Moxa stick combustion smoke absorption device and GC-MS (Gas Chromatography-Mass Spectrometer) combined direct sample injection analysis method thereof

Abstract

The invention discloses a moxa stick combustion smoke absorption device and a GC-MS. The moxa stick combustion smoke absorption device comprises a gas supply unit used for providing combustion gas flow, a connecting pipe used for fixing a combusted moxa stick, a condensing pipe used for condensing moxa stick smoke and an absorption bottle used for absorbing volatile components in the smoke, the air supply unit comprises a combustion bottle, an air guide pipe and an air pump, the air pump is communicated with the combustion bottle through the air guide pipe, the connecting pipe is provided with three insertion openings, the insertion opening in one end is used for inserting moxa sticks and connected with one end of the condensation pipe, the insertion opening in the middle is connected with the combustion bottle, the other end of the condensation pipe is communicated with the absorption bottle, and an adjusting valve is arranged on the air guide pipe. The absorption liquid is directly fed into a GC-MS for detection. The device disclosed by the invention is simple in structure and low in cost, and can be quickly built and used under common laboratory conditions; and the airflow can be regulated and controlled, so that the stability and repeatability of the combustion process are ensured.

Description

Technical Field

[0001] This invention belongs to the field of traditional Chinese medicine analysis and detection technology, specifically relating to a device for absorbing smoke from burning moxa sticks and a method for direct sample injection analysis using GC-MS. Background Technology

[0002] Moxa sticks are widely used for moxibustion therapy and health care, but the smoke produced by their combustion contains complex volatile organic compounds, raising increasing concerns about their efficacy and potential safety. Existing research mainly focuses on the extraction and analysis of volatile oils from raw materials such as mugwort leaves and mugwort floss, while research on the collection and qualitative analysis of the components of the smoke after moxa stick combustion is relatively insufficient.

[0003] Existing smoke sampling methods mostly rely on industrial flue gas samplers or adsorption tube systems, which are complex in structure and expensive. Furthermore, the flow rate and absorption efficiency of combustion smoke are difficult to control stably, easily leading to component loss or poor repeatability. Therefore, developing a device and method that is simple in structure, highly controllable, highly efficient in absorption, and can be directly coupled with GC-MS analysis is of great significance. Summary of the Invention

[0004] To address the aforementioned problems, the present invention aims to provide a device for absorbing smoke from burning moxa sticks and a method for direct sample analysis using GC-MS.

[0005] The specific technical solution is as follows: A device for absorbing smoke from burning moxa sticks includes a gas supply unit for providing combustion airflow, a connecting pipe for fixing the burning moxa stick, a condenser pipe for condensing the smoke from the moxa stick, and an absorption bottle for absorbing volatile components in the smoke. The gas supply unit includes a combustion bottle, a gas guide pipe, and an air pump. The air pump is connected to the combustion bottle through the gas guide pipe. The connecting pipe has three insertion ports: one insertion port is for inserting the moxa stick, another insertion port is connected to one end of the condenser pipe, the middle insertion port is connected to the combustion bottle, and the other end of the condenser pipe is connected to the absorption bottle. The gas guide pipe is equipped with a regulating valve.

[0006] A method for direct sample injection analysis using the above-mentioned moxa stick combustion smoke absorption device coupled with GC-MS includes the following steps: 1) Assemble the smoke absorption device for burning moxa sticks, add ethanol absorption liquid into the absorption bottle, and connect the condenser tube to cooling water for reflux; 2) Light the moxa stick and insert it into the connecting tube; 3) Turn on the air pump, open the regulating valve, adjust the airflow to promote the burning of the moxa stick, and at the same time guide the smoke into the absorbent liquid in the absorption bottle, so that the smoke components can be fully dissolved and absorbed in the ethanol absorbent liquid; 4) Directly inject the absorption solution into GC-MS for detection, and use the NIST database or internal standard method for qualitative or semi-qualitative analysis of the components.

[0007] Furthermore, in step 4), during GC-MS detection, the chromatographic column was SH-I-17Sil MS, the carrier gas was helium, the flow rate was 1.0 ml / min, the injection volume was 1.0 µl, the injection port temperature was 250℃, the ion source temperature was 230℃, and the split ratio was 50:1.

[0008] Further, the gas chromatography temperature program in step 4) is as follows: starting temperature 60℃, increase to 200℃ at 5℃ / min and hold for 20min, then increase to 220℃ at 2℃ / min and hold for 10min, then increase to 250℃ at 2℃ / min and hold for 20min, then increase to 255℃ at 1℃ / min and hold for 10min, then increase to 260℃ at 1℃ / min and hold for 20min, then increase to 270℃ at 0.5℃ / min and hold for 15min.

[0009] Furthermore, in step 2), the airflow rate is 0.5-1.5 L / min, and the sampling time is controlled at 5-15 min.

[0010] The beneficial effects of this invention are as follows: 1) The device of the present invention has a simple structure and low cost, and can be quickly set up and used under ordinary laboratory conditions; 2) The airflow of the device of the present invention is adjustable, which ensures the stability and repeatability of the combustion process; 3) The device of the present invention integrates condensation and absorption, effectively reducing component loss; 4) This invention combines with direct GC-MS injection, simplifying the pretreatment process and improving the reliability of analysis. Attached Figure Description

[0011] Figure 1 This is a schematic diagram of the smoke absorption device for burning moxa sticks according to the present invention; Figure 2 The total ion current (TIC) spectrum is shown in the analysis results of the example.

[0012] In the diagram: 1. Connecting pipe; 2. Condenser pipe; 3. Absorption bottle; 4. Combustion bottle; 5. Gas delivery pipe; 6. Air pump. Detailed Implementation

[0013] The present invention will be further described below with reference to the accompanying drawings and embodiments, but the scope of protection of the present invention is not limited thereto.

[0014] like Figure 1As shown, a smoke absorption device for burning moxa sticks includes a connecting pipe 1, a condenser pipe 2, an absorption bottle 3, a combustion bottle 4, a gas guide pipe 5, and an air pump 6. The air pump 6 is connected to the combustion bottle 4 through the gas guide pipe 5. The connecting pipe 1 has three insertion ports: one port for inserting moxa sticks, another port connected to one end of the condenser pipe 2, and the middle port connected to the combustion bottle 4. The other end of the condenser pipe 2 is connected to the absorption bottle 3. The gas guide pipe 5 is equipped with a regulating valve. The combustion bottle 4 is made of heat-resistant glass.

[0015] A method for direct sample injection analysis using the above-mentioned moxa stick combustion smoke absorption device coupled with GC-MS includes the following steps: 1) Assemble the smoke absorption device for burning moxa sticks, add ethanol absorption liquid into the absorption bottle, and connect the condenser tube 2 to cooling water for reflux; 2) Light the moxa stick and insert it into connecting tube 1; 3) Turn on the air pump 6, open the regulating valve, and adjust the airflow rate to 0.5-1.5L / min, preferably 1.0-1.2L / min to promote the combustion of the moxa stick and guide the smoke into the absorption liquid of the absorption bottle 3. The smoke components are fully dissolved and absorbed in the ethanol absorption liquid. The sampling time is controlled at 5-15min, preferably 10min. 4) Directly inject the absorption solution into GC-MS for detection, and use the NIST database or internal standard method for qualitative or semi-qualitative analysis of the components.

[0016] Gas chromatography-mass spectrometry method determination conditions Column: SH-I-17Sil MS (0.25µm×0.25mm×30m), carrier gas: helium; flow rate: 1.0ml / min; injection volume: 1.0µl; injection port temperature: 250℃; detector temperature: 250℃ / ion source temperature: 230℃; split ratio: 50:1.

[0017] Temperature ramp-up program: Start at 60℃, then ramp to 200℃ at a rate of 5℃ / min and hold for 20 min, then ramp to 220℃ at a rate of 2℃ / min and hold for 10 min, then ramp to 250℃ at a rate of 2℃ / min and hold for 20 min, then ramp to 255℃ at a rate of 1℃ / min and hold for 10 min, then ramp to 260℃ at a rate of 1℃ / min and hold for 20 min, then ramp to 270℃ at a rate of 0.5℃ / min and hold for 15 min.

[0018] Data processing and analysis Raw data acquisition: Total ion current (TIC) spectra were acquired using GC-MS software. The total ion current (TIC) spectra are shown below. Figure 2 As shown.

[0019] Component identification: The mass spectrometry data were compared with the NIST database to confirm the compound name and molecular weight information of each peak. The results are shown in Table 2.

[0020] Table 2 Summary of Compounds Searched Based on Similarity .

Claims

1. A device for absorbing smoke from burning moxa sticks, characterized in that, It includes a gas supply unit for providing combustion airflow, a connecting pipe (1) for fixing the burning moxa stick, a condenser pipe (2) for condensing the smoke from the moxa stick, and an absorption bottle (3) for absorbing volatile components in the smoke. The gas supply unit includes a combustion bottle (4), a gas guide pipe (5), and an air pump (6). The air pump (6) is connected to the combustion bottle (4) through the gas guide pipe (5). The connecting pipe (1) has three insertion ports. One insertion port is used to insert the moxa stick, and the other insertion port is connected to one end of the condenser pipe (2). The middle insertion port is connected to the combustion bottle (4). The other end of the condenser pipe (2) is connected to the absorption bottle (3). The gas guide pipe (5) is equipped with a regulating valve.

2. A method for direct sample injection analysis using the moxa stick combustion smoke absorption device as described in claim 1 coupled with GC-MS, characterized in that, Includes the following steps: 1) Assemble the smoke absorption device for burning moxa sticks, add ethanol absorption liquid into the absorption bottle, and connect the condenser tube (2) to the cooling water for reflux; 2) Light the moxa stick and insert it into the connecting tube (1); 3) Turn on the air pump (6), open the regulating valve, adjust the airflow to promote the burning of the moxa stick, and at the same time guide the smoke into the absorption liquid of the absorption bottle (3). The smoke components are fully dissolved and absorbed in the ethanol absorption liquid. 4) Directly inject the absorption solution into GC-MS for detection, and use the NIST database or internal standard method for qualitative or semi-qualitative analysis of the components.

3. The method as described in claim 2, characterized in that, In step 4), during GC-MS detection, the chromatographic column was SH-I-17SilMS, the carrier gas was helium, the flow rate was 1.0 ml / min, the injection volume was 1.0 µl, the injection port temperature was 250℃, the ion source temperature was 230℃, and the split ratio was 50:

1.

4. The method as described in claim 3, characterized in that, The gas chromatography temperature program in step 4) is as follows: starting temperature 60℃, increase to 200℃ at 5℃ / min and hold for 20min, then increase to 220℃ at 2℃ / min and hold for 10min, then increase to 250℃ at 2℃ / min and hold for 20min, then increase to 255℃ at 1℃ / min and hold for 10min, then increase to 260℃ at 1℃ / min and hold for 20min, then increase to 270℃ at 0.5℃ / min and hold for 15min.

5. The method as described in claim 3, characterized in that, In step 2), the airflow rate is 0.5-1.5 L / min, and the sampling time is controlled at 5-15 min.

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