Detection process for moxa smoke components in moxibustion, corollary equipment and use method of corollary equipment

Abstract

The invention discloses a process for detecting moxa smoke components in moxa-moxibustion in the technical field of moxa smoke component detection, which comprises the following steps: using gas chromatography conditions: a chromatographic column SH-RTx-5 quartz elastic capillary column (30.0 m * 0.25 mm * 0.25 mu m), a split ratio of 1: 55, a flow rate of 1.0 mL.min <-1 >, carrier gas of high-purity helium (99.999%) and a temperature of a sample inlet of 250 DEG C, carrying out temperature programming: keeping the initial temperature of a column box at 60 DEG C for 2 minutes, raising the temperature to 120 DEG C at a speed of 5 DEG C. Min <-1 >, keeping the temperature for 5 minutes, and carrying out temperature programming; the temperature is increased to 230 DEG C at the speed of 10 DEG C / min, the temperature is kept for 10 min, the mass spectrum conditions are that an EI ion source is adopted, the electron energy is 70 eV, the ion source temperature is 230 DEG C, the transmission line temperature is 250 DEG C, the detection ion mass scanning range is 33-500 amu, the sample size is 1 uL, and the solvent delay is 5 min, the extracted moxa smoke is detected through a GC-MS method, and the chemical structure is analyzed. According to the method, the detection process is optimized, and the method can be used for determining the quality standard of moxa / wormwood, so that preliminary experimental data and theoretical basis are provided for popularization and application of moxibustion therapy.

Description

Technical Field

[0001] The present invention relates to the technical field of moxa smoke component detection, and in particular to a moxa smoke component detection process and supporting equipment and a method of using the same. Background Art

[0002] Artemisia argyi H.Lév.&Vaniot, also known as mugwort, is a perennial herb or slightly semi-shrubby plant of the genus Artemisia in the Asteraceae family. The taproot is obvious, slightly thick and long, with many lateral roots, and the underground rhizomes are horizontal; the head inflorescence is oval, sessile or nearly sessile, and the achenes are long ovate or oblong; the stem is solitary or a few, and the plant has a strong aroma; the leaves are grayish-white short soft hairs, with white glandular dots and small pits. Mugwort is widely distributed in nature, growing all over the country and neighboring Asian countries. In China, it is mainly distributed in Guizhou, Hubei, Jilin, Yunnan, Shandong, Gansu, Jiangsu, Zhejiang and other places. Most of them grow in wild wastelands, roadsides, rivers and hillsides at relatively low altitudes and medium and high altitudes. Mugwort wool is a soft and fine cotton-like substance obtained by repeatedly drying, pestling, pounding, and crushing the white side of the mugwort leaves to remove debris and dust. Moxa is the raw material for making moxa sticks and moxa cones, and is also the main material used in moxibustion therapy.

[0003] Moxa smoke, which is the smoke produced after the burning of moxa leaves, is the substance that exerts medicinal effects in moxibustion. According to research, moxa smoke has many pharmacological effects, such as antibacterial disinfection, immune regulation, anti-aging, blood lipid regulation, anti-asthma, anti-allergy, anti-tumor, etc. It can be seen that moxa smoke plays an important role in moxibustion therapy that cannot be ignored. Studies have shown that the mechanism of moxibustion is the thermal stimulation and drug penetration of moxa smoke on the meridians and acupoints of the human body. These drug components should come from the incomplete combustion products of moxa leaves, volatile oils of moxa leaves and their oxidation products. Some people have analyzed the chemical composition of moxa smoke by benzene-methanol mixed solvent extraction and GC-MS method, and obtained 20 identifiable components.

[0004] To this end, this application develops a set of detection processes for the components of moxa smoke in moxibustion and optimizes the process, which can be used to determine the quality standards of moxa wool / moxa grass, and further provide preliminary experimental data and theoretical basis for the promotion and application of moxibustion therapy. Summary of the invention

[0005] The present invention aims to provide a process for detecting components of moxa smoke in moxibustion, supporting equipment and a method of using the same. By optimizing the process, it can be used to determine the quality standard of moxa wool / moxa grass.

[0006] In order to achieve the above object, the present invention provides the following technical solutions:

[0007] A process for detecting components of moxa smoke in moxibustion is disclosed. The process uses a GC-MS method with the following conditions: a chromatographic column SH-RTx-5 quartz elastic capillary column (30.0 m×0.25 mm×0.25 μm), a split ratio of 1:55, a flow rate of 1.0 mL·min-1, a carrier gas of high-purity helium (99.999%), an injection port temperature of 250° C., a program temperature rise: an initial column box temperature of 60° C. is maintained for 2 min, the temperature is increased to 120° C. at a rate of 5° C.·min-1 and maintained for 5 min, and then the temperature is increased to 230° C. at a rate of 10° C.·min-1 and maintained for 10 min. The mass spectrometry conditions include an EI ion source, an electron energy of 70 eV, an ion source temperature of 230° C., a transmission line temperature of 250° C., a detection ion mass scanning range of 33 to 500 amu, an injection volume of 1 uL, and a solvent delay of 5 min to detect the extracted moxa smoke and analyze the chemical structure.

[0008] A supporting device includes a peristaltic pump, a smoke collector and a control device. The peristaltic pump includes an input end and an output end. The smoke collector includes a collecting bottle, a combustion chamber and an extraction bottle arranged in the collecting bottle. A conduit is connected between the combustion chamber and the extraction bottle, and between the collecting bottle and the input end of the peristaltic pump. The control device is used to control the operation of the peristaltic pump. The output end of the peristaltic pump outputs smoke for detection.

[0009] Furthermore, the control device includes a flow rate adjustment switch, a gas flow direction regulator, a peristaltic pump power main switch, a flow rate direction display, a flow rate display, and a manual / automatic working mode switching switch.

[0010] A method for using a supporting device, characterized in that: it includes:

[0011] S1. Use the front conduit to connect the input end of the peristaltic pump and the smoke collector, turn on the main power switch of the peristaltic pump, adjust the flow rate and gas flow direction through the flow rate adjustment switch and the gas flow direction regulator, and check for leaks;

[0012] S2. After checking that everything is correct, add the extractant into the extraction bottle, place the moxa in the combustion chamber, ignite the moxa, and start collecting the moxa smoke for testing.

[0013] Furthermore, the moxa is pretreated before combustion, and the pretreatment process includes: ozone accelerated aging of the moxa, moxa fungus treatment, and the use of moxa from different years and different origins. BRIEF DESCRIPTION OF THE DRAWINGS

[0014] Figure 1 It is a structural schematic diagram of the supporting device;

[0015] Figure 2 This is a comparison chart of UV spectrum;

[0016] Figure 3 To detect the total ion current;

[0017] Figure 4 The total ion current diagram of moxa smoke from moxa burning in different years detected by gas chromatography-mass spectrometry;

[0018] Figure 5 To accelerate the aging of moxa smoke from burning moxa at different times, the total ion current was detected by gas chromatography-mass spectrometry;

[0019] Figure 6 This is the total ion current diagram of the moxa smoke burned after adding different bacteria treatment using gas chromatography-mass spectrometry. DETAILED DESCRIPTION

[0020] The following is further described in detail through specific implementation methods:

[0021] The figure marks in the drawings of the specification include: combustion chamber 1, catheter 2, collecting bottle 3, syringe bottle 4, flow rate adjustment switch 5, gas flow direction regulator 6, flow rate display 7, manual / automatic working mode switching switch 8, peristaltic pump main power switch 9, flow rate direction display 10, peristaltic pump 11.

[0022] Embodiment: A supporting device, such as Figure 1 As shown, it includes a peristaltic pump, a smoke collector and a control device, the peristaltic pump includes an input end and an output end; the smoke collector includes a collecting bottle, a combustion chamber and an extraction bottle arranged in the collecting bottle, and conduits are connected between the combustion chamber and the extraction bottle, and between the collecting bottle and the input end of the peristaltic pump. The control device is used to control the operation of the peristaltic pump, and the output end of the peristaltic pump outputs smoke for detection.

[0023] The method of using the device is as follows:

[0024] S1. Use the front conduit to connect the input end of the peristaltic pump and the smoke collector, turn on the main power switch of the peristaltic pump, adjust the flow rate and gas flow direction through the flow rate adjustment switch and the gas flow direction regulator, and check for leaks;

[0025] S2. After checking that everything is correct, add the extractant into the extraction bottle, place the moxa in the combustion chamber, ignite the moxa, and start collecting the moxa smoke for testing.

[0026] (1) Extraction solvent screening experiment

[0027] The pre-selected reagents were sequentially loaded into a vial, placed inside a smoke collector, and the moxa smoke obtained after burning moxa was passed into the vial. Five solvents with different polarities were used for collection, and the polarity was as follows: water>DMF (dimethylformamide)>anhydrous ethanol>n-butanol>ethyl acetate; the five extracts were concentrated using a rotary evaporator, filtered with a 0.22μm organic phase filter membrane, and scanned with a UV-visible spectrophotometer. Comprehensive evaluation was performed based on the detected UV absorption range and absorbance, so as to select the most suitable extractant.

[0028] from Figure 2 It can be seen from the full spectrum scanned by UV-visible spectrophotometer that within the same spectrum range, the absorbance values ​​of n-butanol and anhydrous ethanol are larger and the UV absorption range is wider. Comparing anhydrous ethanol with n-butanol, anhydrous ethanol is more volatile and unstable, so n-butanol solution is selected as the optimal extraction agent.

[0029] (2) GC-MS method

[0030] The gas chromatography conditions used were: chromatographic column SH-RTx-5 quartz elastic capillary column (30.0m×0.25mm×0.25μm), split ratio 1:55, flow rate 1.0mL·min-1, carrier gas was high-purity helium (99.999%), injection port temperature 250℃, programmed temperature rise: the initial column box temperature was 60℃ and maintained for 2min, then increased to 120℃ at 5℃·min-1 and maintained for 5min, then increased to 230℃ at 10℃·min-1 and maintained for 10min, mass spectrometry conditions: EI ion source, electron energy 70eV, ion source temperature 230℃, transmission line temperature 250℃, detection ion mass scanning range 33~500amu, injection volume: 1uL, solvent delay: 5min. The GC-MS method was used to detect the extracted moxa smoke and analyze the chemical structure.

[0031] (3) Analysis of chemical components of moxa smoke produced by burning moxa from different origins

[0032] Randomly select 10 portions of moxa from different origins, first take 1 portion of moxa, weigh 2.0g and put it into the combustion chamber for combustion, and pass the obtained moxa smoke into a vial containing 8mL of n-butanol solution. After all the moxa is burned, concentrate the collected sample solution to 1.5mL at 75℃ on a rotary evaporator, filter the concentrate with an organic phase filter membrane, and finally use a gas chromatography-mass spectrometer for detection and analysis. The remaining 9 portions of moxa are operated in the same way as above.

[0033] The moxa smoke produced by burning moxa samples from 10 different origins was tested, and the total ion flow diagram was as follows: Figure 3As shown in the figure, by searching the NIST17 database and consulting relevant literature for qualitative analysis, a total of 92 chemical components were detected in the moxa smoke produced by burning moxa, of which 3 chemical components, including phenol, cyclohexenone and o-cresol, were common components in 10 different origins. Seven chemical components, including cyclopentanone and o-cresol, were common in more than 8 different origins. A total of 46 chemical components can be used for medical treatment, and the percentage of each component is shown in Table 1.

[0034] Table 1 - Ingredient percentage chart

[0035]

[0036]

[0037]

[0038]

[0039] To summarize the above test results, the chemical components detected by GC-MS method of moxa smoke produced by burning moxa are mainly phenol, acid, amine, ketone, aldehyde, ester and other types of compounds. The unique chemical component amphetamine in Guizhou moxa samples has a significant excitatory effect on the human central nervous system and is the prototype of synthetic amphetamine drugs. The common chemical component phenol can be used for skin sterilization, itching and acute otitis media, and has certain antioxidant, antibacterial and anti-inflammatory, whitening and spot-removing effects. Indole and 2,6-dimethoxybenzene are aroma components, and neophytadiene is used in various flavors and fragrances. Furan and other food flavoring ingredients are also detected.

[0040] (4) Analysis of chemical composition of moxa smoke produced by moxa burning in different years

[0041] Take 2.0g of new mugwort, three-year-old mugwort and five-year-old mugwort from the same origin and put them into the combustion chamber for combustion. The obtained mugwort smoke is passed into a vial containing 8mL of n-butanol solution. After all the mugwort is burned out, the collected sample solution is concentrated to 1.5mL at 75℃ on a rotary evaporator, and the concentrated solution is filtered through an organic phase filter membrane, and finally detected and analyzed using a gas chromatography-mass spectrometer.

[0042] The moxa smoke produced by burning moxa samples from the same origin in three different years was tested. The total ion flow diagram is as follows: Figure 4 As shown in the figure, 37 chemical components were detected in the moxa smoke produced by burning moxa, among which 1-methylpiperidine was the common chemical component of 3 different years. The percentage content of each component is shown in Table 2. The results show that the moxa of 3 years old is the most suitable.

[0043] Table 2 - Ingredient percentage

[0044]

[0045]

[0046] (5) Analysis of chemical components of moxa smoke produced by combustion of moxa wool at different times of ozone accelerated aging

[0047] Take new moxa from a certain place of origin and put it into a container, connect it to an ozone generator with a catheter, pass ozone into the container for accelerated aging, take 2.0g of moxa aged for 4 hours and 8 hours and put it into the combustion chamber for combustion, and pass the obtained moxa smoke into a vial containing 8mL of n-butanol solution. After all the moxa is burned out, concentrate the collected sample solution to 1.5mL at 75℃ on a rotary evaporator, filter the concentrate with an organic phase filter membrane, and finally use a gas chromatograph-mass spectrometer for detection and analysis.

[0048] The moxa smoke produced by the combustion of moxa samples at two different time points after adding ozone to accelerate aging was detected. The total ion current diagram is as follows: Figure 5 As shown, by searching the NIST17 database and consulting relevant literature for qualitative analysis, a total of 40 chemical components were identified in the moxa smoke produced by burning moxa. The most chemical components were detected after accelerated aging for 4 hours. The percentage results of each component are shown in Table 3.

[0049] Table 3 - Results of percentage of each ingredient

[0050]

[0051]

[0052] (6) Analysis of chemical components of moxa smoke produced by burning moxa after adding different bacteria

[0053] Take new moxa from a certain place of origin and put it into a sealed container, add laboratory preserved strains G and H (hydrogen bacteria) and place it at room temperature for 1 month, take 2.0g of moxa wool and put it into the combustion chamber for combustion, and pass the obtained moxa smoke into a vial containing 8mL of n-butanol solution. After all the moxa wool is burned, concentrate the collected sample solution to 1.5mL at 75℃ on a rotary evaporator, filter the concentrate with an organic phase filter membrane, and finally use a gas chromatography-mass spectrometer for detection and analysis.

[0054] The moxa smoke produced by burning moxa samples treated with two different bacteria from the same origin was detected. The total ion current diagram is shown in the figure below. Figure 6 As shown, a total of 33 chemical components were identified in the moxa smoke produced by burning moxa wool. The chemical components detected by adding G bacteria (Gram) treatment were the most, and the percentage content of each component is shown in Table 4.

[0055] Table 4 - Results of percentage of each ingredient

[0056]

[0057] Conclusion: The GC-MS method was used to detect the moxa smoke produced by burning moxa samples from 10 different origins, including Beijing, Henan, Hubei, Ningxia, Fujian, Guizhou, and Guangdong. A total of 92 chemical components were detected, of which 3 chemical components, including phenol, cyclohexenone, and o-methylphenol, were common components in 10 different origins, but the content of the same component in different origins was significantly different. Seven chemical components, including cyclopentanone and o-methylphenol, were common in more than 8 different origins, and a total of 46 chemical components that can be used for medical treatment were detected. The chemical components of moxa smoke produced by burning new moxa, three-year-old moxa, and five-year-old moxa in Guizhou Province were then detected, and a total of 37 chemical components were detected, among which the three-year-old moxa had the most chemical components. After the new moxa in Guizhou Province was aged for 4 hours and 8 hours with ozone, a total of 40 chemical components were detected in the moxa smoke produced by the combustion of the moxa samples at two different time points; finally, the new moxa in Guizhou was treated with G bacteria and H bacteria for the same time, and a total of 33 chemical components were detected in the moxa smoke produced by the combustion of the moxa samples after the two different bacteria were treated. Among them, the moxa smoke treated with G bacteria had the most chemical components. The chemical composition of moxa smoke is very complex. The chemical composition of moxa smoke produced by the same brand, different origins, different processing techniques, and different aging times of moxa has certain differences. The results of this paper also show that the water content, quality, tightness, and burning time of moxa sticks are different.

Claims

1. A process for detecting components of moxa smoke in moxibustion, characterized in that: The moxa smoke produced by burning moxa was extracted using n-butanol solution; the gas chromatography conditions were as follows: chromatographic column SH-RTx-5 quartz elastic capillary column (30.0m×0.25mm×0.25μm), split ratio 1:55, flow rate 1.0mL·min-1, carrier gas was high-purity helium (99.999%), injection port temperature 250℃, programmed temperature rise: the initial column box temperature was 60℃ and maintained for 2min, then increased to 120℃ at 5℃·min-1 and maintained for 5min, then increased to 230℃ at 10℃·min-1 and maintained for 10min, mass spectrometry conditions: EI ion source, electron energy 70eV, ion source temperature of 230℃, transmission line temperature of 250℃, detection ion mass scanning range of 33 to 500amu, injection volume: 1uL, solvent delay: 5min. The extracted moxa smoke was detected by GC-MS method, and the chemical structure was analyzed.

2. A supporting equipment, characterized in that: It comprises a peristaltic pump, a smoke collector and a control device. The peristaltic pump comprises an input end and an output end. The smoke collector comprises a collecting bottle, a combustion chamber and an extraction bottle arranged in the collecting bottle. A conduit is connected between the combustion chamber and the extraction bottle, and between the collecting bottle and the input end of the peristaltic pump. The control device is used to control the operation of the peristaltic pump. The output end of the peristaltic pump outputs smoke for detection.

3. The supporting equipment according to claim 2, characterized in that: The control device comprises a flow rate adjustment switch, a gas flow direction regulator, a peristaltic pump power main switch, a flow rate direction display, a flow rate display, and a manual / automatic working mode switching switch.

4. A method for using a supporting device, characterized in that: include, S1. Use the front conduit to connect the input end of the peristaltic pump and the smoke collector, turn on the main power switch of the peristaltic pump, adjust the flow rate and gas flow direction through the flow rate adjustment switch and the gas flow direction regulator, and check for leaks; S2. After checking that everything is correct, add the extractant into the extraction bottle, place the moxa in the combustion chamber, ignite the moxa, and start collecting the moxa smoke for testing.

5. The process for detecting moxa smoke components in moxibustion according to claim 4, characterized in that: The moxa is pretreated before combustion, and the pretreatment process includes: accelerating aging of the moxa with ozone, treating the moxa with moxa fungi, and using moxa from different years and from different origins.

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