Wormwood composition and preparation method thereof

Abstract

The invention provides a wormwood composition and a preparation method thereof, and belongs to the technical field of medicines. The preparation method comprises the following steps: carrying out supercritical fluid extraction and molecular distillation on traditional Chinese medicine powder and Qichun Dragon Boat Festival moxa to obtain traditional Chinese medicine essential oil, carrying out solid extraction to obtain a water-soluble active component and an oil-soluble active component, embedding the water-soluble active component to obtain nanoscale capsule powder, adding the nanoscale capsule powder, the oil-soluble active component and an oleophylic emulsifier into the traditional Chinese medicine essential oil, and uniformly mixing to obtain the traditional Chinese medicine essential oil. The preparation method comprises the following steps: dropwise adding an aqueous solution containing a hydrophilic emulsifier and sodium alginate, emulsifying, curing, preparing blasting beads, adding the blasting beads, an atomizing agent and a surfactant into a chitosan solution, mixing, cross-linking, and adjusting the water content, so as to prepare the wormwood composition, in a low-temperature heating process, the blasting beads can be promoted to be broken, contents can be promoted to escape, aerosol is formed along with volatilization of water vapor and traditional Chinese medicine essential oil, and the wormwood composition can be used for preventing and treating diseases. The components are purer, PM2.5 particles are not contained, harm to human health is avoided, the pesticide effect is greatly improved, and the composition is safer, healthier, green and environmentally friendly and has wide application prospects.

Description

Technical Field

[0001] The present invention relates to the field of medical technology, and in particular to a wormwood composition and a preparation method thereof. Background Art

[0002] Mugwort has the function of expelling evil spirits and warming the meridians. After testing countless kinds of herbs, the ancients concluded that the light wave particle energy after burning mugwort is very close to sunlight. Therefore, it is said that the sun is the yang of the sky, and mugwort is the yang of the earth.

[0003] Moxibustion, a method of moxibustion in traditional Chinese medicine, is a method of treatment that uses the heat generated by moxibustion materials made of moxa leaves to stimulate acupuncture points or specific parts of the body surface, and adjusts the disordered physiological and biochemical functions of the human body by stimulating the activity of meridian qi, thereby achieving the purpose of preventing and curing diseases. The use of moxibustion originated after humans mastered the use of fire, which was also in the Stone Age. Moxibustion originated in ancient China. Because its mechanism of action is similar to acupuncture, and it has a complementary therapeutic effect with acupuncture, it is usually used together with acupuncture, so it is called acupuncture. Acupuncture treatment has a far-reaching influence at home and abroad, but when modern people talk about moxibustion, most of the time they only refer to acupuncture, and rarely include moxibustion.

[0004] Moxibustion therapy is an important part of traditional Chinese medicine and one of the oldest medical methods in traditional medicine. Moxibustion has a good effect on more than 100 diseases. It has been widely used in clinical practice in history and has made great contributions to the prosperity of the Chinese nation.

[0005] The effect of moxibustion therapy is comprehensive. On the one hand, the heat stimulation when moxa is burned can adjust the local qi and blood of the human body; on the other hand, moxa itself has medicinal effects. Wu Yiluo of the Qing Dynasty said in "Compendium of Materia Medica": "Moxibustion leaves are bitter and pungent, warm when raw and hot when cooked, and pure yang in nature. They can restore the lost yang, connect the twelve meridians, run through the three yin meridians, regulate qi and blood, expel cold and dampness, warm the uterus, stop bleeding, warm the middle and relieve depression, regulate menstruation and stabilize pregnancy... With moxa fire, it can penetrate all meridians and eliminate all diseases." It can be said that the essence of moxibustion therapy lies in the unique medicinal properties of moxa.

[0006] However, the high temperature of moxibustion therapy can easily burn patients, and the smoke produced by the burning can also pollute the indoor environment. Doctors and patients will increase the risk of respiratory diseases in a smoke-polluted environment. In recent years, a variety of electronic moxibustion heating equipment and technologies have emerged, which can solve the problem of high-temperature burns through electronic temperature control technology. However, since the moxibustion products used are still moxa cones and moxa sticks made of moxa wool, the heat after temperature control cannot make the moxa wool produce smoke, and the medicinal ingredients of moxa cannot be effectively released, which loses the essence of moxibustion therapy. This is also not recognized by the vast majority of doctors and cannot be widely developed in medical institutions.

[0007] Currently, the raw materials used to make various moxa products such as moxa sticks, moxa sticks, moxa cakes, etc. on the market are pure moxa or moxa plus moxa powder. The purpose of moxibustion treatment is achieved through two methods: burning or heating by electronic instruments.

[0008] The first method is to produce smoke aerosol by burning traditional moxa products. This smoke aerosol brings out a large amount of effective ingredients produced by the thermal decomposition of moxa. These effective ingredients achieve therapeutic effects after attaching to the human body through the smoke aerosol. The disadvantage is that the smoke aerosol also contains a variety of harmful combustion particles and chemical products. Inhalation of the human body will cause harm, such as the risk of chronic pharyngitis and other diseases, and cause indoor air pollution.

[0009] The second method is to heat traditional moxa products with electronic instruments for moxibustion treatment. The defect is that traditional moxa products are made of dry pure moxa as raw materials. Although the effective ingredients of moxa are produced by heating, aerosols cannot be effectively produced. This effective ingredient cannot attach to the human body through aerosols to achieve therapeutic effects. Summary of the invention

[0010] The purpose of the present invention is to propose an wormwood composition and a preparation method thereof, which can promote the rupture of the explosive beads and the escape of the contents during the low-temperature heating process. As the water vapor and the essential oil of the traditional Chinese medicine evaporate, an aerosol is formed. The components are purer and do not contain PM2.5 particles, thus avoiding harm to human health, greatly improving the efficacy of the medicine, and being safer, healthier, greener and more environmentally friendly, and having broad application prospects.

[0011] The technical solution of the present invention is achieved in this way:

[0012] The invention provides a method for preparing a mugwort composition. Traditional Chinese medicine powder and Qichun Dragon Boat Festival mugwort are subjected to supercritical fluid extraction and molecular distillation to obtain traditional Chinese medicine essential oil, solid extraction is performed to obtain water-soluble active components and oil-soluble active components, the water-soluble active components are embedded to obtain nano-capsule powder, the water-soluble active components and a lipophilic emulsifier are added to the traditional Chinese medicine essential oil, an aqueous solution containing a hydrophilic emulsifier and sodium alginate is dripped, emulsified, solidified to obtain bursting beads, an atomizer and a surfactant are added to a chitosan solution, stirred and mixed, cross-linked, and the water content of the hydrogel is adjusted to obtain the mugwort composition.

[0013] As a further improvement of the present invention, the following steps are included:

[0014] S1. Preparation of Chinese herbal essential oil: The Chinese herbal powder and Qichun Dragon Boat Festival moxa are mixed evenly, and the Chinese herbal volatile oil is obtained by supercritical fluid extraction, and the Chinese herbal essential oil is obtained by molecular distillation of the Chinese herbal medicine, and the distillation product is collected to obtain the Chinese herbal essential oil, and the solid is retained;

[0015] S2. Extraction of water-soluble active components: The solid in step S1 is added to water, heated to boiling, extracted, filtered, the residue is retained, and the filtrate is dried to obtain a water-soluble active component;

[0016] S3. Extraction of the oil-soluble active component: The filter residue in step S2 was added to an acetone-ethyl acetate solution, heated for extraction, filtered, the filtrate was recovered from ethanol, and dried to obtain an oil-soluble active component;

[0017] S4. Preparation of nano-capsule powder: dissolving a water-soluble active component in water to prepare solution 1, preparing a polylactic acid-polycaprolactone solution to obtain solution 2, using a syringe pump to respectively allow solution 1 and solution 2 to impact the two inlets of a jet mixer in a closed manner, and under the driving action of the syringe pump, the two fluids collide and mix to obtain a nano-capsule suspension, which flows out from the outlet, is filtered with a filter membrane with a pore size of 0.1 μm, washed, and freeze-dried to obtain a nano-capsule powder;

[0018] S5. Preparation of popping beads: adding nano-capsule powder, oil-soluble active ingredients, and lipophilic emulsifier to traditional Chinese medicine essential oil to obtain an oil phase; adding a hydrophilic emulsifier and sodium alginate to water to obtain an aqueous phase; dropping the oil phase into the aqueous phase, emulsifying, dropping calcium chloride solution, solidifying at room temperature, centrifuging, washing, and drying to obtain popping beads;

[0019] S6. Preparation of an atomizer: mixing propylene glycol, glycerin and menthol to obtain an atomizer;

[0020] S7. Preparation of the mugwort composition: dissolve chitosan in acid solution, add explosive beads, atomizer, poloxamer P407 and poloxamer P188 chitosan, stir and mix evenly, add genipin for cross-linking, evaporate water to obtain hydrogel, adjust the water content of the hydrogel, and obtain the mugwort composition.

[0021] As a further improvement of the present invention, the Chinese medicine powder in step S1 is prepared from the following raw materials by weight: 10-15 parts of Shaanxi Sichuan pepper, 3-5 parts of Guizhou agrimony, 10-15 parts of Sichuan Chuanxiong, 10-15 parts of Cimicifuga, 15-25 parts of Inula flower, 7-10 parts of Fructus Liquidambar formosana, 4-6 parts of Uncaria rhynchophylla, 5-15 parts of Herba Artemisiae Argyi, and 3-5 parts of Licorice; the mass ratio of the Chinese medicine powder to Qichun Dragon Boat Festival Artemisia selengensis is 1:1.5-2.5, and the conditions for the supercritical fluid extraction are a CO2 flow rate of 25- 32L / h, extraction pressure 32-35MPa, extraction temperature 42-53℃, decomposition pressure 9.5-10.5MPa, decomposition temperature 50-60℃, time 1-2h, entrainer is ethyl acetate, the addition amount of the entrainer is 2-3%, the heating temperature of the molecular distillation is 90-120℃, the distillation condensation temperature is 0-2℃, the scraping speed is 150-250r / min, the feed flow rate is 3-5mL / min, and the system vacuum is 50-70Pa.

[0022] As a further improvement of the present invention, the solid-to-liquid ratio of the solid to water in step S2 is 1:5-7 g / mL, and the extraction time is 3-5 h.

[0023] As a further improvement of the present invention, the solid-to-liquid ratio of the filter residue and the acetone-ethyl acetate solution in step S3 is 1:3-5 g / mL, the volume ratio of acetone and ethyl acetate in the acetone-ethyl acetate solution is 3-5:7, the temperature of the heating extraction is 40-50° C., and the time is 2-4 h.

[0024] As a further improvement of the present invention, in step S4, the content of polylactic acid in the solution 2 is 22-27wt%, the content of polycaprolactone is 15-20wt%, the content of water-soluble active components in the solution 1 is 10-15wt%; the inner diameter of the inlet is 0.5-1.5mm; and the inner diameter of the outlet is 1.5-2.5mm.

[0025] As a further improvement of the present invention, the mass ratio of the nanocapsule powder, oil-soluble active component, lipophilic emulsifier and traditional Chinese medicine essential oil in step S5 is 3-5:4-6:0.5-1:45-55; the lipophilic emulsifier is selected from at least one of Span-20, Span-40, Span-60, Span-80 and Span-85; the mass ratio of the hydrophilic emulsifier, sodium alginate and water is 2-4:70-100:1000; the hydrophilic emulsifier is selected from at least one of Tween-20, Tween-40, Tween-60, Tween-80 and Tween-85.

[0026] As a further improvement of the present invention, the mass ratio of propylene glycol, glycerol and menthol in step S6 is 3-5:10:7-10.

[0027] As a further improvement of the present invention, the acid solution in step S7 is a 3-5wt% acetic acid or lactic acid solution, the mass ratio of the chitosan, explosive beads, atomizer, poloxamer P407, poloxamer P188, and genipin is 22-25:12-15:3-5:1-2:2-4:0.5-1, and the water content of the adjusted hydrogel is 35-55wt%.

[0028] The present invention further protects an wormwood composition prepared by the above preparation method.

[0029] The present invention has the following beneficial effects:

[0030] Authentic medicinal materials refer to Chinese medicinal materials with unique curative effect and quality that are formed through long-term planting, harvesting and processing under specific geographical, ecological and historical conditions. They are usually related to a certain geographical range, so their names often carry specific geographical indications, such as Sichuan Fritillaria, Yunnan Panax notoginseng, etc. The inventors have obtained the best quality of mugwort produced in Qichun, Hubei Province at 30 degrees north latitude with four distinct seasons through a large number of experimental comparisons, and those picked during the Dragon Boat Festival are the best. (The characteristics of plants depend on the local water, soil, climate, sunshine and other environments). The product of the present invention relies on Hubei Qi mugwort as a medium, and obtains medicinal gas by burning the authentic medicinal materials from various places through the fine grinding ratio. The energy of mugwort is used as a medium for communicating with the body, and the medicinal gas is transported into the body through moxibustion acupuncture points to expel evil and restore the body to nourish all meridians.

[0031] After many years of clinical experience and traveling around the country, the inventor of the present invention found that the mugwort picked during the Dragon Boat Festival in Qichun, Hubei Province is of the best quality and can be combined with other authentic Chinese medicinal materials to complement each other and produce better effects.

[0032] The medicinal effects of selecting Shaanxi Sichuan pepper include warming the middle and dispelling cold, warming the stomach and removing wind, relieving fullness and relieving bloating, resolving phlegm and relieving cough, breaking blood and dredge menstruation, relieving pain, and having the functions of killing insects, removing bacteria, disinfecting and relieving itching.

[0033] We use Guizhou Herba Centipede, which has medicinal uses such as detoxification and tonic. Guizhou is mountainous and has a pure ecology.

[0034] Sichuan Chuanxiong is selected, which has the medicinal effect of promoting qi, activating blood circulation and relieving pain.

[0035] Choose Cimicifuga, which has the medicinal effects of relieving rash, raising yang and lifting sunken, clearing away heat and detoxifying.

[0036] Choose Inula japonica, which has the medicinal effects of resolving phlegm and relieving adverse symptoms, calming the mind and dredging meridians, clearing away heat and calming the mind.

[0037] Choose Rhizoma Lulutong, which has the medicinal effects of dispelling wind and dredging the meridians, promoting diuresis and dampness, and relieving itching.

[0038] Choose Uncaria rhynchophylla, which has the medicinal effects of calming wind and relieving heat, clearing away heat and soothing the liver, and calming the mind.

[0039] Choose knotweed, which has the medicinal effects of clearing away heat, dissipating blood stasis, relieving cough and reducing phlegm.

[0040] Choose licorice, which has the medicinal effects of detoxifying, replenishing the middle and invigorating qi and harmonizing various medicines.

[0041] The above herbs are paired according to monarch, minister, assistant and envoy:

[0042] The main ingredient is Inula fuciformis, which mainly functions to calm the mind, descend qi, resolve phlegm, eliminate abdominal distension, remove stagnation and dredge the meridians.

[0043] The ministers are three flavors: Cimicifuga, Chuanxiong, and Sichuan pepper. Cimicifuga raises yang and lifts the sunken to allow the evil qi to penetrate the surface, Chuanxiong promotes qi and activates blood circulation to assist, and Sichuan pepper clears away evil spirits, purifies the body, and warms the meridians and dredges the collaterals.

[0044] It is supplemented with Rhizoma Lulutong and Herba Lycopodii to further enhance the effects of dispelling wind, unblocking meridians, dispersing blood stasis and reducing phlegm.

[0045] The envoys are licorice, agrimony and Uncaria rhynchophylla. Agrimony can replenish the body, licorice can coordinate the various drugs, and Uncaria rhynchophylla can calm the mind.

[0046] The medicinal materials are matched with Qichun Dragon Boat Festival moxa in a mass ratio of 1:2 (the ratio of traditional medicinal moxa is generally 10% medicinal materials and 90% moxa. The ratio of medicinal materials in the present invention is higher and the curative effect is better. There is no ability to distinguish whether the traditional medicinal materials are authentic, and the quality of moxa is uneven. The present invention selects authentic medicinal materials and uses wormwood with better quality, and the effect is twice the result with half the effort). Use the medium power of moxa to open the acupuncture points of the body, purify the body with medicinal gas, warm the meridians and dredge the collaterals, and resolve phlegm and eliminate stagnation. After clinical research and development, the main sequence of the ratio is now in place, and the curative effect is significant. The product of the present invention has been in actual clinical practice for more than a year and has received numerous praises. A truly pure green health therapy, the efficiency is as high as 95% for daily sub-health conditions such as pain, sub-health, colds and strains.

[0047] Burning Chinese medicine powder and moxa by common methods often generates a large amount of smoke, which is harmful to human health when inhaled. The present invention prepares a hydrogel, which is rich in explosive beads and atomizers. The explosive beads use sodium alginate as a shell material, and contain Chinese medicine essential oil, water-soluble active components and oil-soluble active components. The water-soluble active components are embedded in microcapsules, which can improve their dispersibility in oil-soluble media on the one hand, and on the other hand, the shell material is easily broken during low-temperature heating (below 400°C), thereby releasing the water-soluble active components. At the same time, the bursting beads are easily broken during the low-temperature heating process (below 400°C), thereby promoting the volatilization of the Chinese herbal essential oil. At the same time, the water-soluble active components and the oil-soluble active components will also be brought into the aerosol with the volatilization of the Chinese herbal essential oil. Compared with traditional combustion, the aerosol of the present invention does not contain carbonized particles produced after the combustion of wormwood, and is mainly a water / oil aerosol formed by water vapor and Chinese herbal essential oil with active components. Under the promotion of the atomizer, the components of the aerosol are purer, do not contain PM2.5 particles, and avoid harm to human health. Compared with directly using wormwood as an active component to make a steam aerosol, the present invention obtains Chinese herbal essential oil through extraction, water extraction obtains water-soluble active components, and oil-soluble solvent extraction obtains oil-soluble active components. It can maximize the pharmacological activity of the aerosol and greatly improve the efficacy.

[0048] The present invention adopts supercritical fluid extraction to obtain high-purity volatile oil of traditional Chinese medicine, and under the action of molecular distillation, separates the active components of the essential oil with low boiling point, removes high boiling point impurities, and does not destroy heat-sensitive substances. During the low-temperature heating process, these low-boiling point traditional Chinese medicine essences can volatilize and dissipate well, thereby forming a purer and more stable aerosol.

[0049] In addition, in addition to the traditional propylene glycol and glycerin, the atomizer of the present invention also adds menthol, which greatly improves the transdermal absorption of the aerosol drug particles attached to the surface of human skin, thereby further improving the drug efficacy. In addition, menthol also has a certain effect of participating in the formation of atomization, and the water in the liquid hydrogel and the traditional Chinese medicine essential oil in the bursting beads are converted into gaseous state by heating, thereby improving the composition and particle size distribution of the aerosol.

[0050] Chitosan is a good hydrogel carrier. Under the cross-linking effect of genipin, it can form a hydrogel with a certain water content. By evenly dispersing the bursting beads and atomizers, it can promote the bursting beads to rupture and the contents to escape during the low-temperature heating process. As the water vapor and Chinese medicine essential oil evaporate, an aerosol is formed, which greatly improves the efficacy of the drug and is safer, healthier, and more environmentally friendly.

[0051] The wormwood composition prepared by the present invention can promote the rupture of the explosive beads and the escape of the contents during the low-temperature heating process (below 400°C), and form an aerosol as the water vapor and the essential oil of the traditional Chinese medicine evaporate. The components are purer and do not contain PM2.5 particles, thus avoiding harm to human health, greatly improving the efficacy of the medicine, and being safer, healthier, greener and more environmentally friendly, and having broad application prospects. DETAILED DESCRIPTION

[0052] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0053] Example 1

[0054] The present invention provides a method for preparing a wormwood composition, comprising the following steps:

[0055] S1. Preparation of Chinese herbal essential oil: 10 g of Chinese herbal powder and 15 g of Qichun Dragon Boat Festival moxa were mixed for 15 min, and volatile oil of Chinese herbal medicine was obtained by supercritical fluid extraction. The Chinese herbal medicine was molecularly distilled, and the distillation product was collected to obtain the essential oil of Chinese herbal medicine, and the solid was retained;

[0056] The Chinese medicine powder is prepared from the following raw materials by weight: 10 parts of Sichuan pepper from Shaanxi, 3 parts of Guizhou agrimony, 10 parts of Sichuan chuanxiong, 10 parts of Cimicifuga heracleifolia, 15 parts of Inula flower, 7 parts of Fructus liquidambar formosana, 4 parts of Uncaria rhynchophylla, 5 parts of Herba Artemisiae Argyi, and 3 parts of Licorice;

[0057] The supercritical fluid extraction conditions are as follows: CO2 flow rate of 25 L / h, extraction pressure of 32 MPa, extraction temperature of 42°C, decomposition pressure of 9.5 MPa, decomposition temperature of 50°C, time of 1 h, entrainer of ethyl acetate, and the addition amount of the entrainer of 2%;

[0058] The heating temperature of the molecular distillation is 90°C, the distillation condensation temperature is 0°C, the scraping speed is 150r / min, the feed flow rate is 3mL / min, and the system vacuum degree is 50Pa;

[0059] S2. Extraction of water-soluble active components: 10 g of the solid in step S1 was added to 50 mL of water, heated to boiling, extracted for 3 h, filtered, the residue was retained, and the filtrate was dried to obtain a water-soluble active component;

[0060] S3. Extraction of oil-soluble active components: 10 g of the filter residue in step S2 was added to 30 mL of acetone-ethyl acetate solution, heated to 40 ° C, stirred for extraction for 2 h, filtered, the filtrate was recovered with ethanol, and dried to obtain an oil-soluble active component;

[0061] The volume ratio of acetone to ethyl acetate in the acetone-ethyl acetate solution is 3:7;

[0062] S4. Preparation of nano-capsule powder: dissolving a water-soluble active component in water to prepare solution 1, wherein the content of the water-soluble active component is 10wt%, preparing a polylactic acid-polycaprolactone solution to obtain solution 2, wherein the content of polylactic acid is 22wt%, and the content of polycaprolactone is 15wt%, using a syringe pump to respectively allow solution 1 and solution 2 to be airtightly impacted with two inlets of a jet mixer, and under the driving action of the syringe pump, the two fluids collide and mix to obtain a nano-capsule suspension, which flows out from the outlet, is filtered with a filter membrane with a pore size of 0.1μm, washed, and freeze-dried to obtain nano-capsule powder; the inner diameter of the inlet is 0.5mm; the inner diameter of the outlet is 1.5mm;

[0063] S5. Preparation of popping beads: 3g of nanocapsule powder, 4g of oil-soluble active ingredients, and 0.5g of Span-20 were added to 45g of traditional Chinese medicine essential oil to obtain an oil phase; 2g of Tween-20 and 70g of sodium alginate were added to 1L of water to obtain an aqueous phase; the oil phase was added dropwise to the aqueous phase, emulsified at 8000r / min for 15min, 50mL of 5wt% calcium chloride solution was added dropwise, cured at room temperature for 30min, centrifuged, washed, and dried to obtain popping beads;

[0064] S6. Preparation of atomizer: 3 g of propylene glycol, 10 g of glycerol and 7 g of menthol were stirred and mixed for 10 min to prepare atomizer;

[0065] S7. Preparation of wormwood composition: dissolve 22g chitosan in 200mL 3wt% acetic acid solution, add 12g explosive beads, 3g atomizer, 1g poloxamer P407 and 2g poloxamer P188 and stir for 15min, add 100mL aqueous solution containing 0.5g genipin, cross-link for 5h, heat to 60℃ to evaporate water to obtain hydrogel, adjust the water content of the hydrogel to 35wt% to obtain wormwood composition.

[0066] Example 2

[0067] The present invention provides a method for preparing a wormwood composition, comprising the following steps:

[0068] S1. Preparation of Chinese herbal essential oil: 10 g of Chinese herbal powder and 25 g of Qichun Dragon Boat Festival moxa were mixed for 15 min, and volatile oil of Chinese herbal medicine was obtained by supercritical fluid extraction. The Chinese herbal medicine was molecularly distilled, and the distillation product was collected to obtain the essential oil of Chinese herbal medicine, and the solid was retained;

[0069] The Chinese medicine powder is prepared from the following raw materials by weight: 15 parts of Shaanxi Sichuan pepper, 5 parts of Guizhou agrimony, 15 parts of Sichuan chuanxiong, 15 parts of Cimicifuga heracleifolia, 25 parts of Inula flower, 10 parts of Fructus liquidambar formosana, 6 parts of Uncaria rhynchophylla, 15 parts of Herba Artemisiae Argyi, and 5 parts of Licorice;

[0070] The supercritical fluid extraction conditions are as follows: CO2 flow rate of 32 L / h, extraction pressure of 35 MPa, extraction temperature of 53°C, decomposition pressure of 10.5 MPa, decomposition temperature of 60°C, time of 2 h, entrainer of ethyl acetate, and the addition amount of the entrainer of 3%;

[0071] The heating temperature of the molecular distillation is 120°C, the distillation condensation temperature is 2°C, the scraping speed is 250r / min, the feed flow rate is 5mL / min, and the system vacuum degree is 70Pa;

[0072] S2. Extraction of water-soluble active components: 10 g of the solid in step S1 was added to 70 mL of water, heated to boiling, extracted for 5 h, filtered, the residue was retained, and the filtrate was dried to obtain a water-soluble active component;

[0073] S3. Extraction of oil-soluble active components: 10 g of the residue in step S2 was added to 50 mL of acetone-ethyl acetate solution, heated to 50 ° C, stirred for extraction for 4 h, filtered, the filtrate was recovered with ethanol, and dried to obtain an oil-soluble active component;

[0074] The volume ratio of acetone to ethyl acetate in the acetone-ethyl acetate solution is 5:7;

[0075] S4. Preparation of nano-capsule powder: dissolving a water-soluble active component in water to prepare solution 1, wherein the content of the water-soluble active component is 15 wt %. Preparing a polylactic acid-polycaprolactone solution to obtain solution 2, wherein the content of polylactic acid is 27 wt %, and the content of polycaprolactone is 20 wt %. Using a syringe pump, respectively, solution 1 and solution 2 are sealed and impacted into two inlets of a jet mixer. Under the driving action of the syringe pump, the two fluids collide and mix to obtain a nano-capsule suspension, which flows out from the outlet, is filtered through a filter membrane with a pore size of 0.1 μm, washed, and freeze-dried to obtain a nano-capsule powder; the inner diameter of the inlet is 1.5 mm; the inner diameter of the outlet is 2.5 mm;

[0076] S5. Preparation of popping beads: 5g of nanocapsule powder, 6g of oil-soluble active ingredients, and 1g of Span-40 were added to 55g of traditional Chinese medicine essential oil to obtain an oil phase; 4g of Tween-40 and 100g of sodium alginate were added to 1L of water to obtain an aqueous phase; the oil phase was added dropwise to the aqueous phase, emulsified at 8000r / min for 15min, 50mL of 5wt% calcium chloride solution was added dropwise, cured at room temperature for 30min, centrifuged, washed, and dried to obtain popping beads;

[0077] S6. Preparation of atomizer: 5 g of propylene glycol, 10 g of glycerol and 10 g of menthol were stirred and mixed for 10 min to prepare atomizer;

[0078] S7. Preparation of wormwood composition: dissolve 25g chitosan in 200mL 5wt% lactic acid solution, add 15g explosive beads, 5g atomizer, 2g poloxamer P407 and 4g poloxamer P188, stir and mix for 15min, add 100mL aqueous solution containing 1g genipin, cross-link for 5h, heat to 60℃ to evaporate water to obtain hydrogel, adjust the water content of the hydrogel to 55wt%, and obtain wormwood composition.

[0079] Example 3

[0080] The present invention provides a method for preparing a wormwood composition, comprising the following steps:

[0081] S1. Preparation of Chinese herbal essential oil: 10 g of Chinese herbal powder and 20 g of Qichun Dragon Boat Festival moxa were mixed for 15 min, and volatile oil of Chinese herbal medicine was obtained by supercritical fluid extraction. The Chinese herbal medicine was molecularly distilled, and the distillation product was collected to obtain the essential oil of Chinese herbal medicine, and the solid was retained;

[0082] The Chinese medicine powder is prepared from the following raw materials by weight: 12 parts of Sichuan pepper from Shaanxi, 4 parts of Guizhou agrimony, 12 parts of Sichuan chuanxiong, 12 parts of Cimicifuga heracleifolia, 20 parts of Inula flower, 8 parts of Fructus liquidambar formosana, 5 parts of Uncaria rhynchophylla, 10 parts of Herba Artemisiae Argyi, and 4 parts of Licorice;

[0083] The supercritical fluid extraction conditions are as follows: CO2 flow rate of 29 L / h, extraction pressure of 33 MPa, extraction temperature of 50°C, decomposition pressure of 10 MPa, decomposition temperature of 55°C, time of 1.5 h, entrainer of ethyl acetate, and the addition amount of the entrainer of 2.5%;

[0084] The heating temperature of the molecular distillation is 105°C, the distillation condensation temperature is 1°C, the scraping speed is 200r / min, the feed flow rate is 4mL / min, and the system vacuum degree is 60Pa;

[0085] S2. Extraction of water-soluble active components: 10 g of the solid in step S1 was added to 60 mL of water, heated to boiling, extracted for 4 h, filtered, the residue was retained, and the filtrate was dried to obtain a water-soluble active component;

[0086] S3. Extraction of oil-soluble active components: 10 g of the residue in step S2 was added to 40 mL of acetone-ethyl acetate solution, heated to 45 ° C, stirred and extracted for 3 h, filtered, the filtrate was recovered with ethanol, and dried to obtain an oil-soluble active component;

[0087] The volume ratio of acetone to ethyl acetate in the acetone-ethyl acetate solution is 4:7;

[0088] S4. Preparation of nano-capsule powder: dissolving a water-soluble active component in water to prepare solution 1, wherein the content of the water-soluble active component is 12 wt %. preparing a polylactic acid-polycaprolactone solution to obtain solution 2, wherein the content of polylactic acid is 25 wt % and the content of polycaprolactone is 17 wt %. using a syringe pump, respectively, solution 1 and solution 2 are sealed and impacted into two inlets of a jet mixer. Under the driving action of the syringe pump, the two fluids collide and mix to obtain a nano-capsule suspension, which flows out from the outlet, is filtered through a filter membrane with a pore size of 0.1 μm, washed, and freeze-dried to obtain nano-capsule powder; the inner diameter of the inlet is 1 mm; the inner diameter of the outlet is 2 mm;

[0089] S5. Preparation of popping beads: 4g of nanocapsule powder, 5g of oil-soluble active ingredients, and 0.7g of Span-85 were added to 50g of traditional Chinese medicine essential oil to obtain an oil phase; 3g of Tween-85 and 85g of sodium alginate were added to 1L of water to obtain an aqueous phase; the oil phase was added dropwise to the aqueous phase, emulsified at 8000r / min for 15min, 50mL of 5wt% calcium chloride solution was added dropwise, cured at room temperature for 30min, centrifuged, washed, and dried to obtain popping beads;

[0090] S6. Preparation of atomizer: 4 g of propylene glycol, 10 g of glycerol and 8 g of menthol were stirred and mixed for 10 min to prepare an atomizer;

[0091] S7. Preparation of wormwood composition: dissolve 23g chitosan in 200mL 4wt% acetic acid solution, add 13g explosive beads, 4g atomizer, 1.5g poloxamer P407 and 3g poloxamer P188, stir and mix for 15min, add 100mL aqueous solution containing 0.7g genipin, cross-link for 5h, heat to 60℃ to evaporate water to obtain hydrogel, adjust the water content of the hydrogel to 45wt%, and obtain wormwood composition.

[0092] Comparative Example 1

[0093] Compared with Example 3, the difference is that no molecular distillation is performed in step S1.

[0094] The details are as follows:

[0095] S1. Preparation of Chinese herbal essential oils: 10 g of Chinese herbal powder and 20 g of Qichun Dragon Boat Festival moxa were mixed for 15 min, and extracted by supercritical fluid to obtain Chinese herbal volatile oils, i.e. Chinese herbal essential oils, and the solids were retained;

[0096] The Chinese medicine powder is prepared from the following raw materials by weight: 12 parts of Sichuan pepper from Shaanxi, 4 parts of Guizhou agrimony, 12 parts of Sichuan chuanxiong, 12 parts of Cimicifuga heracleifolia, 20 parts of Inula flower, 8 parts of Fructus liquidambar formosana, 5 parts of Uncaria rhynchophylla, 10 parts of Herba Artemisiae Argyi, and 4 parts of Licorice;

[0097] The conditions of the supercritical fluid extraction are: CO2 flow rate of 29L / h, extraction pressure of 33MPa, extraction temperature of 50°C, decomposition pressure of 10MPa, decomposition temperature of 55°C, time of 1.5h, entrainer of ethyl acetate, and the addition amount of the entrainer is 2.5%.

[0098] Comparative Example 2

[0099] Compared with Example 3, the difference is that step S4 is not performed.

[0100] The details are as follows:

[0101] S1. Preparation of Chinese herbal essential oil: 10 g of Chinese herbal powder and 20 g of Qichun Dragon Boat Festival moxa were mixed for 15 min, and volatile oil of Chinese herbal medicine was obtained by supercritical fluid extraction. The Chinese herbal medicine was molecularly distilled, and the distillation product was collected to obtain the essential oil of Chinese herbal medicine, and the solid was retained;

[0102] The Chinese medicine powder is prepared from the following raw materials by weight: 12 parts of Sichuan pepper from Shaanxi, 4 parts of Guizhou agrimony, 12 parts of Sichuan chuanxiong, 12 parts of Cimicifuga heracleifolia, 20 parts of Inula flower, 8 parts of Fructus liquidambar formosana, 5 parts of Uncaria rhynchophylla, 10 parts of Herba Artemisiae Argyi, and 4 parts of Licorice;

[0103] The supercritical fluid extraction conditions are as follows: CO2 flow rate of 29 L / h, extraction pressure of 33 MPa, extraction temperature of 50°C, decomposition pressure of 10 MPa, decomposition temperature of 55°C, time of 1.5 h, entrainer of ethyl acetate, and the addition amount of the entrainer of 2.5%;

[0104] The heating temperature of the molecular distillation is 105°C, the distillation condensation temperature is 1°C, the scraping speed is 200r / min, the feed flow rate is 4mL / min, and the system vacuum degree is 60Pa;

[0105] S2. Extraction of water-soluble active components: 10 g of the solid in step S1 was added to 60 mL of water, heated to boiling, extracted for 4 h, filtered, the residue was retained, and the filtrate was dried to obtain a water-soluble active component;

[0106] S3. Extraction of oil-soluble active components: 10 g of the residue in step S2 was added to 40 mL of acetone-ethyl acetate solution, heated to 45 ° C, stirred and extracted for 3 h, filtered, the filtrate was recovered with ethanol, and dried to obtain an oil-soluble active component;

[0107] The volume ratio of acetone to ethyl acetate in the acetone-ethyl acetate solution is 4:7;

[0108] S4. Preparation of popping beads: 4g of water-soluble active ingredients, 5g of oil-soluble active ingredients, and 0.7g of Span-85 were added to 50g of traditional Chinese medicine essential oil to obtain an oil phase; 3g of Tween-85 and 85g of sodium alginate were added to 1L of water to obtain an aqueous phase; the oil phase was added dropwise to the aqueous phase, emulsified at 8000r / min for 15min, 50mL of 5wt% calcium chloride solution was added dropwise, cured at room temperature for 30min, centrifuged, washed, and dried to obtain popping beads;

[0109] S5. Preparation of atomizer: 4 g of propylene glycol, 10 g of glycerol and 8 g of menthol were stirred and mixed for 10 min to prepare atomizer;

[0110] S6. Preparation of wormwood composition: 23g chitosan was dissolved in 200mL 4wt% acetic acid solution, 13g explosive beads, 4g atomizer, 1.5g poloxamer P407 and 3g poloxamer P188 were added and stirred for 15min, 100mL of aqueous solution containing 0.7g genipin was added dropwise, cross-linked for 5h, heated to 60°C to evaporate water to obtain hydrogel, and the water content of the hydrogel was adjusted to 45wt% to obtain a wormwood composition.

[0111] Comparative Example 3

[0112] Compared with Example 3, the difference is that no oil-soluble active component is added in step S5.

[0113] The details are as follows:

[0114] S5. Preparation of bursting beads: add 9g of nano-capsule powder and 0.7g of Span-85 to 50g of traditional Chinese medicine essential oil to obtain an oil phase; add 3g of Tween-85 and 85g of sodium alginate to 1L of water to obtain an aqueous phase; add the oil phase dropwise to the aqueous phase, emulsify at 8000r / min for 15min, add 50mL of 5wt% calcium chloride solution dropwise, solidify at room temperature for 30min, centrifuge, wash, and dry to obtain bursting beads.

[0115] Comparative Example 4

[0116] Compared with Example 3, the difference is that no nano-capsule powder is added in step S5.

[0117] The details are as follows:

[0118] S5. Preparation of bursting beads: add 9g of oil-soluble active components and 0.7g of Span-85 to 50g of traditional Chinese medicine essential oil to obtain an oil phase; add 3g of Tween-85 and 85g of sodium alginate to 1L of water to obtain an aqueous phase; add the oil phase dropwise into the aqueous phase, emulsify at 8000r / min for 15min, add 50mL of 5wt% calcium chloride solution dropwise, solidify at room temperature for 30min, centrifuge, wash, and dry to obtain bursting beads.

[0119] Comparative Example 5

[0120] Compared with Example 3, the difference is that menthol is not added in step S6.

[0121] The details are as follows:

[0122] S6. Preparation of atomizer: 4 g of propylene glycol and 10 g of glycerol were stirred and mixed for 10 min to prepare atomizer.

[0123] Test Example 1

[0124] The wormwood compositions prepared in Examples 1-3 and Comparative Examples 1-5 were sucked by the SCS suction simulation sampler according to the set suction mode. The generated gas was quickly diluted by the two-stage dilution system and then entered the DMS500 fast particle size spectrometer. According to the difference in electrical mobility of particles of different particle sizes, the median particle size, particle number concentration, and volume concentration of the aerosol particles were measured. The first dilution was a constant flow sampling method, and the first dilution flow rate was set to 20.0L / min; the second dilution used a rotating disc diluter, and the second dilution ratio was set to 200:1. The heated samples were measured in parallel 3 times, and the average of the parallel measurement data was taken.

[0125] The results are shown in Table 1.

[0126] Table 1

[0127]

[0128] It can be seen from the above table that the wormwood compositions prepared in Examples 1-3 of the present invention have higher particle number concentration and volume concentration after low-temperature heating and suction, and the median particle size is smaller.

[0129] Test Example 2

[0130] Taking 10% chlorpyrifos and commercially available Liushen mosquito repellent floral water (4.5% chlorpyrifos) as controls, the mosquito repellent effectiveness of the wormwood composition obtained in Examples 1-3 or Comparative Examples 1-5 (using MCH ceramic heating plates for temperature control and heating, respectively, controlling the temperature to 220°C, and collecting the released aerosol with oil-absorbing cotton for 20 minutes) was tested according to the method specified in GB / T 13917.9-2009.

[0131] The results are shown in Table 2.

[0132] Table 2

[0133] Group Mosquito repellent duration (min) 10% mosquito repellent 279 Liushen mosquito repellent floral water (4.5% mosquito repellent) 215 Example 1 480 Example 2 475 Example 3 485 Comparative Example 1 462 Comparative Example 2 375 Comparative Example 3 394 Comparative Example 4 327 Comparative Example 5 457

[0134] It can be seen from the above table that the wormwood compositions prepared in Examples 1-3 of the present invention have a good mosquito repellent effect, and the mosquito repellent effect can reach 7 hours.

[0135] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims

1. A method for preparing a wormwood composition, characterized in that: The Chinese medicine powder and Qichun Dragon Boat Festival moxa are subjected to supercritical fluid extraction and molecular distillation to obtain Chinese medicine essential oil, and solid extraction is used to obtain water-soluble active components and oil-soluble active components. The water-soluble active components are embedded to obtain nano-capsule powder, which is added to the Chinese medicine essential oil together with the oil-soluble active components and a lipophilic emulsifier. An aqueous solution containing a hydrophilic emulsifier and sodium alginate is added dropwise, emulsified, and solidified to obtain explosive beads, which are added to a chitosan solution with an atomizer and a surfactant, stirred and mixed, cross-linked, and the water content of the hydrogel is adjusted to obtain a moxa composite.

2. The preparation method according to claim 1, characterized in that: The following steps are involved: S1. Preparation of Chinese herbal essential oil: The Chinese herbal powder and Qichun Dragon Boat Festival moxa are mixed evenly, and the Chinese herbal volatile oil is obtained by supercritical fluid extraction, and the Chinese herbal essential oil is obtained by molecular distillation of the Chinese herbal medicine, and the distillation product is collected to obtain the Chinese herbal essential oil, and the solid is retained; S2. Extraction of water-soluble active components: The solid in step S1 is added to water, heated to boiling, extracted, filtered, the residue is retained, and the filtrate is dried to obtain a water-soluble active component; S3. Extraction of the oil-soluble active component: The filter residue in step S2 was added to an acetone-ethyl acetate solution, heated for extraction, filtered, the filtrate was recovered from ethanol, and dried to obtain an oil-soluble active component; S4. Preparation of nano-capsule powder: dissolving a water-soluble active component in water to prepare solution 1, preparing a polylactic acid-polycaprolactone solution to obtain solution 2, using a syringe pump to respectively allow solution 1 and solution 2 to impact the two inlets of a jet mixer in a closed manner, and under the driving action of the syringe pump, the two fluids collide and mix to obtain a nano-capsule suspension, which flows out from the outlet, is filtered with a filter membrane with a pore size of 0.1 μm, washed, and freeze-dried to obtain a nano-capsule powder; S5. Preparation of popping beads: adding nano-capsule powder, oil-soluble active ingredients, and lipophilic emulsifier to traditional Chinese medicine essential oil to obtain an oil phase; adding a hydrophilic emulsifier and sodium alginate to water to obtain an aqueous phase; dropping the oil phase into the aqueous phase, emulsifying, dropping calcium chloride solution, solidifying at room temperature, centrifuging, washing, and drying to obtain popping beads; S6. Preparation of an atomizer: mixing propylene glycol, glycerin and menthol to obtain an atomizer; S7. Preparation of the mugwort composition: dissolve chitosan in acid solution, add explosive beads, atomizer, poloxamer P407 and poloxamer P188 chitosan, stir and mix evenly, add genipin for cross-linking, evaporate water to obtain hydrogel, adjust the water content of the hydrogel, and obtain the mugwort composition.

3. The preparation method according to claim 2, characterized in that: The Chinese medicine powder in step S1 is prepared from the following raw materials by weight: 10-15 parts of Shaanxi Sichuan pepper, 3-5 parts of Guizhou agrimony, 10-15 parts of Sichuan chuanxiong, 10-15 parts of Cimicifuga, 15-25 parts of Inula flower, 7-10 parts of Fructus Liquidambar formosana, 4-6 parts of Uncaria rhynchophylla, 5-15 parts of Herba Artemisiae Argyi, and 3-5 parts of Licorice; the mass ratio of the Chinese medicine powder to Qichun Dragon Boat Festival Artemisia selengensis is 1:1.5-2.5, and the supercritical fluid extraction condition is a CO2 flow rate of 25-32 L / h, The extraction pressure is 32-35MPa, the extraction temperature is 42-53°C, the decomposition pressure is 9.5-10.5MPa, the decomposition temperature is 50-60°C, the time is 1-2h, the entrainer is ethyl acetate, the addition amount of the entrainer is 2-3%, the heating temperature of the molecular distillation is 90-120°C, the distillation condensation temperature is 0-2°C, the scraping speed is 150-250r / min, the feed flow rate is 3-5mL / min, and the system vacuum is 50-70Pa.

4. The preparation method according to claim 2, characterized in that: The solid-to-liquid ratio of the solid to water in step S2 is 1:5-7 g / mL, and the extraction time is 3-5 h.

5. The preparation method according to claim 2, characterized in that: In step S3, the solid-liquid ratio of the filter residue to the acetone-ethyl acetate solution is 1:3-5 g / mL, the volume ratio of acetone to ethyl acetate in the acetone-ethyl acetate solution is 3-5:7, the temperature of the heating extraction is 40-50° C., and the time is 2-4 h.

6. The preparation method according to claim 2, characterized in that: In step S4, the content of polylactic acid in the solution 2 is 22-27wt%, the content of polycaprolactone is 15-20wt%, and the content of water-soluble active components in the solution 1 is 10-15wt%; the inner diameter of the inlet is 0.5-1.5mm; and the inner diameter of the outlet is 1.5-2.5mm.

7. The preparation method according to claim 2, characterized in that: The mass ratio of the nano-capsule powder, oil-soluble active component, lipophilic emulsifier and Chinese medicine essential oil in step S5 is 3-5:4-6:0.5-1:45-55; the lipophilic emulsifier is selected from at least one of Span-20, Span-40, Span-60, Span-80 and Span-85; the mass ratio of the hydrophilic emulsifier, sodium alginate and water is 2-4:70-100:1000; the hydrophilic emulsifier is selected from at least one of Tween-20, Tween-40, Tween-60, Tween-80 and Tween-85.

8. The preparation method according to claim 2, characterized in that: The mass ratio of propylene glycol, glycerol and menthol in step S6 is 3-5:10:7-10.

9. The preparation method according to claim 2, characterized in that: The acid solution in step S7 is 3-5wt% acetic acid or lactic acid solution, the mass ratio of chitosan, explosive beads, atomizer, poloxamer P407, poloxamer P188, and genipin is 22-25:12-15:3-5:1-2:2-4:0.5-1, and the water content of the adjusted hydrogel is 35-55wt%.

10. A wormwood composition obtained by the preparation method according to any one of claims 1 to 9.

Images