carbomer can be adsorbed through the hydrophilicity and electrostatic attraction of the surface, so that the modified carbomer is spontaneously enriched on the surface of the modified mannose-coated essential oil to form a wrapping layer. At the same time, the hydroxyl group of 1-amino-1-deoxy-β-D-pyranose can be cross-linked with the carboxyl group of the modified carbomer to improve the compactness, thereby obtaining a plant essential oil microcapsule wrapped with a double layer of modified mannose and modified carbomer, thereby significantly improving the stability and enhancing the sustained-release performance. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] In order to more clearly illustrate the technical solutions in the present invention or the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings in the following description are only for the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0027] Figure 1This is an electron microscope photo of the plant essential oil composition described in Example 1 of the present invention; Figure 2 Testing the sleep-aiding effect of the plant essential oil composition of the present invention; Figure 3 This is a test of the sustained-release effect of the plant essential oil composition of the present invention. DETAILED DESCRIPTION

[0028] In order to make the purpose, technical scheme and advantages of the present invention more clear, the present invention is further described in detail below in conjunction with specific embodiments, but the present invention is not limited to the following embodiments. It should be noted that, unless otherwise specified, the chemical reagents involved in the present invention are purchased through commercial channels.

[0029] Example 1: A sleep-aiding plant essential oil composition, the preparation raw materials include the following components in parts by weight: 5 parts of plant essential oil, 1.5 parts of modified mannose, and 3 parts of modified carbomer.

[0030] The raw materials for preparing the plant essential oil include a plant mixture; the plant mixture consists of the following components in parts by weight: 20 parts of lavender, 12 parts of valerian, 8 parts of Michelia, 6 parts of Herba Polygoni Multiflori, 6 parts of Helichrysum sibiricum, 9 parts of Helichrysum odoratum and 7 parts of Swertia japonica.

[0031] The preparation method of plant essential oil comprises the following steps: A1: Add citric acid and tartaric acid into deionized water and mix well to obtain a mixed acid solution. The mass concentrations of citric acid and tartaric acid in deionized water are 100 g / L and 15 g / L, respectively. Freeze-dry the plant mixture at -20°C, crush through a 40-mesh sieve, immerse it completely in the mixed acid solution, stir at 300 rpm, keep warm at 70°C for 3 h, filter, wash with deionized water, add it into a 18wt% honey aqueous solution and immerse it completely, stir at 200 rpm, keep warm at 60°C for 3 h, filter, wash with deionized water to obtain pretreated plants; A2: Add the pretreated plant obtained in step A1 into distilled water in a ratio of 1 g:9 mL. Add 1-ethyl-3-methylimidazolium tetrafluoroborate ionic liquid into the distilled water in a concentration of 1.2 vol%. Heat to boiling and keep it slightly boiling at normal pressure. Distill for 4 h, collect the condensate, let it stand for stratification, take the upper oil phase, and dry it over anhydrous sodium sulfate to obtain plant essential oil.

[0032] The raw materials for preparing modified mannose include the following components in parts by weight: 9 parts of fumaric acid, 14 parts of 1-amino-1-deoxy-β-D-pyranose, and 18 parts of resveratrol.

[0033] The preparation method of modified mannose comprises the following steps: B1: Add 9 g of fumaric acid to 900 mL of DMF and mix well, heat to 50°C, add 14.4 g of EDC and 8.1 g of NHS, stir at 200 rpm for 3 h, add 14 g of 1-amino-1-deoxy-β-D-pyranose, react at 60°C and 600 rpm for 12 h, cool to room temperature, centrifuge at 8000 rpm for 20 min, wash the precipitate with DMF and acetone, and dry at 80°C to obtain fumaric acid-mannose; B2: The fumaric acid-mannose obtained in step B1 was dissolved in formamide to obtain a 20 mg / mL fumaric acid-mannose solution, 18 g of resveratrol was added to 81 mL of dichlorothionyl, reacted at 70°C for 1 h, added to the fumaric acid-mannose solution, 1.8 g of DMAP was added, stirred at 700 rpm for 2 h at 60°C, allowed to stand at 4°C for 3 h, centrifuged at 5000 rpm for 20 min, the precipitate was washed with anhydrous ethanol and deionized water, and dried in vacuo at 50°C to obtain modified mannose.

[0034] The raw materials for preparing the modified carbomer include the following components in parts by weight: 6 parts of carbomer and 5 parts of citric acid.

[0035] Furthermore, the preparation method of the modified carbomer comprises the following steps: C1: Add 5 g of citric acid to 50 mL of deionized water to prepare a 0.1 g / mL citric acid solution, add 6 g of carbomer, 7.2 g of DCC and 4.8 g of NHS to 1200 mL of DMSO, stir at 300 rpm for 6 h, filter, wash the filter cake with deionized water, freeze-dry at -20 °C, add to the citric acid solution, stir at 60 °C and 300 rpm for 4 h; C2: After the reaction of step C1 is completed, the mixture is allowed to stand at 4°C for 3 h, centrifuged at 5000 rpm for 30 min, the precipitate is washed with deionized water, and freeze-dried at -40°C to obtain modified carbomer.

[0036] This embodiment also provides a method for preparing the sleep-aiding plant essential oil composition, comprising the following steps: S1: Take 3 g of modified carbomer and add it to 15 mL of distilled water and mix well to obtain a modified carbomer solution. Add 1.5 g of modified mannose and 5 g of plant essential oil to 25 mL of deionized water, emulsify at 1500 rpm for 30 min, and drip into the modified carbomer solution at a rate of 1.5 mL / min. S2: After the step S1 is added dropwise, the mixture is stirred at 50°C and 600 r / min for 40 min, cooled to room temperature, and centrifuged at 4000 r / min for 30 min. The precipitate is washed with anhydrous ethanol and dried in vacuo at 25°C to obtain a sleep-aiding plant essential oil composition.

[0037] Example 2: A sleep-aiding plant essential oil composition, the preparation raw materials include the following components in parts by weight: 3 parts of plant essential oil, 1 part of modified mannose, and 2 parts of modified carbomer.

[0038] The raw materials for preparing the plant essential oil include a plant mixture; the plant mixture consists of the following components in parts by weight: 15 parts of lavender, 8 parts of valerian, 5 parts of Michelia, 4 parts of Herba Polygoni Multiflori, 4 parts of Helichrysum Sinensis, 5 parts of Helichrysum odoratum and 4 parts of Swertia paniculata.

[0039] The preparation method of plant essential oil comprises the following steps: A1: Add citric acid and tartaric acid into deionized water and mix well to obtain a mixed acid solution. The mass concentrations of citric acid and tartaric acid in deionized water are 80 g / L and 12 g / L, respectively. Freeze-dry the plant mixture at -20°C, crush through a 40-mesh sieve, immerse it completely in the mixed acid solution, stir at 200 rpm, keep warm at 60°C for 2 h, filter, wash with deionized water, add it into a 12wt% honey aqueous solution and immerse it completely, stir at 200 rpm, keep warm at 50°C for 2 h, filter, wash with deionized water to obtain pretreated plants; A2: Add the pretreated plant obtained in step A1 into distilled water in a ratio of 1 g:6 mL. Add 1-ethyl-3-methylimidazolium tetrafluoroborate ionic liquid into the distilled water in a concentration of 0.8 vol%. Heat to boiling and keep it slightly boiling at normal pressure. Distill for 4 h, collect the condensate, let it stand for stratification, take the upper oil phase, and dry it over anhydrous sodium sulfate to obtain plant essential oil.

[0040] The raw materials for preparing modified mannose include the following components in parts by weight: 7 parts of fumaric acid, 10 parts of 1-amino-1-deoxy-β-D-pyranose, and 13 parts of resveratrol.

[0041] The preparation method of modified mannose comprises the following steps: B1: Add 7 g of fumaric acid to 700 mL of DMF and mix well, heat to 50°C, add 11.2 g of EDC and 6.3 g of NHS, stir at 150 rpm for 2 h, add 10 g of 1-amino-1-deoxy-β-D-pyranose, react at 50°C and 500 rpm for 10 h, cool to room temperature, centrifuge at 8000 rpm for 15 min, wash the precipitate with DMF and acetone, and dry at 80°C to obtain fumaric acid-mannose; B2: The fumaric acid-mannose obtained in step B1 was dissolved in formamide to obtain a 15 mg / mL fumaric acid-mannose solution, 13 g of resveratrol was added to 39 mL of dichlorothionyl, reacted at 70°C for 1 h, added to the fumaric acid-mannose solution, 1.3 g of DMAP was added, stirred at 600 rpm for 2 h at 50°C, allowed to stand at 4°C for 2 h, centrifuged at 5000 rpm for 15 min, the precipitate was washed with anhydrous ethanol and deionized water, and dried in vacuo at 40°C to obtain modified mannose.

[0042] The raw materials for preparing the modified carbomer include the following components in parts by weight: 4 parts of carbomer and 3 parts of citric acid.

[0043] Furthermore, the preparation method of the modified carbomer comprises the following steps: C1: Add 3 g of citric acid to 30 mL of deionized water to prepare a 0.1 g / mL citric acid solution, add 4 g of carbomer, 4.8 g of DCC and 3.2 g of NHS to 800 mL of DMSO, stir at 200 rpm for 5 h, filter, wash the filter cake with deionized water, freeze-dry at -20°C, add to 0.1 g / mL citric acid solution, stir at 50°C and 200 rpm for 3 h; C2: After the reaction of step C1 is completed, the mixture is allowed to stand at 4°C for 3 h, centrifuged at 5000 rpm for 20 min, the precipitate is washed with deionized water, and freeze-dried at -40°C to obtain modified carbomer.

[0044] This embodiment also provides a method for preparing the sleep-aiding plant essential oil composition, comprising the following steps: S1: Take 2 g of modified carbomer and add it to 20 mL of distilled water and mix well to obtain a modified carbomer solution. Add 1 g of modified mannose and 3 g of plant essential oil to 25 mL of deionized water, emulsify at 1300 rpm for 20 min, and drip into the modified carbomer solution at a rate of 1 mL / min. S2: After the step S1 is added dropwise, the mixture is stirred at 40°C and 500 r / min for 30 min, cooled to room temperature, and centrifuged at 4000 r / min for 30 min. The precipitate is washed with anhydrous ethanol and dried in vacuo at 25°C to obtain a sleep-aiding plant essential oil composition.

[0045] Example 3: A sleep-aiding plant essential oil composition, the preparation raw materials include the following components in parts by weight: 4 parts of plant essential oil, 1.4 parts of modified mannose, and 2.5 parts of modified carbomer.

[0046] The raw materials for preparing the plant essential oil include a plant mixture; the plant mixture consists of the following components in parts by weight: 18 parts of lavender, 10 parts of valerian, 6 parts of Michelia, 5 parts of Herba Polygoni Multiflori, 5 parts of Helichrysum sibiricum, 7 parts of Helichrysum odoratum and 6 parts of Swertia japonica.

[0047] The preparation method of plant essential oil comprises the following steps: A1: Add citric acid and tartaric acid into deionized water and mix well to obtain a mixed acid solution. The mass concentrations of citric acid and tartaric acid in deionized water are 90 g / L and 14 g / L, respectively. Freeze-dry the plant mixture at -20°C, crush through a 40-mesh sieve, immerse it completely in the mixed acid solution, stir at 250 rpm, keep warm at 65°C for 2.5 h, filter, wash with deionized water, add it into a 15wt% honey aqueous solution and immerse it completely, stir at 200 rpm, keep warm at 55°C for 2.5 h, filter, wash with deionized water to obtain pretreated plants; A2: Add the pretreated plant obtained in step A1 into distilled water in a ratio of 1 g:8 mL. Add 1-ethyl-3-methylimidazolium tetrafluoroborate ionic liquid into the distilled water in a concentration of 1 vol%. Heat to boiling and keep it slightly boiling at normal pressure. Distill for 4 h, collect the condensate, let it stand for stratification, take the upper oil phase, and dry it over anhydrous sodium sulfate to obtain plant essential oil.

[0048] The raw materials for preparing modified mannose include the following components in parts by weight: 8 parts of fumaric acid, 12 parts of 1-amino-1-deoxy-β-D-pyranose, and 15 parts of resveratrol.

[0049] The preparation method of modified mannose comprises the following steps: B1: Add 8 g of fumaric acid to 800 mL of DMF and mix well, heat to 50°C, add 12.8 g of EDC and 7.2 g of NHS, stir at 180 rpm for 2.5 h, add 12 g of 1-amino-1-deoxy-β-D-pyranose, react at 55°C and 550 rpm for 11 h, cool to room temperature, centrifuge at 8000 rpm for 18 min, wash the precipitate with DMF and acetone, and dry at 80°C to obtain fumaric acid-mannose; B2: The fumaric acid-mannose obtained in step B1 was dissolved in formamide to obtain 18 mg / mL fumaric acid-mannose solution, 15 g resveratrol was added to 60 mL thionyl chloride, reacted at 70°C for 1 h, added to the fumaric acid-mannose solution, 1.5 g DMAP was added, stirred at 650 rpm at 55°C for 2 h, allowed to stand at 4°C for 2.5 h, centrifuged at 5000 rpm for 18 min, the precipitate was washed with anhydrous ethanol and deionized water, and dried in vacuo at 45°C to obtain modified mannose.

[0050] The raw materials for preparing the modified carbomer include the following components in parts by weight: 5 parts of carbomer and 4 parts of citric acid.

[0051] The preparation method of modified carbomer comprises the following steps: C1: Add 4 g of citric acid to 40 mL of deionized water to prepare a 0.1 g / mL citric acid solution, add 5 g of carbomer, 6 g of DCC and 4 g of NHS to 1000 mL of DMSO, stir at 250 rpm for 5.5 h, filter, wash the filter cake with deionized water, freeze-dry at -20°C, add to a 0.1 g / mL citric acid solution, and stir at 55°C and 250 rpm for 3.5 h; C2: After the reaction in step C1 is completed, the mixture is allowed to stand at 4°C for 3 h, centrifuged at 5000 rpm for 25 min, the precipitate is washed with deionized water, and freeze-dried at -40°C to obtain modified carbomer.

[0052] This embodiment also provides a method for preparing the sleep-aiding plant essential oil composition, comprising the following steps: S1: Take 2.5 g of modified carbomer and add it to 18 mL of distilled water and mix well to obtain a modified carbomer solution. Add 1.4 g of modified mannose and 4 g of plant essential oil to 28 mL of deionized water, emulsify at 1400 rpm for 25 min, and drip into the modified carbomer solution at a rate of 1.2 mL / min. S2: After the step S1 is added, the mixture is stirred at 45°C and 550 r / min for 35 min, cooled to room temperature, centrifuged at 4000 r / min for 30 min, the precipitate is washed with anhydrous ethanol, and vacuum dried at 25°C to obtain a sleep-aiding plant essential oil composition.

[0053] The only difference between Comparative Example 1 and Example 1 is that the plant composition is composed of the following components in parts by weight: 20 parts of lavender, 12 parts of valerian, 8 parts of Michelia, and 6 parts of Herba Scutellariae.

[0054] The difference between Comparative Example 2 and Example 1 is that deionized water is used instead of the mixed acid solution and the honey aqueous solution.

[0055] The only difference between Comparative Example 3 and Example 1 is that Span 80 is used instead of modified mannose.

[0056] The only difference between Comparative Example 4 and Example 1 is that carbomer is used instead of modified carbomer.

[0057] Experimental Example 1: 1 g of the sleep-aiding plant essential oil composition prepared in Example 3 was mixed with 100 mL of deionized water, and ultrasonically dispersed at 100 W for 3 min. The mixture was pipetted onto a glass slide, and the morphological characteristics of the plant essential oil composition were observed using an electron microscope after the cover slip was replaced.

[0058] The results are as follows Figure 1 As shown, it can be observed from the microscope photograph that the particles of the plant essential oil composition prepared in Example 3 are complete and smooth, each particle is spherical, the particle dispersion is good, and there is very little agglomeration and adhesion.

[0059] Experimental Example 2: Plant essential oils were prepared according to the method of Example 2, recorded as Group A, and plant essential oils without adding semi-maple lotus, permanent flower or Swertia japonica were set up, recorded as Groups B, C and D. The plant essential oils prepared in each group were taken, and the Pittsburgh Sleep Quality Index (PSQI) scale was used to evaluate subjective sleep quality: it consists of 19 self-evaluation and 5 other-evaluation items, and the 19th self-evaluation item and 5 other-evaluation items are not scored. The remaining 18 scoring items are divided into 7 dimensions: sleep quality, sleep time, sleep time, sleep efficiency, sleep disorders, hypnotic drugs and daytime dysfunction. Each dimension is scored from 0 to 3, and the cumulative score of each dimension is the total score of PSQI. In the range of 0 to 21 points, a score of >7 points indicates poor sleep quality, and a score of ≤7 points indicates good sleep quality. When the score before and after the test drops by ≥3 points, it is considered that subjective sleep is improved. During the test, 200 volunteers aged 25-30 (all with a certain tendency to sleep disorders) were recruited and divided into 4 groups, 50 people in each group, half male and half female. The experimental period was 30 days. Every day when the volunteers fell asleep, 5 drops of plant essential oil were dripped into the headrest, and the average PSQI score before and after the test was recorded for 30 days. The results are as follows: Figure 2 shown.

[0060] Figure 2 The results showed that each group of plant essential oils had a certain sleep improvement effect, and the score reduction before and after the test was ≥3 points, and the sleep improvement effect was good. Among them, the sleep improvement effect of group A was the best, indicating that the plant essential oil composition of the present invention has a reasonable compatibility, synergistic effect, and effectively helps sleep.

[0061] Experimental Example 3: 10 g of the plant essential oil compositions prepared in Example 1 and Comparative Examples 1-4 were stored at 25°C under aerobic conditions for 30 days, and the weight was measured every 5 days. The results are as follows: Figure 3 shown.

[0062] Figure 3 The results showed that after storage at 25°C under aerobic conditions for 30 days, the weight reduction of the plant essential oil composition of Example 1 was less than that of Comparative Examples 1-4, and the essential oil release rate was low. The mixed plants used in Comparative Example 1 were different from those in the embodiments and were easier to volatilize, indicating that the plant composition of the present invention was reasonably compatible and had a good sustained-release effect. Comparative Example 2 did not use citric acid, tartaric acid and honey to pretreat the plants, and the extraction efficiency was low, which affected the extraction of effective active ingredients. Comparative Examples 3 and 4 used Span instead of modified mannose and carbomer instead of modified carbomer, respectively, and the encapsulation effect was reduced and the sustained-release function was reduced.

[0063] Experimental Example 4: The plant essential oil compositions obtained in Example 1 and Comparative Examples 1-4 were placed at 40° C. for 21 days, and then observed to see whether precipitation and color change occurred. The results are shown in Table 1.

[0064] Table 1:

[0065] The results in Table 1 show that the plant essential oil composition obtained in Example 1 has no precipitation and no color change after being placed at a high temperature of 40° C. for 21 days, has a long storage time and high stability.

[0066] Those skilled in the art should understand that the discussion of any of the above embodiments is merely illustrative and is not intended to imply that the scope of the present invention is limited to these examples. Under the concept of the present invention, the technical features in the above embodiments or different embodiments may be combined, the steps may be implemented in any order, and there are many other variations of the different aspects of the present invention as described above, which are not provided in detail for the sake of simplicity.

Claims

1. A sleep-aiding plant essential oil composition, characterized in that: The preparation raw materials include the following components in parts by weight: 3-5 parts of plant essential oil, 1-1.5 parts of modified mannose, and 2-3 parts of modified carbomer; The raw materials for preparing the plant essential oil include a plant mixture; the plant mixture is composed of the following components in parts by weight: 15-20 parts of lavender, 8-12 parts of valerian, 5-8 parts of Michelia, 4-6 parts of Herba Scutellariae, 4-6 parts of Helichrysum, 5-9 parts of Helichrysum, and 4-7 parts of Swertia japonica; The preparation method of the plant essential oil comprises the following steps: A1: Add citric acid and tartaric acid to deionized water and mix well to obtain a mixed acid solution, freeze-dry the plant mixture, crush and sieve, completely immerse in the mixed acid solution, stir, keep warm, filter, wash with deionized water, add to a honey aqueous solution and completely immerse, stir, keep warm, filter, wash with deionized water to obtain a pretreated plant; A2: Add the pretreated plant obtained in step A1 into distilled water, add 1-ethyl-3-methylimidazolium tetrafluoroborate ionic liquid into the distilled water, heat to boiling, and keep it slightly boiling under normal pressure, distill, collect condensate, let stand to separate, take the upper oil phase, and dry it with anhydrous sodium sulfate to obtain plant essential oil; The raw materials for preparing the modified mannose include the following components in parts by weight: 7-9 parts of fumaric acid, 10-14 parts of 1-amino-1-deoxy-β-D-pyranose, and 13-18 parts of resveratrol; The preparation method of the modified mannose comprises the following steps: B1: Add fumaric acid to DMF and mix well, heat, add EDC and NHS, stir, add 1-amino-1-deoxy-β-D-pyranose, react under stirring, cool, centrifuge, wash the precipitate, and dry to obtain fumaric acid-mannose; B2: dissolving the fumaric acid-mannose obtained in step B1 in formamide to obtain a fumaric acid-mannose solution, adding resveratrol to thionyl chloride, reacting at 70° C., adding the resveratrol to the fumaric acid-mannose solution, adding DMAP, stirring, standing, centrifuging, washing the precipitate, and vacuum drying to obtain modified mannose; The raw materials for preparing the modified carbomer include the following components in parts by weight: 4-6 parts of carbomer and 3-5 parts of citric acid; The preparation method of the modified carbomer comprises the following steps: C1: Carbomer, DCC and NHS were added to DMSO, stirred, filtered, the filter cake was washed with deionized water, freeze-dried, added to citric acid solution, and stirred for reaction; C2: After the reaction in step C1 is completed, the mixture is allowed to stand at 4°C, centrifuged, and the precipitate is washed with deionized water and freeze-dried to obtain modified carbomer.

2. The sleep-aiding plant essential oil composition according to claim 1, characterized in that: In step A1, the mass concentrations of citric acid and tartaric acid in deionized water are 80-100 g / L and 12-15 g / L respectively; and the mass concentration of the honey aqueous solution is 12-18 wt %.

3. The sleep-aiding plant essential oil composition according to claim 2, characterized in that: In step A2, the ratio of the pretreated plant to distilled water is 1 g: 6-9 mL; the concentration of 1-ethyl-3-methylimidazolium tetrafluoroborate ionic liquid in distilled water is 0.8-1.2 vol%.

4. The sleep-aiding plant essential oil composition according to claim 3, characterized in that: In step B1, the mass concentration of fumaric acid in DMF is 10 mg / mL; the mass ratio of fumaric acid, EDC and NHS is 1:1.6:0.

9.

5. The sleep-aiding plant essential oil composition according to claim 4, characterized in that: In step B2, the mass concentration of fumaric acid-mannose in formamide is 15-20 mg / mL; the usage ratio of resveratrol to thionyl chloride is 2 g:6-9 mL; and the mass ratio of resveratrol to DMAP is 10:

1.

6. The sleep-aiding plant essential oil composition according to claim 5, characterized in that: In step C1, the mass ratio of carbomer, DCC and NHS is 1:1.2:0.8; the mass concentration of DCC in DMSO is 6 mg / mL.

7. A method for preparing the sleep-aiding plant essential oil composition according to any one of claims 1 to 6, characterized in that: The following steps are involved: S1: taking modified carbomer and adding it into distilled water and mixing it evenly to obtain a modified carbomer solution, adding modified mannose and plant essential oil into deionized water, emulsifying them, and dropping them into the modified carbomer solution; S2: After the step S1 is completed, the mixture is stirred, cooled, centrifuged, and the precipitate is washed with anhydrous ethanol and vacuum dried to obtain a sleep-aiding plant essential oil composition.

8. The method for preparing the sleep-aiding plant essential oil composition according to claim 7, characterized in that: In step S1, the mass concentration of the modified carbomer in distilled water is 0.1-0.2 g / mL; the mass concentration of the modified mannose in deionized water is 0.04-0.06 g / mL.

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