CN115201351A - Sample preparation and detection method for measuring fogging agent in tobacco and tobacco products - Google Patents
Sample preparation and detection method for measuring fogging agent in tobacco and tobacco products Download PDFInfo
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- 235000019505 tobacco product Nutrition 0.000 title claims abstract description 39
- 238000001514 detection method Methods 0.000 title abstract description 21
- 238000005464 sample preparation method Methods 0.000 title description 2
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- DNIAPMSPPWPWGF-GSVOUGTGSA-N (R)-(-)-Propylene glycol Chemical compound C[C@@H](O)CO DNIAPMSPPWPWGF-GSVOUGTGSA-N 0.000 claims description 20
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
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- 238000002360 preparation method Methods 0.000 claims description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 3
- 238000007664 blowing Methods 0.000 claims description 3
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/86—Signal analysis
- G01N30/8675—Evaluation, i.e. decoding of the signal into analytical information
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
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- G01N2030/062—Preparation extracting sample from raw material
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Abstract
The invention relates to a rapid pretreatment and detection method of atomizing agents (1, 2-propylene glycol and glycerol) in tobacco and tobacco products, which comprises the steps of crushing and extracting samples to be detected of the tobacco and the tobacco products in a medium collision extraction instrument, and then carrying out solid-liquid separation to obtain a sample solution to be detected; the extractant is C 1 ～C 4 Saturated monoalcohols; linear velocity of medium collision extraction instrument is 4 m.s ‑1 ～6.5m·s ‑1 (ii) a The total extraction time is not more than 4min; the detection limit of the method is 0.038-0.35 mg/g; the recovery rate of the method is 95.21-100.19%; the Relative Standard Deviation (RSD) of the precision experiment is 2.59-3.65%. The new method has the advantages of simplicity, high efficiency, accurate test, high sensitivity, good repeatability and wide application range, and is suitable for various types of tobacco and cigarettes1, 2-propylene glycol and glycerol in the grass product are simultaneously and quickly pretreated and detected.
Description
Technical Field
The invention belongs to the technical field of sample pretreatment and detection, and particularly relates to a method for simultaneously and quickly pretreating and detecting atomizing agents (1, 2-propylene glycol and glycerol) in tobacco and tobacco products.
Background
With the enhancement of public awareness of harmfulness of traditional cigarettes and the increase of government regulation of cigarettes, compared with the traditional cigarettes, the heated cigarettes have small release amount of harmful ingredients, and show a rapid growth trend in the market due to the advantages of physiological feeling, elegant appearance, smoking mode and the like, thereby becoming one of important ways for future development of the tobacco industry. The international companies such as Feimei, enmei tobacco, korea tobacco and Japanese tobacco have invested a great deal of capital for developing and heating cigarette products. Heating cigarette products is also an important direction for the development of tobacco in China. Through research, most of the middle tobacco companies have started producing heated cigarette products and exported abroad. The importance of product quality to enterprises is self-evident, and quality inspection and supervision of products are important means for ensuring the product quality.
Tobacco (dry tobacco leaf) contains partial 1, 2-propanediol, glycerol and other components, and tobacco products made of the tobacco also often contain certain 1, 2-propanediol, glycerol and other components, for example, 1, 2-propanediol and glycerol are added into heated cigarette materials to be used as atomizing agents, and 1, 2-propanediol and glycerol are added into traditional cigarettes to be used as humectants. The content of 1, 2-propylene glycol and glycerol added in the traditional cigarette is low (generally below 2%), while the content of 1, 2-propylene glycol and glycerol added in the heated cigarette is high, and the content is generally 10% -20%.
As 1, 2-propylene glycol and glycerol are ubiquitous in tobacco and tobacco products and have great significance on the sense and mouthfeel of the tobacco products, accurate detection of the content of 1, 2-propylene glycol, glycerol and other components in the tobacco and the tobacco products has great significance on product development and quality monitoring. Currently, the industry standards for 1, 2-propylene glycol and glycerol in tobacco and tobacco products mainly include YC/T243-2008 gas chromatography for measuring 1, 2-propylene glycol and glycerol in tobacco and tobacco products and YC/T244-2008 high performance liquid chromatography for measuring 1, 2-propylene glycol, glycerol and sorbitol in tobacco and tobacco products. For example, the current industry standard method, YC/T243-2008, for the detection of 1, 2-propanediol and glycerol, requires that the sample is dried in an oven at a temperature of not higher than 40 ℃ until the sample can be manually twisted and crushed, and then ground and sieved (YC/T31-1996), which often causes the loss of 1, 2-propanediol and glycerol; a large amount of solvent is needed during sample extraction, so that the environment is polluted; in addition, the extraction time is long, and the analysis and labor cost are increased for the conventional detection of the heated cigarette.
Accordingly, there is a need in the industry for a method for rapidly and accurately determining the amount of aerosolizing agent (e.g., 1, 2-propanediol and glycerol) in tobacco and its products.
Disclosure of Invention
The invention aims to provide a method for quickly pretreating and detecting an atomizing agent (smoking media such as 1, 2-propanediol and glycerol) in a tobacco product. The method provided by the invention has the advantages of short time for pretreatment operation, high extraction efficiency, less solvent consumption, high sensitivity and accurate test, and can change the traditional pretreatment operation which is limited to the treatment modes and methods such as ultrasound, oscillation and the like.
Tobacco (dry based tobacco, e.g., cut tobacco) has greater hardness, toughness, and greater limited adsorption of ingredients than fresh tissue, and the tobacco has a lower content of 1, 2-propanediol and/or glycerol. Due to the characteristics of the special structure and the component content of the tobacco, the difficulty of extracting and measuring the 1, 2-propylene glycol and/or glycerol of the tobacco is multiplied. In addition, for the tobacco product, 1, 2-propylene glycol and/or glycerol are/is selectively added, however, other additives are needed in the tobacco product, for example, in the novel tobacco sheet, a binder is needed, and the added components have a certain negative effect on the determination of 1, 2-propylene glycol and/or glycerol. Furthermore, 1, 2-propanediol and/or glycerol have certain volatility characteristics, and improper sample processing means can result in the loss of 1, 2-propanediol and/or glycerol.
Therefore, how to break through the special structural limitation of tobacco and products thereof, and reducing the loss of 1, 2-propylene glycol and/or glycerol is the key to realize the high-efficiency extraction and detection of 1, 2-propylene glycol and/or glycerol in tobacco and products thereof, and is also an industrial problem. Aiming at the technical problem, the invention provides the following solving means through intensive research:
a method for preparing samples to be tested for measuring an atomizing agent in tobaccos and tobacco products comprises the steps of extracting the samples to be tested of the tobaccos and the tobacco products in a medium collision extraction instrument, and then carrying out solid-liquid separation to obtain a sample solution to be tested;
the extractant is C 1 ～C 4 Saturated monoalcohols;
linear velocity of medium collision extraction instrument is 4 m.s -1 ～6.5m·s -1 ；
The total time of extraction is not higher than 4min.
The research of the invention discovers that the extraction treatment in the mode is innovatively carried out on the tobacco and the tobacco products thereof, and the synergistic effect can be generated based on the combined control of the extracting agent, the extraction linear velocity and the time, so that the structural limitation of the tobacco and the tobacco products and the limitation of the self characteristic of the atomizing agent can be broken through, the high-efficiency extraction can be realized, and the determination effect can be improved.
In the invention, the cooperative control of the extraction mode and the conditions thereof is the key for breaking through the structural limitation of the tobacco and the products thereof and improving the determination accuracy of the tobacco and the products thereof. 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 cooperation, further improving the efficient extraction of the atomizing agent in the tobacco structure of the sample to be detected, and improving the detection effects such as the recovery rate, the sensitivity and the like of the detection.
In the invention, the alcohol is at least one of methanol, ethanol and isopropanol; methanol is preferred. The research unexpectedly finds that the methanol is adopted as the extracting agent, the methanol and the extracting process have better cooperativity, the extracting efficiency and the extracting effect of the atomizing agent in the sample to be detected can be further improved, and the subsequent detection recovery rate, sensitivity and accuracy can be further improved.
Preferably, the material-liquid ratio of the sample to be detected to the extracting agent is 0.025-0.1 g/mL; more preferably 0.03 to 0.05g/mL. The research finds that the combination of the extraction mode is beneficial to further improving the extraction effect of the 1, 2-propylene glycol and the glycerol in a synergistic way in the preferable feed-liquid ratio; the synergistic extraction performance of the unit extractant is obviously improved.
Preferably, the homogenizer is a FastPrep from MPBiomedials @ -24 instruments.
Preferably, the lysis medium used is at least one of medium S, medium M or medium D;
wherein the medium S is a 1/8 inch stainless steel ball;
media M was 1/4 inch cylindrical ceramic beads;
medium D is 1.4mm ceramic beads;
preferably, the lysis medium used is medium M.
Preferably, the linear velocity of the medium impact extractor is 4 m.s -1 ～5m·s -1 . Under the extraction mode, the combined control of linear velocity is further matched, so that the component loss can be reduced, and the extraction performance can be improved.
Preferably, the extraction process comprises 1 to 4 repeated extraction operations. In the invention, the extraction process can be a single extraction operation or a plurality of extraction operations. When a plurality of extraction operations are employed, the time interval between the extraction operations is, for example, 1 to 3min.
In the invention, the time of single extraction operation is less than or equal to 60s; preferably 50 to 60 seconds.
Preferably, the total time of extraction is 1 to 3min. Under the extraction mode, the combined control of extraction procedures and time is further matched, so that the component loss can be reduced, and the extraction performance can be improved.
The tobacco is a dry-based raw material;
preferably, the tobacco product includes, but is not limited to, at least one of tobacco leaves, cut tobacco and tobacco sheets.
Preferably, the atomizing agent is at least one of 1, 2-propylene glycol and glycerol.
In the invention, after extraction, standing is carried out, and supernatant is filtered by a membrane to obtain the solution to be detected.
The invention also provides a method for measuring the fogging agent in the tobacco and the tobacco products, the solution to be measured is prepared by the method, and then the gas chromatography measurement is carried out.
The invention innovatively adopts a medium collision extraction mode to treat tobacco and products thereof, and carries out cooperative control on conditions such as an extracting agent, a treatment program, treatment time, a material ratio and the like according to the polarity, the solubility and other properties of 1, 2-propylene glycol and glycerol, so that two components can be extracted out to the maximum extent by using a proper extracting agent in a short time, a treated solution is treated by a filter membrane after standing, and finally, the detection is carried out by using a gas chromatography method.
Preferably, the detector for chromatographic measurement is a FID (flame ionization detector).
Preferably, the gas chromatography conditions are: the gas chromatographic column is 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 sample introduction is carried out, wherein the split ratio is 50; 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 rate is 25mL/min.
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 corresponding adapters, and the number of samples which can be treated at one time in the invention is 12.
Advantageous effects
1. The research of the invention finds that the structural limitation of tobacco and products thereof can be broken through by medium collision extraction and the cooperative control of the conditions, the loss of 1, 2-propylene glycol and glycerol in the treatment process can be avoided, the extraction rate can be effectively improved, and the determination effect can be improved. Moreover, the method has simple process, short treatment time (shortened to within 2 minutes), low solvent consumption, solvent saving and pollution reduction.
2. The technical scheme of the invention has high treatment efficiency and better treatment effect, for example, the detection limit of two target objects is 0.038-0.35 mg/g and the quantification limit is 0.13-1.17 mg/g by using the method in the invention; the recovery rate of the method is 95.21-100.19%; the Relative Standard Deviation (RSD) of the precision experiment is 2.59-3.65%. The developed new method is simple, efficient, accurate in test, high in sensitivity, good in repeatability and wide in application objects, and is suitable for simultaneous and rapid pretreatment and detection of 1, 2-propylene glycol and glycerol in various types of tobaccos and tobacco products.
Drawings
FIG. 1 is a chromatogram for testing 1, 2-propanediol and glycerol in a tobacco product using GC-FID;
1. methanol (extractant, t =1.220 min) 2, 1, 2-propanediol (t =2.607 min) 3, 1, 4-butanediol (internal standard, t =4.241 min) 4, glycerol (t =4.388 min)
FIG. 2 is a view showing the microscopic size change of tobacco shreds before and after medium collision extraction treatment and oscillation extraction
Detailed Description
1) Preparing a standard solution and preparing a standard curve.
2) Optimizing pretreatment conditions: considering the polarity, solubility and other properties of 1, 2-propylene glycol and glycerol, three extractants, namely methanol, ethanol and isopropanol, are mainly screened; in order to realize the maximum extraction of 1, 2-propylene glycol and glycerol in the tobacco products, the proportion of the feed liquid is optimized; in order to stabilize the state of the processed sample, the measurement result is constant and reliable, the processing procedure of the medium collision extraction 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 industry standard detection method.
3) Adding 1, 2-propylene glycol and glycerol with low, medium and high levels into certain tobacco sheets, performing rapid pretreatment and chromatographic analysis on the sample subjected to standard addition, and calculating the standard addition recovery rate.
4) The same sample is tested several times, and the intra-day precision and the inter-day precision are calculated.
5) The samples were analyzed for various types of tobacco products.
In this case, the media impact extractor is, except where specifically stated, manufactured by the company MP Biomedicals, model FastPrep @ -24. The cracking medium used during the extraction treatment was M, which is 1/4 inch cylindrical ceramic beads.
In the invention, the time of single extraction is 1min unless otherwise stated, and when the extraction time is multiple of 1min, the extraction is repeated for a plurality of times, and when the extraction is repeated for a plurality of times, the time interval between the extraction times is, for example, 1-2 min.
The internal standard substance is 1, 4-butanediol (the addition amount of the solution to be tested is 2.5 mg/mL)
The gas chromatography conditions were: the gas chromatographic column is 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 sample introduction is carried out, wherein the split ratio is 50; 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 the present invention, the propylene glycol refers to 1, 2-propylene glycol unless otherwise specified.
The industry standard method is YC/T243-2008 < determination of tobacco and tobacco products 1, 2-propylene glycol and glycerol gas chromatography >. The specific operation is as follows: 1. sample preparation: if the tobacco leaves are tobacco leaves, randomly extracting a part of the tobacco leaves from each part of the laboratory sample, brushing fine soil and sand grains on the tobacco leaves by using a soft hairbrush, extracting main veins, and cutting the tobacco leaves into pieces or shreds; if the cigarette is a cigarette, the cigarette paper and the filter material are removed from the tobacco shreds completely. Putting tobacco leaves (or tobacco shreds) into an oven, drying in the oven at a temperature of not higher than 40 deg.C until the tobacco leaves (or tobacco shreds) can be taken out of the oven by finger-twisting, grinding immediately, and grinding for a time not longer than 2min. Then sieving, and grinding and sieving the unsieved fine vein again. The sieved powder was immediately filled into a clean and dry jar and sealed. Fully shaking and mixing evenly to obtain the prepared sample. 2. Sample extraction: about 2g of sample was weighed to the nearest 0.01g and placed in a 150mL Erlenmeyer flask. Adding 50mL of extractant methanol, shaking and extracting for 2h with a plug, and standing the extract for 10-15 min. The supernatant was analyzed by gas chromatography.
EXAMPLE 1 preparation of Standard solution and preparation of Standard Curve
Accurately weighing 0.5g of 1, 2-propylene glycol (accurate to 0.0001 g) and 0.5g of glycerol (accurate to 0.0001 g) in a 50mL volumetric flask, and performing constant volume by using a methanol solution containing 1, 4-butanediol (2.5 mg/mL) as an internal standard to obtain a standard stock solution. Respectively transferring 0.1 mL, 0.2 mL, 0.5 mL, 1.0 mL, 2.0 mL, 3.0 mL and 5.0mL of mixed standard stock solutions into 7 10mL volumetric flasks, and performing constant volume by using a methanol solution containing an internal standard to prepare a 7-grade standard working solution. GC-FID analysis was performed on the series of standard solutions. And taking the ratio of the peak area of each target substance to the peak area of the internal standard substance as a vertical coordinate, and the ratio of the concentration of each target substance to the concentration of the internal standard substance as a horizontal coordinate to obtain a linear regression equation of the two target substances. 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: extractant study
The effect of different extractants on the test results of 1, 2-propanediol and glycerol was tested with tobacco sheet a. The specific operation is as follows: weighing 1g of sample of the flake a in three parts, putting the sample into a 15mL centrifuge tube containing a lysis medium M without any grinding and shearing treatment, respectively adding 10mL of different extracting agents, and processing at a medium collision extraction instrument speed of 4 m.s -1 The treatment time is 1 minute, and the supernatant is taken out for chromatographic analysis by a filter membrane after standing for 2 minutes.
In the extractant research experiment, several extractants, namely n-hexane, acetonitrile, methanol, ethanol and isopropanol are selected, and the test results are shown in table 2. It can be seen that the test results for 1, 2-propanediol and glycerol with methanol, ethanol and isopropanol as extractants under the same conditions are significantly higher than the test results with n-hexane and acetonitrile as extractants, with methanol being the most preferred extractant.
TABLE 2 Effect of different extractants and treatment times on the results of the 1, 2-propanediol and glycerol tests
When methanol is used as an extracting agent and the extraction time is prolonged, the test result is slightly increased when the extraction time is prolonged from 1min to 2min, but the change is not large, the extraction time is continuously increased, and the content of the measured 1, 2-propylene glycol and glycerol is reduced; research shows that under the pretreatment method, the extraction effect can be improved through synergy based on the combined control of the extracting agent and the time.
Example 3: research on material-liquid ratio in extraction process
Experiments were conducted with tobacco sheet b to examine the effect of the feed-liquid ratio on the test results for 1, 2-propanediol and glycerol. The specific operation is as follows: weighing a certain mass of a sheet b sample (the mass of the sample is added according to the feed-liquid ratio in the table below), putting the sample into a 15mL centrifuge tube containing a cracking medium M without any grinding and shearing treatment, adding 10mL of an extractant methanol containing an internal standard 1, 4-butanediol (the concentration is 2.5 mg/mL), and processing at a medium collision extraction instrument speed of 4M & s -1 The treatment time is 1 minute, and the supernatant is taken out for chromatographic analysis by a filter membrane after standing for 2 minutes. The results are shown in Table 3.
TABLE 3 Experimental results of different material ratios for detection
Note: the material-liquid ratio refers to the ratio of weight to volume, wherein the unit of weight is g, and the unit of volume is mL;
the results show that: under the pretreatment process, the cooperation can be further realized by further combining the material-liquid ratio, and a better extraction effect can be obtained, for example, when the material-liquid ratio is 0.3-0.5 g/mL, particularly 0.4 (g/mL), the test results of two objects tend to be stable, and the test result at the time is higher than that of an industry standard method. If the proportion is not controlled in the preferred proportion of the invention, the synergistic effect is reduced and the extraction effect is not ideal.
Example 4: research on linear velocity and time of extraction instrument
And (3) performing an experiment on the heated cigarette slice c of the sample to be tested, and further investigating the influence of the linear velocity and the processing time of the medium impact extraction instrument on the test result of the 1, 2-propylene glycol and the glycerol. The specific operation is as follows: accurately weighing 0.4g of flake c sample, putting the flake c sample into a 15mL centrifuge tube containing a cracking medium M without any grinding and shearing treatment, adding 10mL of extractant methanol containing internal standard 1, 4-butanediol (the concentration is 2.5 mg/mL), referring to a table 4 for medium collision extraction instrument treatment speed and treatment time, standing for 2min, and taking a supernatant fluid filter membrane for chromatographic analysis. The test results are shown in table 4.
TABLE 4 influence of different processing speeds and times of the media impact extractor on the 1, 2-propanediol and glycerol test results
Researches show that the extraction effect can be further improved and extraction omission can be avoided by cooperatively controlling the line speed and the time under the pretreatment means of the invention. For example, 4m · s -1 ～5m·s -1 And 1-3 min, the extraction effect can be synergistically improved, and a better synergistic effect is achieved. For example, when the treatment time is 1min and experiments are conducted using different treatment speeds, it is found that the treatment speed is increased to 5m · s -1 The results were almost unchanged, and the test results decreased as the processing speed continued to increase. When the linear velocity of the extraction instrument is 4 m.s -1 The delay time is long in processing time, when the processing time is prolonged to 2min, the test result is slightly increased, and the test result is reduced when the processing time is continuously prolonged. Therefore, the optimized optimal pretreatment condition is that the extractant is methanol and the treatment speed is 4 m.s -1 The treatment time is 2 minutes, and the material-liquid ratio is 0.4. The detection result is higher than that of the industry standard method.
Example 5: experimental study of recovery
3 parts of certain tobacco sheet d are taken for experimental study on the recovery rate, and the specific operation is as follows: accurately weighing 0.4g of tobacco sheet d sample, putting the tobacco sheet d sample into a 15mL centrifuge tube containing a cracking medium M without any grinding and shearing treatment, adding standard solutions of 1, 2-propylene glycol and glycerol with low, medium and high levels into the tube respectively, repeating the steps for 3 times at each addition level, then adding 10mL of extractant methanol containing internal standard 1, 4-butanediol (the concentration is 2.5 mg/mL), and treating the tobacco sheet d sample by using a medium collision extractor at a treatment speed of 4M s -1 The treatment time is 2 minutes, and after standing for 2 minutes, a supernatant fluid is taken out to be subjected to chromatographic analysis by a filter membrane. The normalized recovery was calculated and the results are shown in table 5. The results show that the standard recovery rates of 1, 2-propylene glycol and glycerol are respectively 95.56-99.44% and 95.21-100.19%, and are within the specified allowable range (95-105%, GB/T27417-2017), which indicates that the accuracy of the developed method is higher.
Table 5 recovery test results for methods
Example 6: experimental study on precision
The tobacco sheet e is used for researching the day precision and the day precision, and the specific operation is as follows: accurately weighing 0.4g of tobacco sheet e sample, putting the tobacco sheet e sample into a 15mL centrifuge tube containing a cracking medium M without any grinding and shearing treatment, adding 10mL of extractant methanol containing internal standard 1, 4-butanediol (the concentration is 2.5 mg/mL) into the tube, and processing the sample by a medium collision extraction instrument at a speed of 4M s -1 The treatment time is 2 minutes, and the supernatant is taken out for chromatographic analysis by a filter membrane after standing for 2 minutes. The samples were tested in 6 replicates and the results are shown in table 6. The test results are: the intra-day precision RSD of the 1, 2-propylene glycol is 2.59 percent, and the inter-day precision RSD is 2.68 percent; daily dose of glycerolThe precision RSD was 2.85% and the daytime precision RSD was 3.65%. The results show that the method has good repeatability and stable test.
TABLE 6 Intra-day and inter-day precision experiments
Example 7: determination of actual samples
Under the optimized condition, the tobacco products of different types are pretreated and detected by a newly developed method, and the specific operation is as follows: accurately weighing 0.4g of different types of tobacco products without any grinding and shearing treatment, placing into a 15mL centrifuge tube containing a lysis medium M, adding 10mL of extractant methanol containing internal standard 1, 4-butanediol (concentration of 2.5 mg/mL) into the tube, and processing at a medium collision extraction apparatus processing speed of 4 m.s -1 The treatment time is 2 minutes, and after standing for 2 minutes, a supernatant fluid is taken out to be subjected to chromatographic analysis by a filter membrane. The test results are shown in Table 7. It can be seen that under the optimized conditions, the contents of 1, 2-propylene glycol and glycerol in tobacco leaves, tobacco shreds and different types of tobacco sheets are different, and the contents of 1, 2-propylene glycol and glycerol in the novel tobacco products are obviously higher than those of the traditional cigarettes. 1, 2-propanediol and glycerol have higher test results than the standard method (due to losses during grinding or shearing) when using the method developed herein.
TABLE 7 analysis results of the actual samples
The embodiment shows that the newly developed medium collision extraction pretreatment method is utilized, based on the combined control of the treatment extraction solvent, the linear velocity and the time, the complete extraction of the 1, 2-propylene glycol and the glycerol in the tobacco and tobacco products can be rapidly and efficiently completed within 2 minutes, and the gas chromatography is combined for efficient detection and application. Compared with the pretreatment method (oscillation extraction for 2 h) in the industry standard, the new method has obvious advantages, and then microscopic changes of the cut tobacco before and after the treatment of the two methods are respectively observed by using a scanning electron microscope, as shown in figure 2. 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 rapidly pretreating and detecting 1, 2-propylene glycol and glycerol in tobacco and tobacco products, does not need any grinding and shearing treatment, is simple and convenient to operate, saves time, is high in efficiency, and is high in sensitivity, accuracy, recovery rate and repeatability of the developed new method. 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 (14)
1. A preparation method of a sample to be tested for measuring an atomizing agent in tobacco and tobacco products is characterized in that the sample to be tested of the tobacco and the tobacco products is crushed and extracted in a medium collision extraction instrument, and then solid-liquid separation is carried out to obtain a sample solution to be tested;
the extractant is C 1 ～C 4 Saturated monoalcohols;
linear velocity of medium collision extraction instrument is 4 m.s -1 ～6.5m·s -1 ；
The total time of extraction is not higher than 4min.
2. The method according to claim 1, wherein the alcohol is at least one of methanol, ethanol, and isopropanol; methanol is preferred.
3. The method according to claim 1, wherein the ratio of the sample to be tested to the extractant is 0.025 to 0.1g/mL; more preferably 0.03 to 0.05g/mL.
4. The method of claim 1, wherein the lysis medium used in the extraction treatment is at least one of medium S, medium M, or medium D;
wherein the medium S is a 1/8 inch stainless steel ball;
media M is 1/4 inch cylindrical ceramic beads;
medium D is 1.4mm ceramic beads;
preferably, the lysis medium used is medium M.
5. The method of claim 1, wherein the medium impact extractor is FastPrep from MP Biomedicals corporation @ -24 instruments.
6. The process according to claim 1, wherein the linear velocity of the medium impact extractor is 4 m.s -1 ～5m·s -1 。
7. The method of claim 1, wherein the extraction process comprises 1 to 4 extraction operations.
8. The method of claim 7, wherein the time for a single extraction run is less than or equal to 60 seconds; preferably 50 to 60 seconds.
9. The process according to any one of claims 1 to 8, wherein the total time of extraction is from 1 to 3min.
10. The method of claim 1, wherein the tobacco is a dry-based material;
preferably, the tobacco product includes, but is not limited to, at least one of tobacco leaf, cut tobacco and tobacco sheet.
11. The production method according to any one of claims 1 to 10, wherein the atomizing agent is at least one of 1, 2-propanediol and glycerol.
12. A method for the determination of fogging agents in tobacco and tobacco products, characterised in that a solution to be tested is prepared by a method according to any one of claims 1 to 11, followed by gas chromatography.
13. The method of claim 12, wherein the chromatographic detector is FID.
14. The method of determining aerosolization agent in tobacco and tobacco products of claim 12, wherein the gas chromatography conditions are: the gas chromatographic column is 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 sample introduction is divided and the division ratio is 50; 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 rate is 25mL/min.
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