CN115201345A - Sample pretreatment and detection method for moisture and/or nicotine in tobacco and tobacco products - Google Patents
Sample pretreatment and detection method for moisture and/or nicotine in tobacco and tobacco products Download PDFInfo
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Abstract
The invention provides a sample pretreatment method beneficial to detecting moisture and/or nicotine in tobacco and tobacco products, which comprises the steps of extracting samples to be detected of the tobacco and the tobacco products in a medium collision extractor to obtain a sample solution to be detected; the extractant comprises alcohol. The invention also provides a means for carrying out gas chromatography determination on the sample solution to be determined. The pretreatment method provided by the invention has the advantages that due to the high cracking and extraction efficiency, compared with the traditional method, the pretreatment time is greatly shortened, and the labor and the cost can be greatly saved; because the sample does not need to be sheared, ground and other treatment processes before extraction, the loss of moisture is reduced, and the measured result is more real and reliable. The research of the invention finds that the detection limits of the two components are 0.030-0.22 mg/g; the recovery rate of the method is 95.61-100.39%; the Relative Standard Deviation (RSD) of the precision experiment is 1.58-3.87%.
Description
Technical Field
The invention belongs to the field of sample pretreatment and detection, and particularly relates to a method for simultaneously and quickly pretreating and detecting moisture and nicotine in tobacco and tobacco products.
Background
The moisture content in tobacco and tobacco products is one of the important quality indexes, and has great influence on the storage safety, the internal quality and the like of the tobacco and the tobacco products. Nicotine is a key active ingredient of tobacco products, and the total nicotine content in the heated cigarette material is closely related to the strength, the irritation and the like of the heated cigarette. The accurate detection of the contents of components such as moisture, nicotine and the like in tobacco and tobacco products has great significance for product development and quality monitoring.
Many national and industrial standards for moisture and nicotine in tobacco and tobacco products have emerged, such as YC/T31-1996, GB/T23357-2009, YC/T345-2010, YC/T246-2008 and YC/T383-2010.
The oven method in the national standard and industry standard methods of the moisture and nicotine in the tobacco and the tobacco products is not suitable for measuring the moisture in the heated cigarette, and the Karl Fischer method needs special instruments and equipment and has no popularization. The time required by the pretreatment operation is 2 hours to 1 day, and the period is long; and the two indexes need to be detected respectively, so that the difficulty, the analysis cost and the labor cost are increased for the conventional analysis of the tobacco products.
Disclosure of Invention
In order to solve the problem that the conventional tobacco and tobacco product samples are difficult to be synchronously pretreated, a first object of the invention is to provide a sample pretreatment method which is favorable for detecting moisture and/or nicotine in the tobacco and the tobacco products, and the invention aims to realize synchronous and rapid extraction of the moisture and the nicotine in tobacco components to be detected by the pretreatment method, thereby being favorable for realizing synchronous determination of the moisture and the nicotine.
A second object of the present invention is to provide a method for detecting moisture and/or nicotine in tobacco and tobacco products.
The tobacco of the invention is dry-based raw material (such as cut tobacco). The tobacco product includes at least one of tobacco leaf, tobacco shred and tobacco sheet.
Tobacco (dry-based tobacco, such as cut tobacco) and tobacco products thereof are various in types, and compared with living tissues, the tobacco has higher hardness and toughness, and a dry cell wall structure has stronger limited adsorption performance on moisture and nicotine, so that the extraction difficulty of the moisture and the nicotine, particularly the extraction difficulty of the nicotine synchronously, is influenced to a great extent. Aiming at the technical problem, the existing means respectively sample different measurement objects, so that not only is a processing procedure increased, but also the loss of a test target is easily caused, and the moisture and nicotine content of tobacco and tobacco products can not be accurately and synchronously identified, which is not beneficial to the accurate and comprehensive evaluation of the properties of the tobacco and the tobacco products. Aiming at the technical problem in the industry, the technical scheme of the invention provides the following technical scheme:
a sample pretreatment method beneficial to detecting moisture and/or nicotine in tobacco and tobacco products is characterized in that samples to be detected of the tobacco and the tobacco products are extracted in a medium collision extractor to obtain a sample solution to be detected;
the extractant comprises alcohol.
The research of the invention finds that the extraction agent and the extraction process are cooperatively combined, so that the synchronous, quick and efficient extraction of the moisture and nicotine in the tobacco components can be unexpectedly and effectively realized, and the quick and efficient determination of the moisture and nicotine is facilitated.
The research of the invention finds that the synergistic combination of the extracting agent and the cracking is the key for improving the high-efficiency extraction of the water and/or the nicotine of the sample to be detected. Research also finds that the combined control of the components of the extracting agent, the content of the extracting agent and the extraction process is beneficial to further forming the synergy, further improving the efficient extraction of the water and/or nicotine of the sample to be detected, and improving the detection effects such as the recovery rate and the sensitivity of the detection.
Preferably, the alcohol is a mono-to di-alcohol.
More preferably, the extractant is C1-C4 monoalcohol, and still more preferably at least one of methanol, ethanol and isopropanol; most preferred is methanol. The research shows that methanol is adopted as an extracting agent, the methanol and the extracting process have better cooperativity, the extraction efficiency and the extraction effect of the water and the nicotine of the sample to be detected can be further improved, and the subsequent detection recovery rate, the sensitivity and the accuracy can be further improved.
Preferably, the extractant further comprises an organic base. The research of the invention also finds that certain organic alkali is further compatible in the extractant, which is beneficial to further cooperating with alcohol and an extraction process, and further improving the effect of pretreatment.
More preferably, the organic base is triethylamine.
Preferably, the volume ratio of the alcohol to the organic base in the extractant is 100:0.1 to 30; preferably 100: more preferably 100. The research of the invention finds that the control in the required range is helpful for further improving the cooperativity of the extracting agent and the extraction process and further improving the determination effect.
Preferably, the material-liquid ratio of the sample to be detected to the extracting agent is 0.025-0.2 g/mL; preferably 0.03 to 0.1g/mL; more preferably 0.03 to 0.05g/mL. In the invention, the material-liquid ratio refers to the weight-volume ratio of the sample to be detected and the extracting agent.
In the invention, the linear velocity of the medium collision extraction instrument is 4 m.s -1 ~6.5m·s -1 。
In the extraction treatment of the present invention, single extraction or multiple extractions may be performed.
Preferably, the time for a single extraction treatment is 60 seconds or less. The extraction treatment frequency is preferably 1 to 3 times; the total time of the extraction treatment process is preferably 1 to 3min.
Preferably, the cracking medium used in the extraction process is M, which is 1/4 inch cylindrical ceramic beads, but is not limited thereto.
The invention also provides a method for detecting moisture and/or nicotine in tobacco and tobacco products, which is characterized in that a sample to be detected is pretreated by adopting the method, a solution to be detected is obtained by solid-liquid separation, and then gas phase analysis is carried out.
The research of the invention finds that the synchronous determination of the moisture and/or the nicotine can be realized by the precursor method, and the synchronous determination of the moisture and/or the nicotine, especially the moisture and the nicotine, can be realized by the GC-based determination.
In the present invention, GC measurement can be realized based on existing equipment and means.
Preferably, after the pretreatment extraction is finished, standing or centrifuging treatment is carried out, and a supernatant is taken and filtered to obtain the solution to be detected.
In the invention, the water content is detected by a TCD detector; preferably, nicotine is detected using a FID detector.
The moisture content was measured by using a gas chromatography column HP-PLOT/Q, which was 30m (length) × 0.53mm (inner diameter) × 1.8 μm (film thickness); the nicotine test adopts a gas chromatographic column as Rtx @ -BAC1, with a gauge of 30m (length) x 0.32mm (inner diameter) x 1.8 μm (film thickness);
the temperature raising program is that the initial temperature is 90 ℃, the temperature is kept for 1min, the temperature is raised to 120 ℃ at 15 ℃/min, the temperature is raised to 240 ℃ at 40 ℃/min, and the temperature is kept for 4min; the temperature of a sample inlet is 250 ℃; the sample introduction amount is 1 mu L, and the split flow sample introduction is carried out, wherein the split flow ratio is 50: 1; the carrier gas is nitrogen, and the flow is 1.8mL/min; the detector temperature was 275 ℃; the hydrogen flow is 40mL/min; the air flow is 450mL/min; the tail gas blowing is nitrogen, and the flow is 25mL/min.
The invention applies a rapid pretreatment instrument to the rapid pretreatment process of tobacco and tobacco products, screens and optimizes conditions such as an extracting agent, a treatment program, treatment time, a material ratio and the like according to the polarity, the solubility and the like of water and nicotine, simultaneously extracts two components to the maximum extent by using a proper extracting agent in a short time, and finally detects the treated solution by a gas chromatography method after centrifugal operation and filtration membrane treatment.
The method has the advantages of short time for pretreatment operation, high extraction efficiency, less solvent consumption, high test accuracy and high sensitivity, and can change the traditional pretreatment operation which is only limited to the treatment modes and methods such as ultrasound, oscillation and the like.
Advantageous effects
1. According to the technical scheme, grinding and extraction of various tobacco products can be quickly realized, and the time of pretreatment operation is greatly shortened; for example, the pretreatment time can be shortened to 1 minute.
2. According to the technical scheme of the invention, compared with the traditional treatment method, the required extracting agent is reduced, the solvent can be saved, and the pollution is reduced. In addition, the pretreatment operation can be greatly simplified, the sample does not need to be pre-crushed, the water loss and the component change caused in the grinding process are reduced, and the test result can be more accurate.
3. Due to the high-efficiency pretreatment process, the method can realize the synchronous determination of the water and the nicotine, and has the detection limit of 0.030-0.22 mg/g and the quantification limit of 0.10-0.73 mg/g; the recovery rate is 95.61-100.39%; the Relative Standard Deviation (RSD) of the precision experiment is 1.58-3.87%.
4. The batch pretreatment operation can be simultaneously carried out on a plurality of tobacco or tobacco products to be detected, the number of samples to be detected which are simultaneously treated is determined by the corresponding adapter, and the number of samples which can be treated at one time in the invention is 12.
Drawings
FIG. 1 is a chromatogram for testing moisture in a tobacco product using a GC-TCD method; (1 is water 2, isopropanol (internal standard of water)
FIG. 2 shows a chromatogram for testing nicotine in a tobacco product using GC-FID; wherein, 3, 4, n-heptadecane (internal standard of nicotine)
FIG. 3 is a view showing the microscopic size change of tobacco shreds before and after medium collision extraction treatment and oscillation extraction
Detailed Description
The technical scheme of the invention is as follows:
1) Preparing a standard solution and preparing a standard curve.
2) Optimizing pretreatment conditions: selecting and optimizing the extracting agent according to the properties of the water, the polarity, the solubility and the like of the nicotine; adjusting the pH value by using organic base, and optimally screening the ratio of the alcohol solvent to the organic base; in order to realize the complete extraction of water and nicotine in the tobacco products, the proportion of the feed liquid is optimized; in order to stabilize the state of the processed sample, the measuring result is constant and reliable, the processing procedure of the rapid processing instrument is optimized, and the processing time is reduced as much as possible. And comparing the optimized test result with the test result of the row marking method.
3) Respectively adding water and nicotine with low, medium and high levels into a certain tobacco sheet, performing rapid pretreatment and chromatographic analysis on the sample subjected to standard addition, and calculating the standard addition recovery rate.
4) And (5) detecting the sample for multiple times, and calculating the intra-day precision and the inter-day precision.
5) Sample analysis was performed on various types of smoking article materials.
In the following case, water is detected using a TCD detector unless otherwise stated; nicotine was detected using a FID detector.
The moisture content was measured by using a gas chromatography column HP-PLOT/Q having a specification of 30m (length) x 0.53mm (inner diameter) x 1.8 μm (film thickness); the nicotine test adopts a gas chromatographic column as Rtx @ -BAC1, with a gauge of 30m (length) x 0.32mm (inner diameter) x 1.8 μm (film thickness);
the temperature raising procedure is that the initial temperature is 90 ℃, the temperature is kept for 1min, the temperature is raised to 120 ℃ at 15 ℃/min, the temperature is raised to 240 ℃ at 40 ℃/min, and the temperature is kept for 4min; the temperature of a sample inlet is 250 ℃; the sample introduction amount is 1 mu L, and the split flow sample introduction is carried out, wherein the split flow ratio is 50: 1; the carrier gas is nitrogen, and the flow rate is 1.8mL/min; the detector temperature was 275 ℃; the hydrogen flow is 40mL/min; the air flow is 450mL/min; the tail gas blowing is nitrogen, and the flow rate is 25mL/min.
In this case, the media impact extractor is, except where specifically stated, of the type FastPrep, manufactured by MP Biomedicals, inc @ -24。
In the present invention, unless otherwise stated, the time for single extraction is 1min, and when the time for extraction is a multiple of 1min, it means that the extraction is performed several times, and when the extraction is performed several times, the time interval between the extraction is, for example, 1-2 min.
Example 1: preparation of standard solution and preparation of standard curve:
respectively preparing standard working solutions with water concentrations of 0, 1, 2, 4, 6, 10, 15, 20 and 30 mg/mL; standard working solutions with nicotine concentrations of 0.05, 0.1, 0.3, 0.6, 1.2, 2.0 mg/mL. The internal standards are isopropanol (internal standard of moisture) and n-heptadecane (internal standard of nicotine), and the series of standard solutions are subjected to gas chromatography analysis. And taking the ratio of the peak area of each target to the peak area of the internal standard as a vertical coordinate, and taking the ratio of the concentration of each target to the concentration of the internal standard as a horizontal coordinate, so as to obtain a linear regression equation of the two targets. And the detection limit and the quantification limit of the method were calculated, and the results are shown in table 1. The result shows that the working curves of the two targets have good linearity and high sensitivity.
TABLE 1 Linear parameters, detection limits and quantitation limits of two targets
Example 2: investigation of alcohols in extractants
In consideration of the properties of water and nicotine such as solubility, polarity and the like, the invention selects three extracting agents, namely methanol, ethanol and isopropanol, to respectively carry out extraction operation on the heated cigarette slice a, and the test results are shown in table 2. At this time, the feed-liquid ratio was 0.1g/mL, and the processing speed of the medium collision extraction apparatus was 4 m.s -1 The treatment time for a single extraction was 1 minute. The test results of two components are obviously higher than that of ethanol and isopropanol which are used as extracting agents under the same conditions, so that methanol is selected as the extracting agent, but the test result is lower than that of an industrial standard method, and the test result is not changed greatly after the treatment time is prolonged.
TABLE 2 Effect of different extractants and treatment times on moisture and nicotine test results
Example 3: investigation of alkaline extractants and ratios
3.1: the industry standard method comprises the following steps:
and (3) selecting and heating the cigarette sheet b, and determining by using an industry standard method YC/T246-2008: accurately weighing 1.000g of sample in a triangular flask, adding 7mL of sodium hydroxide solution (5 mol/L), standing for 15min, then adding 50mL of extracting agent methyl tert-butyl ether, shaking for 2h, standing, and taking the supernatant for analysis.
The results of testing nicotine with and without sodium hydroxide solution treatment using the test method described above are compared, as shown in table 3. Therefore, part of nicotine in the tobacco sheets exists in the form of nicotine salt, and alkali treatment is needed to change the nicotine salt into free nicotine, so that relevant detection can be carried out.
TABLE 3 comparison of results of nicotine testing with and without alkaline treatment
3.2: preferred alcohol-organic base process of the present invention
Weighing a heated cigarette sheet sample (cigarette sheet b), putting the heated cigarette sheet sample into a 15mL centrifuge tube (containing a cracking medium M), adding 10mL of an extracting agent (methanol and triethylamine (volume ratio is shown in Table 4); feed-liquid ratio is 0.1 g/mL) into the tube, adding an internal standard, and making the linear velocity of a medium collision extraction instrument be 4M s -1 The treatment time is 1min, the influence of methanol and triethylamine solutions with different volume ratios on the nicotine test result is examined, and the result is shown in table 4. It can be seen that the nicotine test results gradually increased with the increase of triethylamine content; when the volume ratio of methanol to triethylamine is 100; in addition, the existence of triethylamine and the content of triethylamine have no influence on the moisture test.
Table 4 experimental results of detection of methanol triethylamine solutions with different proportions
It can be known from tables 3 and 4 that, by adopting the technical scheme of the invention, the nicotine extraction effect similar to that of the industrial standard high-concentration sodium hydroxide can be obtained through the organic base, and more importantly, the synchronous extraction of water which can not be realized by the industrial standard method can be realized.
Example 4: study of the feed-to-liquid ratio of the extraction Process
Weighing a certain mass of a heated cigarette sheet sample c, placing the heated cigarette sheet sample c into a 15mL centrifuge tube (containing a cracking medium M), adding 10mL of an extracting agent (methanol: triethylamine =100 15) into the tube, adding an internal standard, and controlling the linear velocity of a medium collision extraction instrument to be 4M · s -1 The treatment time is 1min, the mass of the flake sample is weighed according to the feed-liquid ratio (flake mass g and extractant volume) in Table 5mL ratio). The results of the different feed-to-liquid ratios are shown in table 5. The results show that: when the ratio of the material to the liquid is 0.04g/mL, the test results of the two targets tend to be stable, the quality of the sheet sample is continuously reduced, and the result is not changed greatly.
TABLE 5 Experimental results of different material ratios for detection
Example 5: research on linear velocity and time of an extraction instrument:
the tobacco sheet (same as example 4) was optimized for the treatment program (including the treatment speed and the treatment time) of the medium impact extractor under the condition of the material-liquid ratio of 0.04g/mL. The results are shown in Table 6, from which it can be seen that the test results for moisture and nicotine hardly changed with increasing the processing speed and time. Therefore, the optimized optimal pretreatment conditions are that the extractant is methanol, the treatment speed is 4 m.s < -1 >, the treatment time is 1 minute, and the material-liquid ratio is 0.04g/mL.
TABLE 6 influence of different processing speeds and times of the medium impact extractor on the moisture and nicotine test results
Example 6: study on recovery and precision
Weighing 3 parts of tobacco sheet (sheet d), adding three levels of low, medium and high water and nicotine standard solutions, placing the tobacco sheet (sheet d) into a 15mL centrifuge tube with a plug and containing a cracking medium M, adding 10mL methanol triethylamine extract containing an internal standard (volume ratio is 100:15; material-liquid ratio is 0.04 g/mL), and processing speed of a medium collision extraction instrument is 4M s -1 The treatment time is 1min, and after standing, supernatant (which can be diluted appropriately according to actual conditions) is taken and subjected to gas chromatography analysis after being filtered by a filter membrane. The spiked recoveries were calculated 3 times for each addition level and the results are shown in table 7. The results show that the standard recovery rates of the water and the nicotine are respectively 95.61-100.39% and 97.41-100%.26 percent, and is within the specified allowable range (95 percent to 105 percent, GB/T27417-2017), the method has higher accuracy.
Recovery of the process of Table 7
The tobacco sheet d was subjected to the in-day precision and in-day precision tests using the optimized pretreatment conditions and test conditions, and the results of the tests are shown in table 8, in which 6 parallel tests were performed on the sample each time. The test results are: the moisture intra-day precision RSD is 1.63 percent, and the inter-day precision RSD is 3.87 percent; nicotine had an intra-day precision RSD of 1.58% and an inter-day precision RSD of 1.76%. The results show that the method has good repeatability and stable test.
TABLE 8 Intra-day and inter-day precision experiments
Example 7: determination of actual samples
Weighing samples to be detected of different types of tobacco products, placing the samples into 15mL of centrifuge tubes with plugs and containing a cracking medium M, adding 10mL of methanol triethylamine extract containing an internal standard (volume ratio is 100: 15), extracting for 1min (4M s -1 ) Standing for 2min, filtering the supernatant (which can be diluted properly according to actual conditions) and performing gas chromatography. The results are shown in Table 9. It can be seen that under optimized conditions the moisture and nicotine content of the lamina (dry), cut tobacco and different types of tobacco sheets are different, and that the test results for moisture using the method developed by the present invention are higher than the standard method (due to losses during grinding or shearing); the test results of nicotine using the method developed by the present invention were lower than the test results of the standard method YC/T246-2008 (the test deviation of moisture affects the calculation of nicotine content).
TABLE 9 analysis results of 8 samples
The embodiment shows that the newly developed extraction pretreatment method can quickly and efficiently complete the complete extraction of moisture and nicotine in tobacco and tobacco products within 1 minute, and is combined with gas chromatography for efficient detection and application. Compared with the pretreatment method (oscillation extraction for 2-3 h) in the industry standard, the new method has obvious advantages, and then microscopic changes of the cut tobacco before and after the two methods are respectively observed by a scanning electron microscope, as shown in figure 3. As can be seen from the figure, the cut tobacco after the extraction treatment becomes particles with the size less than or equal to 30 μm, but the cut tobacco before and after the oscillation extraction treatment can not be obviously changed. Due to the high-efficiency cracking effect of medium collision extraction, the contact area between the tobacco product to be detected and the extracting agent in unit mass is greatly increased, so that the dissolution of the target compound is accelerated, and the extraction efficiency is improved.
The invention establishes a method for simultaneously and quickly pre-treating and detecting the moisture and nicotine in the tobacco products, has simple and convenient operation, does not need additional treatment such as crushing, grinding and the like on samples, saves time and has high efficiency, and the developed new method has accurate test, high sensitivity, high recovery rate and good repeatability. The analysis result of the actual sample shows that the method can test various types of tobacco product materials and has wide application range.
Claims (16)
1. A sample pretreatment method beneficial to detecting moisture and/or nicotine in tobacco and tobacco products is characterized in that samples to be detected of the tobacco and the tobacco products are extracted in a medium collision extractor to obtain a sample solution to be detected;
the extractant comprises alcohol.
2. The method of claim 1, wherein the alcohol is a mono-to di-alcohol.
3. The method of claim 2, wherein the extractant is a C1-C4 monoalcohol; preferably at least one of methanol, ethanol and isopropanol; methanol is more preferable.
4. The method for pretreating samples, which is convenient for detecting moisture and/or nicotine in tobacco and tobacco products, according to any one of claims 1 to 3, wherein the extractant further comprises an organic base.
5. The method of claim 4, wherein the organic base is triethylamine.
6. The method of claim 4, wherein the volume ratio of alcohol to organic base in the extractant is 100:0.1 to 30; preferably 100: more preferably 100.
7. The method for pretreating samples for detecting moisture and/or nicotine in tobacco and tobacco products according to claim 4, wherein the material-to-liquid ratio of the sample to be detected to the extracting agent is 0.025-0.2 g/mL; preferably 0.03 to 0.1g/mL; more preferably 0.03 to 0.05g/mL.
8. The method for pretreating a sample for detecting moisture and/or nicotine in tobacco and tobacco products according to any of claims 1 to 7, wherein the linear velocity of extraction is 4 m-s -1 ~6.5m·s -1 。
9. The method for pretreating a sample for detecting moisture and/or nicotine in tobacco and tobacco products according to any one of claims 1 to 8, wherein in the extraction treatment process, the time of a single extraction treatment is less than or equal to 60s; the total time of the extraction treatment process is 1-3 min.
10. The method of any of claims 1 to 8, wherein the lysis medium used in the extraction process is M, which is 1/4 inch cylindrical ceramic beads, but is not limited thereto.
11. The method of claim 1, wherein the tobacco is a dry-based material.
12. The method of claim 1, wherein the tobacco product comprises at least one of, but not limited to, tobacco leaf, tobacco shred and tobacco sheet.
13. A method for detecting moisture and/or nicotine in tobacco and tobacco products, characterized in that a sample to be detected is pretreated by the method of any one of claims 1 to 12, a solution to be detected is obtained by solid-liquid separation, and then chromatography detection is carried out.
14. The method according to claim 13, wherein the solution to be tested is obtained by standing or centrifuging after the pretreatment extraction, and filtering the supernatant.
15. The method of claim 13, wherein moisture and/or nicotine is detected using a TCD detector; preferably, nicotine is detected using a FID detector.
16. The method of claim 15, wherein the moisture test is performed using a gas chromatography column HP-PLOT/Q, having a specification of 30m (length) x 0.53mm (inner diameter)1.8 μm (film thickness); the nicotine test adopts a gas chromatographic column as Rtx @ -BAC1, with a gauge of 30m (length) x 0.32mm (inner diameter) x 1.8 μm (film thickness);
the temperature raising program is that the initial temperature is 90 ℃, the temperature is kept for 1min, the temperature is raised to 120 ℃ at 15 ℃/min, the temperature is raised to 240 ℃ at 40 ℃/min, and the temperature is kept for 4min; the temperature of a sample inlet is 250 ℃; the sample injection amount is 1 mu L, and the split flow sample injection is carried out, wherein the split flow ratio is 50: 1; the carrier gas is nitrogen, and the flow rate is 1.8mL/min; the detector temperature was 275 ℃; the hydrogen flow is 40mL/min; the air flow is 450mL/min; the tail gas blowing is nitrogen, and the flow rate is 25mL/min.
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