A kind of agarwood-tangerine peel compound volatile oil for improving sleep and application thereof

Abstract

The invention discloses a kind of agarwood-tangerine peel compound volatile oil and its application for improving sleep, including: low-acid rapeseed oil, sweet orange essential oil, geranium essential oil, supercritical volatile agarwood essential oil and supercritical volatile tangerine peel essential oil; wherein, by volume ratio, low-acid rapeseed oil: sweet orange essential oil: geranium essential oil: supercritical volatile agarwood essential oil: supercritical volatile tangerine peel essential oil = 6-8: 9-11: 4-6: 0.5-1.5: 0.5-1.5; the compound volatile oil is administered by atomization sniffing, for improving sleep. The present invention extracts agarwood volatile oil and tangerine peel volatile oil by a specific process, and is proportioned in a specific ratio, effectively combining the traditional Chinese medicine functions of agarwood and tangerine peel for calming the nerves and regulating qi and resolving phlegm, can significantly improve the user's sleep condition, help the user to enter a deep sleep state faster, extend the deep sleep duration, thereby improving the overall sleep quality.

Description

Technical Field

[0001] The invention relates to the technical field of natural plant essential oil products, and in particular to a kind of agarwood-tangerine peel compound volatile oil for improving sleep and application thereof. Background Art

[0002] In the fast-paced and high-pressure modern society, insomnia has become a common problem that affects people's quality of life. Insomnia not only affects daytime work and study efficiency, but also causes a series of psychological and physical health problems in severe cases, such as depression, anxiety, cardiovascular disease, etc. Therefore, finding effective methods to treat insomnia has become an important issue in the field of public health.

[0003] Traditional treatments for insomnia mainly include drug therapy and behavioral therapy. However, long-term use of sleeping pills may lead to dependence and a series of side effects, such as daytime sleepiness, lack of concentration, memory loss, etc. As a result, people are gradually turning to safer and more natural therapies to improve sleep quality, including traditional Chinese medicine, aromatherapy, etc.

[0004] Among many natural therapies, plant compound volatile oils have attracted widespread attention due to their naturalness, low side effects, and ease of use. In particular, certain plant essential oils with sedative and tranquilizing effects, such as lavender and chamomile, have been proven to help improve sleep quality. However, there are many types of compound volatile oil products on the market, but few products are highly targeted and effective.

[0005] As traditional Chinese medicines, agarwood and tangerine peel have the effects of calming the mind and regulating qi, eliminating phlegm, and harmonizing the internal organs. Agarwood has long been used to treat neurasthenia and other symptoms, while tangerine peel is used to regulate the spleen and stomach and relieve chest tightness. However, there are relatively few studies on the application of the two in the field of compound volatile oils, especially in improving sleep.

[0006] Therefore, the present invention proposes an agarwood-tangerine peel compound volatile oil, aiming to combine the characteristics of agarwood and tangerine peel to develop a natural therapy that can both regulate qi and resolve phlegm and calm the mind, thereby providing a new option for improving insomnia. Summary of the invention

[0007] In order to overcome the shortcomings of the prior art, the present invention provides an agarwood-tangerine peel compound volatile oil for improving sleep and an application thereof, which is used to solve the limitations of the existing plant-based compound volatile oil in improving sleep effects, thereby achieving a more significant tranquilizing effect and enhancing the effect of improving insomnia.

[0008] To solve the above problems, the technical solution adopted by the present invention is as follows:

[0009] A composite agarwood-tangerine peel volatile oil for improving sleep, comprising: low-acid rapeseed oil, sweet orange essential oil, geranium essential oil, supercritical volatile agarwood essential oil and supercritical volatile tangerine peel essential oil;

[0010] Among them, calculated by volume ratio, the low-acid rapeseed oil: sweet orange essential oil: geranium essential oil: supercritical volatile agarwood essential oil: supercritical volatile tangerine peel essential oil = 6-8: 9-11: 4-6: 0.5-1.5: 0.5-1.5.

[0011] As a preferred embodiment of the present invention, the low-medium acid rapeseed oil is measured by gas chromatography, and the content of medium acid is less than 0.1% by mass percentage, the content of oleic acid in its fatty acid composition is 55%-65%, and the content of polyphenol antioxidants is 0.02%-0.04%;

[0012] The low-acid rapeseed oil is extracted from rapeseed by cold pressing, and the erucic acid content of the rapeseed is less than 2%.

[0013] As a preferred embodiment of the present invention, the sweet orange essential oil is measured by gas chromatography, and the content of d-limonene is 5%-15% and the content of β-pinene is 1%-5% by mass percentage;

[0014] The method comprises the following steps: extracting cold-pressed sweet orange essential oil from sweet orange peel by a low-temperature cold pressing method, measuring the cold-pressed sweet orange essential oil and placing it in a charging bottle of a molecular distillation device, setting the vacuum degree to 7-8 Torr and the molecular distillation temperature to 60-80° C., adjusting the rotor speed of a scraper to 250-350 r / min after the vacuum degree and the molecular distillation temperature reach the set values, opening a feed valve, feeding the cold-pressed sweet orange essential oil at a rate of 3.5-4.5 mL / min, performing molecular distillation, and collecting the distilled light phase component to obtain the sweet orange essential oil.

[0015] As a preferred embodiment of the present invention, the geranium essential oil is measured by gas chromatography, and the content of citronellol is 20%-30%, the content of geraniol is 10% to 15%, and the total content of citronellol and geraniol is 40%-50% by mass percentage;

[0016] The method comprises the following steps: weighing fresh geranium stems and leaves, placing them into a steam distillation device, adding deionized water, heating and distilling at 70-100° C. for 1.5-2.5 hours, and separating them through an oil-water separator to obtain geranium essential oil distillate;

[0017] Weigh the geranium essential oil distillate and place it in a flask, connect the flask to one end of the SDE simultaneous distillation extraction device, and use an electric heating jacket to heat it at 100-120° C., connect the other end of the SDE simultaneous distillation extraction device to a round-bottom flask filled with dichloromethane, heat the round-bottom flask in a water bath at 65-75° C., distill and extract for 3.5-4.5 hours, and collect the dichloromethane extract;

[0018] Anhydrous sodium sulfate is added to the dichloromethane extract to dry and filter it, and then concentrated by a rotary evaporator at 40-50° C. to obtain the geranium essential oil.

[0019] As a preferred embodiment of the present invention, the supercritical volatile agarwood essential oil is determined by gas chromatography, and the content of sesquiterpenoids is 20%-30%, the content of α-pinene is 5%-10%, and the content of oxidized linalool is 10%-15%, calculated by mass percentage.

[0020] As a preferred embodiment of the present invention, the supercritical volatile agarwood essential oil is extracted by supercritical CO2 extraction, and the extraction conditions include:

[0021] The agarwood wood is crushed to pass through a 40-60 mesh screen and placed in an extractor. After the CO2 is pressurized to 5-8MPa and cooled to -5°C to 0°C, the flow rate of CO2 entering the extractor is dynamically adjusted;

[0022] The primary extraction pressure is controlled at 22-25 MPa, the primary extraction temperature is 35-40°C, and the extraction is continued for 2-3 hours;

[0023] The pressure of the secondary extraction is controlled to be 25-30MPa, the temperature of the secondary extraction is 40-45°C, and the extraction is continued for 1-1.5 hours;

[0024] The primary separation pressure is controlled at 12-15MPa and the primary separation temperature is controlled at 30-35°C; the secondary separation pressure is controlled at 5-8MPa and the secondary separation temperature is controlled at 20-25°C.

[0025] As a preferred embodiment of the present invention, when dynamically adjusting the flow rate of CO2, it includes:

[0026] During primary extraction, the flow rate of CO2 is controlled at 15-20 kg / h, and during secondary extraction, the flow rate of CO2 is controlled at 25-30 kg / h.

[0027] As a preferred embodiment of the present invention, the supercritical volatile tangerine peel essential oil is determined by gas chromatography, and the content of d-limonene is 60%-80%, the content of geraniol is 5%-10%, and the content of decanal is 1%-3% by mass percentage.

[0028] As a preferred embodiment of the present invention, the supercritical volatile tangerine peel essential oil is extracted by supercritical CO2 extraction, and the extraction conditions include:

[0029] Crush the tangerine peel to pass through a 40-50 mesh sieve, and perform supercritical extraction for 2-3 hours;

[0030] The extraction pressure is controlled at 15-20MPa, the extraction temperature is controlled at 30-35°C, the CO2 flow rate is controlled at 10-12kg / h during the 0-1.5h of extraction, and the CO2 flow rate is controlled at 15-20kg / h during the 1.5-3h of extraction;

[0031] The primary separation pressure is controlled at 8-10MPa and the primary temperature is controlled at 30-40℃; the secondary separation pressure is controlled at 3-5MPa and the separation temperature is controlled at 20-25℃.

[0032] The invention discloses an application of agarwood-tangerine peel compound volatile oil for improving sleep, wherein the compound volatile oil is administered by atomization inhalation to improve sleep.

[0033] Compared with the prior art, the present invention has the following beneficial effects:

[0034] (1) Significantly improve sleep quality: Agarwood volatile oil and tangerine peel volatile oil are extracted through a specific process and mixed in a specific ratio, effectively combining the traditional Chinese medicine functions of agarwood and tangerine peel in calming the mind and regulating qi and resolving phlegm, which can significantly improve the user's sleep condition; in actual use, the compound volatile oil supplemented with specific low-acid rapeseed oil, sweet orange essential oil, and geranium essential oil can help users enter a deep sleep state faster, prolong the deep sleep duration, and thus improve the overall sleep quality;

[0035] (2) Through the detection of brain tissue neurotransmitters, the agarwood-tangerine peel volatile oil reduced the content of 5-HT in the hypothalamus and increased the content of 5-HT in the hippocampus, indicating that the agarwood-tangerine peel volatile oil has an effect on improving insomnia by affecting the content of neurotransmitters such as 5-HT in the body, thereby effectively regulating sleep and maintaining mental stability;

[0036] (3) It can be seen from the open field test in the examples that the agarwood-tangerine peel volatile oil significantly reduced the moving distance, maximum speed and average speed of the insomnia model rats, and increased the rest time, indicating that the agarwood-tangerine peel volatile oil can improve sleep and has a better sleep improvement effect than traditional drugs for treating insomnia (such as diazepam solution);

[0037] (4) High safety and low side effects: The present invention optimizes the extraction process and ratio to retain the effective ingredients of agarwood and tangerine peel to the maximum extent, while reducing the risk of potential irritation and adverse reactions; compared with traditional drug treatments, the compound volatile oil of the present invention is safer and more natural, has fewer side effects when used for a long time, and is suitable for people of all physiques;

[0038] (5) Wide applicability and convenient use: The compound volatile oil of the present invention is designed with user convenience in mind. It is easy to carry and use and can be used in a variety of ways, such as aromatherapy lamps, diffusers, and aromatherapy devices. It is not only suitable for home environments, but can also be used in offices and during travel to help improve sleep problems in different situations.

[0039] (6) Optimizing physiological and psychological conditions: In addition to improving sleep, the compound volatile oil of the present invention can also regulate people's emotions through its unique aroma, helping to relieve daytime stress and anxiety and improve overall mental health;

[0040] (7) High economic benefits: The compound volatile oil of the present invention, by combining the modern application of traditional Chinese herbal medicine with innovative technology, not only increases the added value of the product, but also helps to promote the culture of traditional Chinese medicine, thus having high economic benefits and market competitiveness in the health care product market;

[0041] (8) Scientific support: This invention is not only based on traditional Chinese medicine theory, but also combines modern scientific research. Through experiments, it verifies the efficacy and safety of compound volatile oil in improving sleep, providing a solid scientific basis for the application of the product.

[0042] The present invention is further described in detail below in conjunction with the accompanying drawings and specific embodiments. BRIEF DESCRIPTION OF THE DRAWINGS

[0043] Figure 1 This is a graph showing the results of measuring the rat's autonomic activity index according to an embodiment of the present invention;

[0044] Figure 2 A heat map of a rat movement path according to an embodiment of the present invention;

[0045] Figure 3 This is a graph showing the effect of sniffing volatile oil from an example of the present invention on the 5-HT content in the brain tissue of rats with liver depression and insomnia. DETAILED DESCRIPTION

[0046] The agarwood-tangerine peel compound volatile oil for improving sleep provided by the present invention comprises: low-acid rapeseed oil, sweet orange essential oil, geranium essential oil, supercritical volatile agarwood essential oil and supercritical volatile tangerine peel essential oil;

[0047] Among them, by volume ratio, low-acid rapeseed oil: sweet orange essential oil: geranium essential oil: supercritical volatile agarwood essential oil: supercritical volatile tangerine peel essential oil = 6-8: 9-11: 4-6: 0.5-1.5: 0.5-1.5.

[0048] Preferably, by volume ratio, low-acid rapeseed oil: sweet orange essential oil: geranium essential oil: supercritical volatile agarwood essential oil: supercritical volatile tangerine peel essential oil = 8:11:6:1.5:1.5.

[0049] Preferably, the low-medium acid rapeseed oil is determined by gas chromatography, and the medium acid content is less than 0.1% by mass percentage, the oleic acid content in its fatty acid composition is 55%-65%, and the content of polyphenol antioxidants is 0.02%-0.04%;

[0050] Among them, low-acid rapeseed oil is extracted from rapeseed by cold pressing, and the erucic acid content of rapeseed is less than 2%.

[0051] Specifically, the content of mesogenic acid below 0.1% reduces the irritation of the compound volatile oil, improves the comfort when used by inhalation and sniffing, and helps users relax and improve sleep quality. Oleic acid with a content of 55%-65% helps maintain the stability of the compound volatile oil during atomization, ensuring that the sleep-inducing ingredients are evenly released and fully absorbed, thereby effectively improving sleep quality. Polyphenol antioxidants with a content of 0.02%-0.04% can reduce the oxidative degradation of active ingredients during atomization, ensuring that the sleep-inducing effect of the compound volatile oil is long-lasting and stable when inhaled and sniffed.

[0052] Specifically, extraction through the cold pressing method can effectively retain the natural plant sterols and antioxidant substances in rapeseed, help maintain the stability of the compound volatile oil during atomization and inhalation, and enhance the sleep-inducing effect.

[0053] More preferably, by adding an appropriate amount of natural antioxidants (such as rosemary extract) during the cold pressing extraction process, the stability of the low-acid rapeseed oil can be further improved, thereby ensuring the complete release of volatile components during the atomization and sniffing process, thereby enhancing the sedative and relaxing effects.

[0054] Preferably, the sweet orange essential oil is determined by gas chromatography, and the content of d-limonene is 5%-15% and the content of β-pinene is 1%-5% by mass percentage;

[0055] The method comprises the following steps: extracting cold-pressed sweet orange essential oil from sweet orange peel by a low-temperature cold pressing method, measuring 40-60 mL of the cold-pressed sweet orange essential oil and placing it in a charging bottle of a molecular distillation device, setting the vacuum degree to 7-8 Torr, and the molecular distillation temperature to 60-80° C., adjusting the rotor speed of a scraper to 250-350 r / min after the vacuum degree and the molecular distillation temperature reach the set values, opening a feed valve, feeding the cold-pressed sweet orange essential oil at a rate of 3.5-4.5 mL / min, performing molecular distillation, and collecting the distilled light phase component to obtain the sweet orange essential oil.

[0056] Specifically, 5%-15% d-limonene can soothe the nervous system and reduce anxiety through sniffing, thereby improving the sleep-aiding effect. 1%-5% β-pinene can help relax the respiratory tract and reduce tension when atomized and sniffed, and further enhance the sleep-aiding effect through olfactory stimulation, thereby reducing the frequency of waking up at night.

[0057] More preferably, the content of β-pinene is 3%-5%. 3%-5% β-pinene can cooperate with d-limonene to exert a soothing effect, provide a more obvious sedative effect, and help accelerate the process of falling asleep.

[0058] Specifically, the low-temperature cold pressing method combined with molecular distillation technology, and based on the above-mentioned combination of extraction parameters, can effectively extract active ingredients such as d-limonene and β-pinene in sweet orange peel that have sedative and sleep-inducing effects.

[0059] Preferably, the geranium essential oil is determined by gas chromatography, and the content of citronellol is 20%-30%, the content of geraniol is 10% to 15%, and the total content of citronellol and geraniol is 40%-50% by mass percentage;

[0060] The method comprises the following steps: weighing 1.5-2.5 kg of fresh geranium stems and leaves, loading them into a 20 L steam distillation device, adding 4-6 L of deionized water, heating and distilling at 70-100° C. for 1.5-2.5 h, and separating them through an oil-water separator to obtain geranium essential oil distillate;

[0061] Weigh 450-550 mL of geranium essential oil distillate and place it in a 1 L flask, connect the 1 L flask to one end of a SDE simultaneous distillation extraction device, and heat it at 100-120° C. using an electric heating jacket, connect the other end of the SDE simultaneous distillation extraction device to a 100 mL round-bottom flask filled with 25-35 ml of dichloromethane, heat the round-bottom flask in a 65-75° C. water bath, distill and extract for 3.5-4.5 hours, and collect the dichloromethane extract;

[0062] Anhydrous sodium sulfate is added to the dichloromethane extract to dry and filter, and then concentrated by a rotary evaporator at 40-50° C. to obtain geranium essential oil.

[0063] Specifically, 20%-30% citronellol, administered by atomization and sniffing, can relieve tension through the olfactory system, promote physical and mental relaxation, and thus effectively improve sleep quality. 10% to 15% geraniol can promote neuroregulation through atomization and sniffing, reduce the number of awakenings at night, and improve overall sleep quality. A total content of 40%-50% citronellol and geraniol can produce a synergistic sedative effect when atomized and sniffed, helping users relieve stress and anxiety and enhance the experience of falling asleep.

[0064] Specifically, the above extraction process can effectively retain the citronellol and geraniol components in geranium essential oil, ensuring that the soothing aroma is released during the atomization and sniffing process, helping to relax the nerves and promote sleep. In addition, it can also remove rough impurities and improve the purity of the essential oil, making it gentler on the respiratory system during atomization and sniffing, thereby enhancing the overall sleep-inducing effect of the compound volatile oil.

[0065] Preferably, the supercritical volatile agarwood essential oil is determined by gas chromatography, and the content of sesquiterpenoids is 20%-30%, the content of α-pinene is 5%-10%, and the content of oxidized linalool is 10%-15%, calculated by mass percentage.

[0066] More preferably, the supercritical volatile agarwood essential oil is extracted by supercritical CO2 extraction, and the extraction conditions include:

[0067] The agarwood wood is crushed to pass through a 40-60 mesh screen and placed in an extractor. After the CO2 is pressurized to 5-8MPa and cooled to -5°C to 0°C, the flow rate of CO2 entering the extractor is dynamically adjusted;

[0068] The primary extraction pressure is controlled at 22-25 MPa, the primary extraction temperature is 35-40°C, and the extraction is continued for 2-3 hours;

[0069] The pressure of the secondary extraction is controlled to be 25-30MPa, the temperature of the secondary extraction is 40-45°C, and the extraction is continued for 1-1.5 hours;

[0070] The primary separation pressure is controlled at 12-15MPa and the primary separation temperature is controlled at 30-35°C; the secondary separation pressure is controlled at 5-8MPa and the secondary separation temperature is controlled at 20-25°C.

[0071] Specifically, 20%-30% of sesquiterpenoids are administered by atomization and sniffing, which has a calming and soothing effect, helps reduce the user's anxiety and improves the quality of sleep. 5% to 10% of α-pinene is administered by atomization and sniffing, which can help users relax their respiratory tract and relieve nervous tension, further enhancing the sleep-aiding effect. 10%-15% of oxidized linalool is administered by atomization and sniffing, which can activate the olfactory nerves and induce relaxation and soothing reactions, thereby effectively reducing the number of awakenings at night and improving the quality of deep sleep.

[0072] Specifically, pressurizing CO2 to 5-8MPa and cooling it to -5℃ to 0℃ ensures that CO2 is in a liquid state before entering the extractor, thereby optimizing the extraction efficiency. The parameter setting of the primary extraction can ensure that the sleep-inducing ingredients such as sesquiterpenes and oxidized linalool are fully extracted during the extraction process. The parameter setting of the secondary extraction can ensure that more high-molecular-weight sedative ingredients are extracted to further enhance the sleep-inducing effect during atomization and sniffing. After the extraction is completed, a two-stage decompression separation is used to separate different volatile components and ensure the purity and stability of the final agarwood essential oil.

[0073] More preferably, when dynamically adjusting the flow rate of CO2, it includes:

[0074] During primary extraction, the flow rate of CO2 is controlled at 15-20 kg / h, and during secondary extraction, the flow rate of CO2 is controlled at 25-30 kg / h.

[0075] Specifically, a CO2 flow rate of 15-20 kg / h is used to extract volatile components with lower molecular weight, and a CO2 flow rate of 25-30 kg / h is used to extract active components with higher molecular weight, ensuring sufficient release of sedative components in the final extract.

[0076] Preferably, the supercritical volatile tangerine peel essential oil is determined by gas chromatography, and the content of d-limonene is 60%-80%, the content of geraniol is 5%-10%, and the content of decanal is 1%-3%, by mass percentage.

[0077] More preferably, the supercritical volatile tangerine peel essential oil is extracted by supercritical CO2 extraction, and the extraction conditions include:

[0078] Crush the tangerine peel until it passes through a 40-50 mesh sieve, and perform supercritical extraction for 2-3 hours;

[0079] The extraction pressure is controlled at 15-20MPa, the extraction temperature is controlled at 30-35°C, the CO2 flow rate is controlled at 10-12kg / h during the 0-1.5h of extraction, and the CO2 flow rate is controlled at 15-20kg / h during the 1.5-3h of extraction;

[0080] The primary separation pressure is controlled at 8-10MPa and the primary temperature is controlled at 30-40℃; the secondary separation pressure is controlled at 3-5MPa and the separation temperature is controlled at 20-25℃.

[0081] Specifically, 60%-80% d-limonene administered by atomization and sniffing can effectively reduce anxiety and stress, thereby promoting relaxation and sleep. 5%-10% geraniol administered by atomization and sniffing can produce a mild soothing effect, helping users fall asleep quickly and improve sleep quality. 1%-3% decanal can bring a soft aroma when atomized and sniffed, enhance the comfort of breathing, further support the relaxation of the nervous system, and reduce the frequency of nighttime awakenings.

[0082] Specifically, at the beginning of extraction, a lower CO2 flow rate is used in combination with a specific extraction pressure and extraction temperature to extract light molecular volatile components such as limonene. At the end of extraction, the CO2 flow rate is increased to extract higher molecular weight sedative components such as geraniol and decanal, ensuring the comprehensive extraction of sleep-inducing active ingredients in the essential oil. Secondary separation is to obtain high-purity tangerine peel essential oil, thereby optimizing the sleep-inducing effect of atomized inhalation administration.

[0083] The application of the agarwood-tangerine peel compound volatile oil for improving sleep provided by the present invention is to administer the compound volatile oil by atomization inhalation to improve sleep.

[0084] The following examples are provided to further illustrate the present invention, but the scope of the present invention is not limited thereto.

[0085] In this example, rats with liver depression type insomnia in TCM syndrome classification were used as model animals to study the efficacy of the compound volatile oil containing the agarwood-tangerine peel drug pair in improving insomnia, and the efficacy and mechanism of action of the drug pair were studied.

[0086] Embodiment 1

[0087] By volume ratio, low-acid rapeseed oil: sweet orange essential oil: geranium essential oil: supercritical volatile agarwood essential oil: supercritical volatile tangerine peel essential oil = 8:11:6:1.5:1.5.

[0088] Supercritical volatile agarwood essential oil was determined by gas chromatography, and the content of sesquiterpenoids was 20%-30%, the content of α-pinene was 5%-10%, and the content of oxidized linalool was 10%-15%, calculated by mass percentage.

[0089] Supercritical volatile agarwood essential oil is extracted by supercritical CO2 extraction, and the extraction conditions include:

[0090] The agarwood wood was crushed to pass through a 40-mesh screen and placed in an extractor. After the CO2 was pressurized to 5MPa and cooled to -5°C, the flow rate of CO2 entering the extractor was dynamically adjusted.

[0091] The primary extraction pressure was controlled to be 22 MPa, the primary extraction temperature was controlled to be 35°C, and the extraction was continued for 2 hours;

[0092] The pressure of the secondary extraction was controlled to be 25 MPa, the temperature of the secondary extraction was controlled to be 40°C, and the extraction was continued for 1 hour;

[0093] The primary separation pressure is controlled at 12MPa and the primary separation temperature is controlled at 30°C; the secondary separation pressure is controlled at 5MPa and the secondary separation temperature is controlled at 20°C.

[0094] When dynamically adjusting the flow rate of CO2, it includes:

[0095] During the primary extraction, the flow rate of CO2 was controlled at 15 kg / h, and during the secondary extraction, the flow rate of CO2 was controlled at 25 kg / h.

[0096] Supercritical volatile tangerine peel essential oil is determined by gas chromatography, and the content of d-limonene is 60%-80%, the content of geraniol is 5%-10%, and the content of decanal is 1%-3% by mass percentage.

[0097] Supercritical volatile tangerine peel essential oil is extracted by supercritical CO2 extraction, and the extraction conditions include:

[0098] Crush the tangerine peel until it passes through a 40-mesh sieve and perform supercritical extraction for 2 h;

[0099] The extraction pressure was controlled at 15 MPa, the extraction temperature was controlled at 30°C, the CO2 flow rate was controlled at 10 kg / h during the 0-1.5 h of extraction, and the CO2 flow rate was controlled at 15 kg / h during the 1.5-3 h of extraction;

[0100] The primary separation pressure is controlled at 8MPa and the primary temperature is controlled at 30°C; the secondary separation pressure is controlled at 3MPa and the separation temperature is controlled at 20°C.

[0101] The low-medium acid rapeseed oil was determined by gas chromatography. The content of medium acid was less than 0.1% by mass, the content of oleic acid in its fatty acid composition was 55%-65%, and the content of polyphenol antioxidants was 0.02%-0.04%;

[0102] Among them, low-acid rapeseed oil is extracted from rapeseed by cold pressing, and the erucic acid content of rapeseed is less than 2%.

[0103] The sweet orange essential oil was determined by gas chromatography, and the content of d-limonene was 5%-15% and the content of β-pinene was 1%-5% by mass percentage;

[0104] Among them, cold-pressed sweet orange essential oil is extracted from sweet orange peel by a low-temperature cold pressing method, 40 mL of cold-pressed sweet orange essential oil is measured and placed in a charging bottle of a molecular distillation device, the vacuum degree is set to 7 Torr, and the molecular distillation temperature is set to 60°C. After the vacuum degree and the molecular distillation temperature reach the set values, the speed of the scraper rotor is adjusted to 250 r / min, the feed valve is opened, the cold-pressed sweet orange essential oil is fed at a rate of 3.5 mL / min, molecular distillation is performed, and the distilled light phase components are collected to obtain sweet orange essential oil.

[0105] The geranium essential oil was determined by gas chromatography, and the content of citronellol was 20%-30%, the content of geraniol was 10% to 15%, and the total content of citronellol and geraniol was 40%-50% by mass percentage;

[0106] 1.5 kg of fresh geranium stems and leaves were weighed and placed in a 20 L steam distillation device, 4 L of deionized water was added, heated and distilled at 70 ° C for 1.5 h, and separated by an oil-water separator to obtain geranium essential oil distillate;

[0107] Weigh 450 mL of geranium essential oil distillate and place it in a 1 L flask. Connect the 1 L flask to one end of the SDE simultaneous distillation extraction device and heat it at 100 ° C using an electric heating mantle. Connect the other end of the SDE simultaneous distillation extraction device to a 100 mL round-bottom flask filled with 25 ml of dichloromethane. Heat the round-bottom flask in a 65 ° C water bath and distill and extract for 3.5 hours, and collect the dichloromethane extract.

[0108] Anhydrous sodium sulfate was added to the dichloromethane extract to dry and filter it, and then concentrated by a rotary evaporator at 40° C. to obtain geranium essential oil.

[0109] Embodiment 2

[0110] By volume ratio, low-acid rapeseed oil: sweet orange essential oil: geranium essential oil: supercritical volatile agarwood essential oil: supercritical volatile tangerine peel essential oil = 6:9:4:0.5:0.5.

[0111] Supercritical volatile agarwood essential oil was determined by gas chromatography, and the content of sesquiterpenoids was 20%-30%, the content of α-pinene was 5%-10%, and the content of oxidized linalool was 10%-15%, calculated by mass percentage.

[0112] Supercritical volatile agarwood essential oil is extracted by supercritical CO2 extraction, and the extraction conditions include:

[0113] The agarwood wood was crushed to pass through a 60-mesh screen and placed in an extractor. After the CO2 was pressurized to 8MPa and cooled to 0°C, the flow rate of CO2 entering the extractor was dynamically adjusted.

[0114] The primary extraction pressure was controlled to be 25 MPa, the primary extraction temperature was controlled to be 40°C, and the extraction was continued for 3 hours;

[0115] The pressure of the secondary extraction was controlled to be 30 MPa, the temperature of the secondary extraction was controlled to be 45°C, and the extraction was continued for 1.5 hours;

[0116] The primary separation pressure was controlled at 15 MPa and the primary separation temperature was controlled at 35°C; the secondary separation pressure was controlled at 8 MPa and the secondary separation temperature was controlled at 25°C.

[0117] When dynamically adjusting the flow rate of CO2, it includes:

[0118] During the primary extraction, the flow rate of CO2 was controlled at 20 kg / h, and during the secondary extraction, the flow rate of CO2 was controlled at 30 kg / h.

[0119] Supercritical volatile tangerine peel essential oil is determined by gas chromatography, and the content of d-limonene is 60%-80%, the content of geraniol is 5%-10%, and the content of decanal is 1%-3% by mass percentage.

[0120] Supercritical volatile tangerine peel essential oil is extracted by supercritical CO2 extraction, and the extraction conditions include:

[0121] Crush the tangerine peel until it passes through a 50-mesh sieve and perform supercritical extraction for 3 h;

[0122] The extraction pressure was controlled at 20 MPa, the extraction temperature was controlled at 35°C, the CO2 flow rate was controlled at 12 kg / h during the extraction period of 0-1.5 h, and the CO2 flow rate was controlled at 20 kg / h during the extraction period of 1.5-3 h;

[0123] The primary separation pressure is controlled at 10MPa and the primary temperature is controlled at 40°C; the secondary separation pressure is controlled at 5MPa and the separation temperature is controlled at 25°C.

[0124] The low-medium acid rapeseed oil was determined by gas chromatography. The content of medium acid was less than 0.1% by mass, the content of oleic acid in its fatty acid composition was 55%-65%, and the content of polyphenol antioxidants was 0.02%-0.04%;

[0125] Among them, low-acid rapeseed oil is extracted from rapeseed by cold pressing, and the erucic acid content of rapeseed is less than 2%.

[0126] The sweet orange essential oil was determined by gas chromatography, and the content of d-limonene was 5%-15% and the content of β-pinene was 1%-5% by mass percentage;

[0127] Among them, cold-pressed sweet orange essential oil is extracted from sweet orange peel by a low-temperature cold pressing method, 60 mL of cold-pressed sweet orange essential oil is measured and placed in a charging bottle of a molecular distillation device, the vacuum degree is set to 8 Torr, and the molecular distillation temperature is set to 80°C. After the vacuum degree and the molecular distillation temperature reach the set values, the speed of the scraper rotor is adjusted to 350 r / min, the feed valve is opened, the cold-pressed sweet orange essential oil is fed at a rate of 4.5 mL / min, molecular distillation is performed, and the distilled light phase components are collected to obtain sweet orange essential oil.

[0128] The geranium essential oil was determined by gas chromatography, and the content of citronellol was 20%-30%, the content of geraniol was 10% to 15%, and the total content of citronellol and geraniol was 40%-50% by mass percentage;

[0129] 2.5 kg of fresh geranium stems and leaves were weighed and placed in a 20 L steam distillation device, 6 L of deionized water was added, and the mixture was heated and distilled at 100 ° C for 2.5 h, and separated by an oil-water separator to obtain geranium essential oil distillate;

[0130] Weigh 550 mL of geranium essential oil distillate and place it in a 1 L flask. Connect the 1 L flask to one end of the SDE simultaneous distillation extraction device and heat it at 120 ° C using an electric heating mantle. Connect the other end of the SDE simultaneous distillation extraction device to a 100 mL round-bottom flask filled with 35 ml of dichloromethane. Heat the round-bottom flask in a 75 ° C water bath. Distill and extract for 4.5 hours, and collect the dichloromethane extract.

[0131] Anhydrous sodium sulfate was added to the dichloromethane extract to dry and filter it, and then concentrated by a rotary evaporator at 50° C. to obtain geranium essential oil.

[0132] Modeling of insomnia rats and the administration process of compound volatile oil in treatment

[0133] The blank group had no external stimulation, and the other groups were respectively bound with medical tape to restrict their forelimbs, and insisted on clamping the rat's tail every day, the tail was 1 / 3 of the proximal end, for 45 minutes a day, so that it was in a fighting state, without breaking the skin and bleeding, for 20 consecutive days. From the 16th day of model establishment, the rats in the control group, the positive group and each example group were injected with 450 mg / kg of para-chlorophenylalanine (PCPA) dissolved in physiological saline for 2 consecutive days. From the 7th day of tail clamping stimulation, the positive group was gavaged with 1 mg / kg of diazepam solution dissolved in physiological saline; the blank group and the control group were gavaged with physiological saline of the same volume as the diazepam solution; the example group was given the agarwood-tangerine peel compound volatile oil of Examples 1 and 2, and the atomized inhalation administration was performed through an aromatherapy olfactory device once a day for 14 consecutive days.

[0134] The main body of the aromatherapy olfactory device is composed of a transparent plexiglass box with a size of 80*80*65cm and a lid and four transparent plexiglass boxes with a size of 30*30*30cm. The small boxes are evenly placed at the bottom of the large box, and the aromatherapy atomizer for holding the compound volatile oil is placed in the center of the large box. The rat is placed in the aromatherapy olfactory device, and 1ml of the compound volatile oil of Examples 1 and 2 is added to the spray pot of the aromatherapy atomizer, and water is added to the maximum scale of 8ml. After the aromatherapy atomizer is started for about 45 minutes, the spray pot of the aromatherapy atomizer no longer produces mist. At this time, the volatile oil in the aromatherapy atomizer is basically atomized completely, without residue or a little residue at the bottom. At this time, turn off the aromatherapy atomizer switch, wait until the compound volatile oil in the aromatherapy olfactory device is completely or almost tasteless, open the aromatherapy olfactory device, take out the rat, and the sniffing is completed. The sniffing time of each embodiment group is 1h. Test after sniffing.

[0135] Open field test

[0136] The rat open field test was conducted within 1 hour after the end of drug administration. The light in the laboratory was kept constant and dim, with the minimum brightness that could distinguish the subtle activities of rats at a distance of 1.5 cm as the standard. The room temperature was 20±1℃, the humidity was 60%~70%, and the laboratory was kept quiet. The bottom of the open field was black, and a camera was placed directly above the central area of ​​the open field. The rats were first placed in the laboratory to adapt for 10 minutes. After the experiment began, the rats were quickly placed alone in the center of the open field, with their heads fixed to one side. After the rats were released, the video analysis system was immediately started to automatically collect videos. Each rat was adapted to the open field box for 3 minutes, and the measurement time was 5 minutes. After the measurement, the fecal particles and urine left by the rats were removed, and the environment in the box was cleaned with low-concentration alcohol. After the alcohol evaporated and became odorless, the next test was carried out. Less than 2cm / s was considered resting, and greater than 20cm / s was considered fast movement. The single target tracking mode was used for measurement, and the maximum speed, average speed, moving speed, rest time, low-speed movement time, and high-speed movement time of each rat were recorded.

[0137] From Table 1, Figure 1 , Figure 2 It can be seen that compared with the blank group, the control group and the positive group, the embodiment group can significantly reduce the moving distance (Dist), maximum speed (V.max) and average speed (V.mean) of rats in the open field test, and increase the rest time (Res.T) of rats in the open field test, indicating that agarwood-tangerine peel volatile oil can improve the insomnia symptoms of rats. Figure 1 The results were expressed as mean ± standard error and statistically processed by t test. , , compared with the control group, , .

[0138] Table 1 Results of determination of related indicators of rats' spontaneous activities ( )

[0139]

[0140] Note: Compared with the blank group, , , compared with the control group, , .

[0141] Detection of neurotransmitters in brain tissue

[0142] After the treatment, the rats in each group were killed, and the hypothalamus and hippocampus tissues of the rats were taken out. The 5-hydroxytryptamine (5-HT) content in the hypothalamus and hippocampus tissues of the rats in each group was determined by enzyme-linked immunosorbent assay. 5-HT has the function of regulating sleep and maintaining mental stability. The content of 5-HT in the hypothalamus and hippocampus tissues can reflect the mental and neurological state of the organism. Table 2 shows the statistical results of the determination of 5-HT content in the hypothalamus and hippocampus tissues of the rats in each group.

[0143] As can be seen from Table 2, compared with the control group, the 5-HT content in the hypothalamus of the rats in the positive group and the embodiment group was reduced, and the 5-HT content in the hippocampus was increased. This shows that the volatile oil of agarwood-tangerine peel can effectively regulate sleep and maintain mental stability by affecting the content of neurotransmitters such as 5-HT in the body, and has the effect of treating insomnia. Figure 3 The results were expressed as mean ± standard error and statistically processed by t test. , , compared with the control group, , .

[0144] Table 2 Effects of volatile oil inhalation on 5-HT content in brain tissue of insomnia rats ( )

[0145]

[0146] Note: Compared with the blank group, , , compared with the control group, , .

[0147] in conclusion

[0148] (1) It can be seen from the above open field test that the agarwood-tangerine peel volatile oil significantly reduced the moving distance, maximum speed and average speed of the insomnia model rats, and increased the rest time, indicating that the agarwood-tangerine peel volatile oil can improve sleep and has a better effect on improving sleep than traditional drugs for treating insomnia (such as diazepam solution).

[0149] (2) Through the detection of neurotransmitters in brain tissue, the agarwood-tangerine peel volatile oil reduced the content of 5-HT in the hypothalamus and increased the content of 5-HT in the hippocampus, indicating that the agarwood-tangerine peel volatile oil can effectively regulate sleep and maintain mental stability by affecting the content of neurotransmitters such as 5-HT in the body, and has the effect of improving insomnia.

[0150] The above-mentioned embodiments are only preferred embodiments of the present invention and cannot be used to limit the scope of protection of the present invention. Any non-substantial changes and substitutions made by technicians in this field on the basis of the present invention shall fall within the scope of protection required by the present invention.

Claims

1. A kind of agarwood-tangerine peel compound volatile oil for improving sleep, characterized in that: It is composed of the following components: low-medium acid rapeseed oil, sweet orange essential oil, geranium essential oil, supercritical volatile agarwood essential oil and supercritical volatile tangerine peel essential oil; Wherein, by volume ratio, the low-acid rapeseed oil: sweet orange essential oil: geranium essential oil: supercritical volatile agarwood essential oil: supercritical volatile tangerine peel essential oil = 6-8: 9-11: 4-6: 0.5-1.5: 0.5-1.5; Wherein, the low-medium acid rapeseed oil is measured by gas chromatography, and the content of medium acid is less than 0.1% by mass.

2. The agarwood-tangerine peel compound volatile oil for improving sleep according to claim 1, characterized in that: The low-acid rapeseed oil is measured by gas chromatography, and the content of oleic acid in its fatty acid composition is 55%-65% by mass, and the content of polyphenol antioxidants is 0.02%-0.04% by mass; The low-acid rapeseed oil is extracted from rapeseed by cold pressing, and the erucic acid content of the rapeseed is less than 2%.

3. The agarwood-tangerine peel compound volatile oil for improving sleep according to claim 1, characterized in that, The sweet orange essential oil is measured by gas chromatography, and the content of d-limonene is 5%-15% and the content of β-pinene is 1%-5% by mass percentage; The method comprises the following steps: extracting cold-pressed sweet orange essential oil from sweet orange peel by a low-temperature cold pressing method, measuring the cold-pressed sweet orange essential oil and placing it in a charging bottle of a molecular distillation device, setting the vacuum degree to 7-8 Torr and the molecular distillation temperature to 60-80° C., adjusting the rotor speed of a scraper to 250-350 r / min after the vacuum degree and the molecular distillation temperature reach the set values, opening a feed valve, feeding the cold-pressed sweet orange essential oil at a rate of 3.5-4.5 mL / min, performing molecular distillation, and collecting the distilled light phase component to obtain the sweet orange essential oil.

4. The agarwood-tangerine peel compound volatile oil for improving sleep according to claim 1, characterized in that: The geranium essential oil is measured by gas chromatography, and the content of citronellol is 20%-30%, the content of geraniol is 10% to 15%, and the total content of citronellol and geraniol is 40%-50% by mass percentage; The method comprises the following steps: weighing fresh geranium stems and leaves, placing them into a steam distillation device, adding deionized water, heating and distilling at 70-100° C. for 1.5-2.5 hours, and separating them through an oil-water separator to obtain geranium essential oil distillate; Weigh the geranium essential oil distillate and place it in a flask, connect the flask to one end of the SDE simultaneous distillation extraction device, and use an electric heating jacket to heat it at 100-120° C., connect the other end of the SDE simultaneous distillation extraction device to a round-bottom flask filled with dichloromethane, heat the round-bottom flask in a water bath at 65-75° C., distill and extract for 3.5-4.5 hours, and collect the dichloromethane extract; Anhydrous sodium sulfate is added to the dichloromethane extract to dry and filter it, and then concentrated by a rotary evaporator at 40-50° C. to obtain the geranium essential oil.

5. The agarwood-tangerine peel compound volatile oil for improving sleep according to any one of claims 1 to 4, characterized in that: The supercritical volatile agarwood essential oil is determined by gas chromatography, and the content of sesquiterpenoids is 20%-30%, the content of α-pinene is 5%-10%, and the content of oxidized linalool is 10%-15% by mass percentage.

6. The agarwood-tangerine peel compound volatile oil for improving sleep according to claim 5, characterized in that: The supercritical volatile agarwood essential oil is extracted by supercritical CO2 extraction, and the extraction conditions include: The agarwood wood is crushed to pass through a 40-60 mesh screen and placed in an extractor. After the CO2 is pressurized to 5-8MPa and cooled to -5°C to 0°C, the flow rate of CO2 entering the extractor is dynamically adjusted; The primary extraction pressure is controlled at 22-25 MPa, the primary extraction temperature is 35-40°C, and the extraction is continued for 2-3 hours; The pressure of the secondary extraction is controlled to be 25-30MPa, the temperature of the secondary extraction is 40-45°C, and the extraction is continued for 1-1.5 hours; The primary separation pressure is controlled at 12-15MPa and the primary separation temperature is controlled at 30-35°C; the secondary separation pressure is controlled at 5-8MPa and the secondary separation temperature is controlled at 20-25°C.

7. The agarwood-tangerine peel compound volatile oil for improving sleep according to claim 6, characterized in that: When dynamically adjusting the flow rate of CO2, it includes: During primary extraction, the flow rate of CO2 is controlled at 15-20 kg / h, and during secondary extraction, the flow rate of CO2 is controlled at 25-30 kg / h.

8. The agarwood-tangerine peel compound volatile oil for improving sleep according to claim 7, characterized in that: The supercritical volatile tangerine peel essential oil is measured by gas chromatography, and the content of d-limonene is 60%-80%, the content of geraniol is 5%-10%, and the content of decanal is 1%-3% by mass percentage.

9. The agarwood-tangerine peel compound volatile oil for improving sleep according to claim 8, characterized in that: The supercritical volatile tangerine peel essential oil is extracted by supercritical CO2 extraction, and the extraction conditions include: Crush the tangerine peel to pass through a 40-50 mesh sieve, and perform supercritical extraction for 2-3 hours; The extraction pressure is controlled at 15-20MPa, the extraction temperature is controlled at 30-35°C, the CO2 flow rate is controlled at 10-12kg / h during the 0-1.5h of extraction, and the CO2 flow rate is controlled at 15-20kg / h during the 1.5-3h of extraction; The primary separation pressure is controlled at 8-10MPa and the primary temperature is controlled at 30-40℃; the secondary separation pressure is controlled at 3-5MPa and the separation temperature is controlled at 20-25℃.

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