Artemisia argyi aging method

Abstract

The invention relates to a method for treating traditional Chinese medicinal materials, in particular to a method for aging folium artemisiae argyi. The method comprises the steps that in a closed environment, ozone is used for fumigating folium artemisiae argyi, ultraviolet irradiation is assisted, and treatment is conducted twice every day; continuous treatment is conducted for 25 d to 35 d; the ozone fumigation is 110-130 minutes in each treatment, and the ultraviolet radiation is 25-35 minutes in each treatment. By means of the method, the problems that due to the fact that the traditional aging process is slow, the occupied space of a wormwood storage site is large, the occupied time is long, and the capital occupation is high can be solved, and the folium artemisiae argyi which is naturally aged for three years in quality can be obtained within a short time.

Description

Technical Field

[0001] The invention relates to a method for processing Chinese medicinal materials, and in particular to a method for aging wormwood leaves. Background Art

[0002] Artemisia argyi is the dried leaves of Artemisia argyi LevL.et Vant., a plant of the Asteraceae family. Artemisia argyi is a commonly used traditional Chinese medicine in my country, which has the effects of dispelling cold and relieving pain, warming the meridians and stopping bleeding. Pharmacologically, artemisia argyi has anti-inflammatory, antibacterial, antioxidant, and hypoglycemic effects. In addition to being used directly as medicine, artemisia argyi can also be made into moxa sticks, which can be used to stimulate the acupuncture points of the human body with heat to adjust the disordered physiological and biochemical state of the human body, thereby achieving the effect of treating diseases. Artemisia argyi has a long history of medicinal use, a wide range of sources, and few toxic and side effects. Artemisia argyi has a long history of medicinal use. Many classics record that "the older the artemisia argyi is, the better it is." Especially when used in moxibustion therapy, aged artemisia argyi is more favored.

[0003] A large number of studies have shown that the older the wormwood is, the better it is because of the accumulation of active substances during its storage, but the accumulation mechanism is still unclear. Volatile oil is a major chemical component in wormwood and an important component for its pharmacological effects. Current studies have found that volatile oils in wormwood mainly contain chemical components such as monoterpenes and their derivatives, sesquiterpenes and their derivatives, ketones (aldehydes), alcohols (phenols), acids (esters), alkanes (alkenes), etc., which have anti-inflammatory, antibacterial, antiviral, antiasthmatic, antitussive and expectorant, antiallergic, analgesic and other pharmacological activities. Among them, eucalyptol and borneol are specified as quality mark components of wormwood in the 2020 edition of the Chinese Pharmacopoeia. In addition to volatile oils, phenolic acids and flavonoids are also one of the main chemical components of wormwood. Studies have shown that with the extension of natural storage time, the content of phenolic acid and total flavonoids in three-year-old wormwood reaches a peak, so there is a saying that "three-year-old wormwood is the best."

[0004] However, the natural aging of mugwort leaves takes a long time, which cannot meet the market demand for high-quality aged mugwort leaves. Summary of the invention

[0005] In order to solve the above technical problems, the present invention provides a method for aging wormwood leaves.

[0006] To achieve the above object, the present invention adopts the following technical solution:

[0007] A method for aging wormwood leaves, comprising: fumigating the wormwood leaves with ozone in a closed environment, supplemented by ultraviolet irradiation, twice a day; continuously treating for 25 to 35 days;

[0008] Each treatment lasts for 110 to 130 minutes of ozone fumigation and 25 to 35 minutes of ultraviolet irradiation.

[0009] In some embodiments of the present invention, the wormwood leaf is dried wormwood leaf.

[0010] In some embodiments of the present invention, the concentration of ozone fumigation is 0.5 ppm to 0.8 ppm.

[0011] In some embodiments of the present invention, the ultraviolet light intensity is 25W to 35W.

[0012] In some embodiments of the present invention, the interval between two treatments per day is 6 hours to 8 hours.

[0013] In some embodiments of the present invention, ultraviolet irradiation is performed simultaneously with ozone fumigation.

[0014] Compared with the prior art, the present invention has the following beneficial effects:

[0015] The present invention proves that ozone fumigation supplemented with ultraviolet irradiation can accelerate the aging of mugwort leaves, provides a method for aging mugwort leaves, and provides more feasibility for solving the problems of large space occupation, long occupancy time, high capital occupation, and high quality maintenance cost of mugwort storage sites caused by the slow traditional aging process. Accelerate the research on mugwort aging technology and use modern technology to accelerate the aging process of mugwort leaves, providing more feasibility for solving the problems of long site occupation time and high quality maintenance cost caused by the slow traditional aging process. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] Figure 1 A is the zero cycle of Artemisia argyi 0 Microscopic identification of powder; 1 in the picture is T-shaped hair, 2 is uniseriate non-glandular hair, 3 is pore, and 4 is calcium oxalate cluster crystal.

[0017] Figure 2 Thin layer chromatogram.

[0018] Figure 3 Mixed reference substance and Artemisia argyi zero cycle A 0 High performance liquid chromatogram of the sample; Figure 3 A in the figure represents the HPLC chromatogram of the mixed reference substance; Figure 3 The B in it represents the zero cycle A of Artemisia argyi 0 HPLC chromatogram of the samples.

[0019] Figure 4 This is the linear relationship diagram of chlorogenic acid.

[0020] Figure 5 This is the linear relationship diagram of 3,5-dicaffeoylquinic acid.

[0021] Figure 6 This is the linear relationship diagram of brown cyanidin.

[0022] Figure 7 This is the linear relationship diagram of isoeilflavin.

[0023] Figure 8 Processing of mugwort leaves for one cycle A 1 HPLC chromatogram of the assay.

[0024] Fig. 9 For the second cycle of mugwort treatment A 2 HPLC chromatogram of the assay.

[0025] Fig.10 Three cycles of treatment for mugwort A 3 HPLC chromatogram of the assay.

[0026] Fig.11 Processing Phase IV A for Artemisia argyi 4 HPLC chromatogram of the assay.

[0027] Fig.12 Five cycles of treatment of mugwort leaves A 5 HPLC chromatogram of the assay. DETAILED DESCRIPTION

[0028] The present invention is described in detail below in conjunction with specific examples, but it should not be construed as limiting the present invention. Unless otherwise specified, the technical means used in the following examples are conventional means well known to those skilled in the art, and the materials, reagents, etc. used in the following examples, unless otherwise specified, can be obtained from commercial sources.

[0029] 1. Materials and reagents

[0030] Table 1 Materials and reagents

[0031] name Batch No. / Specification factory Artemisia argyi - Xinyang Shen'ai Agricultural Development Co., Ltd. Isozepin 000863-202312 / reference substance Jiangxi Herborist Biotechnology Co., Ltd. 3,5-Di-caffeoylquinic acid 000318-202209 / reference Jiangxi Herborist Biotechnology Co., Ltd. Borneol 190031-202007 / reference Jiangxi Herborist Biotechnology Co., Ltd. Eucalyptus nkL-01435240101 / Control Chengdu Sodium Columbium Lithium Biotechnology Co., Ltd. Toluene Analytical grade Tianjin Aopusheng Chemical Co., Ltd. Methanol Analytical grade Zhengzhou Piney Chemical Reagent Factory Methanol Chromatographic pure Tianjin Komiou Chemical Reagent Co., Ltd. Acetonitrile Chromatographic pure Zhengzhou Piney Chemical Reagent Factory Anhydrous ethanol Analytical grade Zhengzhou Piney Chemical Reagent Factory Ether Analytical grade Shanghai Malu Pharmaceutical Factory Ethyl acetate Analytical grade Tianjin Aopusheng Chemical Co., Ltd. 95% ethanol Analytical grade Zhengzhou Piney Chemical Reagent Factory n-Hexane Analytical grade Tianjin Aopusheng Chemical Co., Ltd. Petroleum ether (60-90℃) analysis Analytical grade Tianjin Aopusheng Chemical Co., Ltd. Vanillin Analytical grade Tianjin Komiou Chemical Reagent Development Center sulfuric acid 20231030 / Analytical grade Wuhan Zhongtian Chemical Co., Ltd. Ashless filter paper 16946859 Shanghai Weixi Biotechnology Co., Ltd.

[0032] 2. Experimental instruments

[0033] Table 2 Experimental instruments

[0034] name model factory Electron microscopy Primo Star Carl Zeiss Suzhou Co., Ltd. Gas chromatography-mass spectrometry TRACE1310-ISQ7000 Thermo Fisher Scientific High performance liquid chromatography L600-DP6 Beijing Puxi General Instrument Co., Ltd. Ultrasonic Cleaner KQ-500DE Kunshan Ultrasonic Instrument Co., Ltd. High speed Chinese medicine grinder LG-01 Ruian Baixin Pharmaceutical Machinery Co., Ltd. refrigerator BCD-555WKM Hefei Midea Royalstar Refrigerator Co., Ltd. Clean bench SW-CJ-1D Suzhou Purification Equipment Co., Ltd. Ozone disinfection machine FL-805N Shenzhen Feili Electrical Technology Co., Ltd. Thermostatic heating jacket ZGar Beijing Yongguangming Medical Instrument Co., Ltd. Electronic balance (0.0001g) FA2004 Shanghai Puchun Measuring Instrument Co., Ltd. Electronic balance (0.001g) FCS-10C Shanghai Yueping Scientific Instrument Co., Ltd. Electric heating blast drying oven 101-3B Zhejiang Lichen Instrument Technology Co., Ltd.

[0035] Embodiment 1: A kind of method of aging wormwood leaf

[0036] 1. Test methods

[0037] The medicinal material used in the present invention is Xinyang mugwort leaves produced in 2023, which are identified as dried leaves of Artemisia argyiLevL.et Vant. of the Asteraceae family.

[0038] Aged mugwort leaves are obtained by subjecting mugwort leaves to ozone fumigation treatment. The specific method is as follows: ozone fumigation is carried out in a closed environment, and ozone is produced by an ozone disinfector to maintain the ozone concentration in the closed environment at 0.6±0.05ppm. One cycle is seven days. Every morning, ozone fumigation treatment is supplemented by ultraviolet light irradiation (ultraviolet light intensity is 30W), ozone treatment for 2h, ultraviolet light irradiation for 0.5h, and ozone fumigation treatment is supplemented by ultraviolet light irradiation (ultraviolet light intensity is 30W) in the afternoon, ozone treatment for 2h, ultraviolet light irradiation for 0.5h, and the interval between morning and afternoon treatments is 6h. Ozone production is stopped for the remaining time, and a total of 5 cycles are processed. The zero cycle is before the mugwort leaves are treated, the first cycle is the first treatment, followed by the second cycle, the third cycle, the fourth cycle, the fifth cycle... and so on, and are numbered A respectively. 0 , A 1 , A 2 , A 3 , A 4 , A 5 ...in A 0 , A 1 , A 2 , A 3 , A 4 , A 5 …and take samples for quality evaluation.

[0039] 2. Analysis

[0040] The ozone fumigation of different periods of moxa leaves (A 0 , A 1 , A 2 , A 3 , A 4 , A 5 ……) and naturally aged wormwood leaves for index component determination. High performance liquid chromatography was used to determine the total flavonoids content, gas chromatography was used to determine the borneol and eucalyptol content, and gas chromatography-mass spectrometry was used to analyze the composition of volatile oil components. The determination data were analyzed and compared with the content change trend of index components in naturally aged wormwood leaves to determine whether the wormwood leaves were aged.

[0041] 3. Quality inspection of mugwort leaves

[0042] (1) Microscopic identification

[0043] According to the 2020 edition of the Pharmacopoeia of the People's Republic of China, the zero cycle A 0 Conduct microscopic identification. Figure 1 As shown in the figure, under microscope observation, there are three types of microscopic features of Artemisia argyi, namely non-glandular hairs (T-shaped hairs and uniseriate non-glandular hairs), stomata and calcium oxalate clusters, which are in line with the provisions of the pharmacopoeia.

[0044] (2) Thin layer chromatography identification

[0045] Identification was carried out according to the thin layer chromatography method in Part 4 of the 2020 edition of the Pharmacopoeia of the People's Republic of China.

[0046] Preparation of test solution: Take A 0 , A 1 , A 2 , A 3 , A 4 , A 5 Take 2g of each powder, add 25mL of petroleum ether (60-90℃), heat under reflux in a water bath for 30min, filter, evaporate to dryness, add 1mL of n-hexane to the residue to dissolve it, and use it as the test sample.

[0047] Method: Use a spotting capillary to absorb the above 6 solutions, spot the samples, use petroleum ether (60-90℃)-toluene-acetone (10:8:0.5) as the developing agent, develop, dry, spray with 1% vanillin sulfuric acid solution, and heat at 105℃ until the spots are clearly colored.

[0048] like Figure 2 As shown in the figure, the TLC results show that, under the same sample amount, the main spots of the same color appear in the chromatogram of the test sample and at the corresponding position of the chromatogram of the control medicinal material, which are in line with the provisions of the pharmacopoeia.

[0049] (3) Determination of moisture content, total ash content, and acid-insoluble ash content of mugwort leaves

[0050] The determination is carried out according to the provisions of the 2020 edition of the Pharmacopoeia of the People's Republic of China.

[0051] Table 3 Moisture content of mugwort leaves

[0052]

[0053]

[0054] The results are shown in Table 3. 0 , A 1 , A 2 , A 3 , A 4 , A 5 The water contents are 9.64%, 8.19%, 8.38%, 7.29%, 6.25% and 6.80% respectively, all not exceeding 15.0%, which is in line with the requirements of the Pharmacopoeia.

[0055] Table 4 Total ash content of Artemisia argyi

[0056] Test product name Test sample weight (g) Crucible weight after ashing (g) Total ash weight (g) Total ash (%) <![CDATA[A 0 ]]> 3.5939 28.0298 0.3252 9.05 <![CDATA[A 1 ]]> 3.5482 29.0852 0.3046 8.58 <![CDATA[A 2 ]]> 3.5548 28.5923 0.3470 9.76 <![CDATA[A 3 ]]> 3.5622 28.7095 0.3132 8.79 <![CDATA[A 4 ]]> 3.6114 28.1405 0.3038 8.41 <![CDATA[A 5 ]]> 3.5618 27.6890 0.2962 8.32

[0057] The results are shown in Table 4. By calculation, we can get A 0 , A 1 , A 2 , A3 , A 4 , A 5 The total ash contents were 9.05%, 8.58%, 9.76%, 8.79%, 8.41% and 8.32% respectively, all not exceeding 12.0%, which is in compliance with the requirements of the pharmacopoeia.

[0058] Table 5 Insoluble ash content of folate

[0059]

[0060] The results are shown in Table 5. By calculation, we can get A 0 , A 1 , A 2 , A 3 , A 4 , A 5 The insoluble ash contents are 1.06%, 0.36%, 0.21%, 0.26%, 0.25% and 0.17% respectively, all of which do not exceed 3.0%, which is in line with the requirements of the Pharmacopoeia.

[0061] (4) Determination of Artemisia argyi content by gas chromatography

[0062] 1) Chromatographic conditions

[0063] 50% phenyl-methylpolysiloxane was used as the stationary phase (column length was 30m, inner diameter was 0.25mm, and film thickness was 0.25μm); the column temperature was programmed, with an initial temperature of 45°C, and then increased to 75°C at a rate of 2°C per minute, and maintained for 5min; then increased to 90°C at a rate of 1°C per minute, and maintained for 6min; then increased to 150°C at a rate of 5°C per minute; finally increased to 250°C at a rate of 10°C per minute, and maintained for 5min, with the injection port temperature at 240°C; and the detector temperature at 250°C. The flow rate was 0.6mL per minute, split injection, and the split ratio was 5:1.

[0064] 2) Preparation of reference solution

[0065] Take appropriate amounts of eucalyptol reference substance and borneol reference substance, weigh them accurately, and add ethyl acetate to prepare a mixed solution containing 0.2 mg of eucalyptol and 0.1 mg of borneol per 1 mL.

[0066] 3) Sample solution preparation

[0067] Take Artemisia argyi A 0 , A 1 , A 2 , A 3 , A 4 , A 5Take an appropriate amount, cut into pieces of about 0.5 cm, take about 2.5 g, weigh accurately, put in a round-bottom flask, add 300 mL of water, and connect to a volatile oil analyzer. Extract according to the requirements of the 2020 edition of the Pharmacopoeia of the People's Republic of China.

[0068] 4) Determination

[0069] Accurately pipette 1 μL of the reference solution and the test solution respectively, inject into the gas chromatograph for determination.

[0070] Table 6 Eucalyptus globulus oil and borneol content

[0071] Test product name <![CDATA[A 0 (%)]]> <![CDATA[A 1 (%)]]> <![CDATA[A 2 (%)]]> <![CDATA[A 3 (%)]]> <![CDATA[A 4 (%)]]> <![CDATA[A 5 (%)]]> Eucalyptus 0.225 0.112 0.170 0.213 0.182 0.245 Borneol 0.039 0.060 0.054 0.070 0.094 0.077

[0072] The 2020 edition of the Pharmacopoeia of the People's Republic of China requires that the content of eucalyptol shall not be less than 0.050% and the content of borneol shall not be less than 0.020% based on the dry product. As shown in Table 6, both the treated and untreated products meet the requirements of the 2020 edition of the Pharmacopoeia of the People's Republic of China.

[0073] 4. Determination of flavonoids content in Artemisia argyi by HPLC

[0074] (1) Preparation of test samples

[0075] Preparation of reference solution: Accurately weigh appropriate amounts of chlorogenic acid, 3,5-dicaffeoylquinic acid, cyanidin, and isoeupretinoic acid reference substances, and add chromatographic methanol to prepare mixed reference solutions with concentrations of 28.8 μg / mL, 88.0 μg / mL, 8.3 μg / mL, and 34.2 μg / mL for chlorogenic acid, 3,5-dicaffeoylquinic acid, cyanidin, and isoeupretinoic acid, respectively, for use.

[0076] Preparation of sample solution: Accurately weigh about 0.5 g of each wormwood powder (passed through a 60-mesh sieve) and place it in a stoppered conical flask. Accurately add 15 mL of 75% methanol by volume and weigh the solution. After ultrasonic extraction for 0.5 h, weigh the solution and add 75% methanol to make up the weight. Shake well, let it stand, and pipette the supernatant through a 0.45 μm microporous filter membrane to obtain the solution.

[0077] (2) Content determination

[0078] Chromatographic conditions and system suitability test: The chromatographic column is Omega PoLar 100-5-C 18Chromatographic column (4.6×250mm, 3μm); mobile phase: acetonitrile (A)-0.2% phosphoric acid water (B), gradient elution (0-3min, 17%A; 3-15min, 17%A→24%A; 15-18min, 24%A; 18-35min, 24%A→28%A; 35-40min, 28%A→48%A; 40-55min, 48%A→63%A; 55-60min, 63%A→90%A); flow rate: 0.6mL / min; column temperature: 35℃; detection wavelength: 330nm; running time: 60min. Under this chromatographic condition, chlorogenic acid, 3,5-dicaffeoylquinic acid, cyanidin, and isoeupretinoic acid were well separated from each other and achieved baseline separation with other components, as shown in Figure 2. Figure 3 .

[0079] (3) Linear relationship investigation

[0080] Accurately pipette 0.2, 0.5, 1.0, 1.5, 2.0, 3.0, and 4.0 mL of the mixed reference stock solution prepared in "(1)" into a 10 mL volumetric flask, dilute to the mark with methanol, and mix. Accurately pipette appropriate amounts of the above series of solutions, and perform injection analysis according to the chromatographic conditions under "(2)". Regression analysis was performed with the mass concentration (X, μg / mL) of the four components as the horizontal axis and the peak area (Y) as the vertical axis. The results are shown in Table 1. Figure 4 , Figure 5 , Figure 6 , Figure 7 , Table 7.

[0081] Table 7 Linear relationship investigation

[0082]

[0083] (4) Precision test

[0084] The same sample solution was accurately pipetted and injected six times continuously under the conditions in item (2). The RSD of the peak area is shown in Table 8. The results show that the precision of the instrument is good.

[0085] (5) Stability test

[0086] The same sample solution was accurately pipetted and injected at 0, 2, 4, 8, and 12 h after preparation, respectively. The injections were continued under the conditions in (2). The RSD of the peak area is shown in Table 8. The results showed that the sample solution was stable within 12 h.

[0087] (6) Repeatability test

[0088] Accurately weigh 6 portions of mugwort powder to prepare sample solutions. Samples were injected according to the conditions in item (2), and the peak areas were recorded to calculate the contents. The average contents of the four components to be tested (chlorogenic acid, 3,5-dicaffeoylquinic acid, cyanidin, and isocyanidin) were 3.473 mg / g, 9.038 mg / g, 1.073 mg / g, and 3.151 mg / g, respectively, and the RSDs were all less than 3.0%, indicating that the method had good repeatability. The RSDs of the contents are shown in Table 8.

[0089] Table 8 Results of precision, stability and repeatability of the four components in Artemisia argyi

[0090] Compound Precision RSD (%) Stability RSD (%) Repeatability RSD (%) Chlorogenic acid 1.22 1.47 1.06 3,5-Di caffeoylquinic acid 0.98 1.12 1.05 Brown cyanidin 1.36 1.55 1.12 Isozepin 1.74 1.69 1.51

[0091] (7) Recovery test

[0092] Weigh about 0.05g of wormwood powder with known content (chlorogenic acid content is 3.473mg / g, 3,5-dicaffeoylquinic acid is 9.038mg / g, cyanidin is 1.073mg / g, and tangeretin is 3.151mg / g), a total of 6 portions, accurately weigh, and place in a 50mL stoppered conical flask, accurately add 20.0mL of 75% methanol, and then accurately add 5.0mL of mixed reference substances with concentrations of chlorogenic acid, 3,5-dicaffeoylquinic acid, cyanidin, and isoeupretinoic acid of 28.8μg / mL, 88.0μg / mL, 8.3μg / mL, and 34.2μg / mL, respectively. Prepare the sample solution according to the preparation method under (2). The determination was carried out under the conditions of item (2) and the average recovery and RSD of each component were calculated. See Table 9. The average recovery of the four components was between 98.63% and 100.67%, and the RSD was less than 3.0%. The results showed that the accuracy of the method was good.

[0093] Table 9: Sample recovery test of 4 components in Artemisia argyi (n=6)

[0094]

[0095]

[0096] (8) Sample measurement

[0097] Sample content determination: Accurately weigh 6 portions of untreated mugwort powder and mugwort powder treated with ozone for different periods of time, prepare sample solutions, and analyze and determine under the conditions under (2), such as Figure 8 , Fig. 9 , Fig.10 , Fig.11 , Fig.12 . Calculate the content and see the results in Table 10.

[0098] Table 10 Determination results of chlorogenic acid, 3,5-dicaffeoylquinic acid, cyanidin and isoeupretinoic acid in Artemisia argyi

[0099]

[0100] Studies have shown that the total flavonoid content of wormwood in different years gradually increases with the extension of storage time, reaches a peak in the third year, and then drops sharply. As shown in Table 10, with the increase in the number of ozone fumigation treatments, total flavonoids gradually increase, and the content of some flavonoids decreases in the fifth cycle, which is the same as the change trend of naturally aged wormwood. It shows that wormwood completes aging during ozone fumigation. Ozone fumigation is an effective means to accelerate the aging of wormwood. Pharmacological studies have now proved that the total flavonoids in wormwood have good antioxidant, anti-inflammatory, free radical scavenging and effective effects of preventing lipid peroxidation from causing cell damage, and the adverse reactions are small, and it is expected to be better developed and applied. Therefore, the present invention uses flavonoids as the main indicator component of wormwood aging to investigate, and ozone fumigation treatment of wormwood is equivalent to three years of natural aging of wormwood in four cycles. That is, ozone fumigation of wormwood for 28d is equivalent to the aging effect of natural aging for 1095d.

[0101] 5. GC-MC determination of volatile oil components

[0102] (1) Extraction of volatile oil from Artemisia argyi

[0103] Grind the mugwort leaves into coarse powder, accurately weigh 300g, put it in a 5L round-bottom flask, add 3000mL of purified water according to the solid-liquid ratio of 1:10, then connect it to a Soxhlet extractor, soak for 2h, place it in an electric heating mantle and reflux and heat it to boiling, keep it at a slight boiling for about 5h, until the amount of oil in the measuring device no longer increases, stop heating, slowly release the water to separate the volatile oil, dry it with anhydrous sodium sulfate after separation, and label it in batches (A 0 , A 1 , A 2 , A 3 , A 4 , A 5 , B 0 , B 1 , B 0 For the wormwood leaves that have been naturally aged for one year in 2022, B 1 The 2022 mugwort leaves were fumigated for one cycle in April 2024 according to the above-mentioned ozone fumigation method) and placed in brown glass bottles and stored at 4°C for later use.

[0104] (2) GC-MS analysis conditions

[0105] Instrument: Headspace (TriPlus300) gas chromatography (TRACE1310) mass spectrometry (ISQ7000) coupling instrument (Thermo Fisher Scientific, USA), Chromeleon7.2 data processing system.

[0106] Gas chromatography conditions: 50% phenyl-methylpolysiloxane as stationary phase (column length 30m, inner diameter 0.25mm, film thickness 0.25μm); column temperature program, initial temperature 45℃, temperature rise to 75℃ at a rate of 2℃ per minute, keep for 5min; then temperature rise to 90℃ at a rate of 1℃ per minute, keep for 6min; then temperature rise to 150℃ at a rate of 5℃ per minute; finally temperature rise to 250℃ at a rate of 10℃ per minute, keep for 5min, injection port temperature 240℃; detector temperature 250℃. Flow rate 0.6mL per minute, split injection, split ratio 5:1.

[0107] Mass spectrometry conditions: select EI electron source with electron energy of 70ev, ion source temperature of 250℃, mass scanning range: 50-550m / z. The mass spectrometry standard library was used for chemical component identification, and the peak area normalization method was used for quantification to measure the normalized content of each chemical component in volatile oil of Artemisia argyi.

[0108] (3) Experimental results and analysis

[0109] The extracted volatile oil of Artemisia argyi was subjected to gas chromatography-mass spectrometry analysis according to the GC-MS analysis method (2) and compared with the standard NIST spectral library to obtain the chemical components and their normalized contents in the volatile oil as shown in Table 11.

[0110] Table 11 Chemical composition analysis of volatile oil of Artemisia argyi

[0111]

[0112]

[0113] Experiments have shown that the types and contents of volatile oil components in wormwood vary greatly during natural aging. From the data in Table 11, it can be seen that the types and contents of volatile oil in wormwood after ozone fumigation have changed, which is consistent with the changes in wormwood after natural aging. Ozone fumigation did not cause significant changes in the types and contents of volatile oil in wormwood, indicating that this accelerated aging method is feasible.

[0114] Through microscopic identification and thin layer chromatography identification of mugwort leaves treated with ozone fumigation at different treatment cycles, it was found that ozone fumigation did not affect the identification results of mugwort leaves. Through the detection of moisture, total ash, acid-insoluble ash and volatile oil content, it was found that the above quality indicators all changed with the extension of treatment time, but all quality evaluation indicators met the requirements of the Chinese Pharmacopoeia. The contents of four representative components in mugwort samples were determined by high performance liquid chromatography. The phenolic acid and flavonoids in mugwort leaves that play a pharmacological role gradually increased, that is, the phenolic acid and flavonoids in mugwort leaves treated with ozone fumigation gradually increased with the increase in the number of treatments, which was the same as the change trend of the phenolic acid and flavonoids in naturally aged mugwort leaves. It shows that ozone fumigation can be used to accelerate the aging of mugwort leaves. The types and contents of volatile oils were determined by GC-MS, and it was found that there was no significant change in the types and contents of volatile oils, and the types and contents of volatile oils in naturally aged mugwort leaves of different years changed. Volatile oils, phenolic acids and flavonoids are all active ingredients of mugwort leaves, and their contents affect the efficacy of mugwort leaves.

[0115] The present invention proves that ozone fumigation can age mugwort leaves, provides a method for aging mugwort leaves, and provides more feasibility for solving the problems of large space occupied by mugwort storage sites, long occupancy time, high capital occupation, and high quality maintenance costs caused by the slow traditional aging process. Accelerate the research on mugwort aging technology and use modern technology to accelerate the aging process of mugwort leaves, providing more feasibility for solving the above problems caused by the slow traditional aging process.

[0116] Obviously, those skilled in the art can make various changes and modifications to the present invention without departing from the spirit and scope of the present invention. Thus, if these modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include these modifications and variations.

Claims

1. A method for aging wormwood leaves, characterized in that: include: In a closed environment, ozone is used to fumigate the mugwort leaves, supplemented by ultraviolet irradiation, twice a day for 25 to 35 days; Each treatment lasts for 110 to 130 minutes of ozone fumigation and 25 to 35 minutes of ultraviolet irradiation.

2. The method for aging wormwood leaves according to claim 1, characterized in that: The wormwood leaf is dried wormwood leaf.

3. The method for aging wormwood leaves according to claim 1, characterized in that: During ozone fumigation, the ozone concentration in the closed environment is maintained at 0.5ppm~0.8ppm.

4. The method for aging wormwood leaves according to claim 1, characterized in that: The ultraviolet light intensity is 25W~35W.

5. The method for aging wormwood leaves according to claim 1, characterized in that: The interval between two treatments per day is 6 to 8 hours.

6. The method for aging wormwood leaves according to claim 1, characterized in that: UV irradiation is carried out simultaneously with ozone fumigation.

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