CN115932120A - Detection method of tobacco shred swelling agent - Google Patents
Detection method of tobacco shred swelling agent Download PDFInfo
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- CN115932120A CN115932120A CN202310047376.7A CN202310047376A CN115932120A CN 115932120 A CN115932120 A CN 115932120A CN 202310047376 A CN202310047376 A CN 202310047376A CN 115932120 A CN115932120 A CN 115932120A
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Abstract
The invention discloses a method for detecting a tobacco shred swelling agent, and belongs to the technical field of instrument analysis and detection. The detection method of the tobacco shred swelling agent provided by the invention utilizes HS-GC/MS to measure the components of the tobacco shred swelling agent, can be used for carrying out rapid analysis, is simple and convenient to operate, does not need pretreatment, has less manual intervention, and improves the working efficiency and the analysis accuracy. The method for detecting the tobacco shred expanding agent can simulate the volatilization process of the expanding agent after the tobacco shreds are expanded, is scientific and reasonable in design, accurate and reliable in measurement, and is suitable for popularization in the industry. According to the detection method of the tobacco shred expanding agent, the using amount of the tobacco shreds can reach or even exceed that of tobacco leaf raw materials of 1 cigarette, the content of the components of the tobacco shred expanding agent is ensured to be high enough, the method is particularly suitable for analyzing trace chemical components, and one-time analysis is ensured to be completed. Can meet the requirement of rapid analysis of a large amount of tobacco shred raw materials, and provides a new method for rapid analysis of components of the tobacco shred expanding agent in the tobacco shreds.
Description
Technical Field
The invention relates to a method for detecting a tobacco shred swelling agent, and belongs to the technical field of instrument analysis and detection.
Background
The tobacco shred raw materials are important factors influencing the sensory quality of the cigarettes, and the expanded tobacco shreds can reduce the consumption of the tobacco shreds in a single box of the cigarettes and can also reduce the tar release amount of the cigarettes. The tar content of smoke of the cigarette doped with 10% of expanded cut tobacco is reduced by 14.7% compared with the cigarette not doped with the expanded cut tobacco, and if the expanded cut tobacco is completely used, the tar content can be reduced by 41%. Thus, tobacco expansion agents are one of the important areas of research in the tobacco industry.
In the prior art, a carbon dioxide tobacco shred expansion technology and a Freon tobacco shred expansion technology are commonly used. But the carbon dioxide expansion method has large investment, high breakage rate, large tobacco shred loss, complex production process and high production cost. The traditional freon tobacco shred expansion agent (trichlorofluoromethane CFC-11) has an ODP index of 1.0 and a great damage to the ozone layer, and is forbidden to use. In order to fill up the technical blank caused by the CFC-11 tobacco shred expansion technology, some environmental-friendly tobacco shred expansion agents capable of replacing CFC-11 are reported, and the application of the environmental-friendly tobacco shred expansion agents is reported in patents CN 1823637A, CN 1199592C, CN 101766328A, CN 110973684A, CN 111264898A, CN 101617854B and CN 107981408B. Chinese patent CN 1823637A discloses a tobacco shred expansion agent composition, which discloses five tobacco shred expansion agent compositions, wherein the first tobacco shred expansion agent composition is composed of pentafluorobutane and heptafluoropropane, the second tobacco shred expansion agent composition is composed of pentafluorobutane and hexafluoropropane, the third tobacco shred expansion agent composition is composed of pentafluorobutane and pentafluoropropane, the fourth tobacco shred expansion agent composition is composed of pentafluorobutane and tetrafluoroethane, and the fifth tobacco shred expansion agent composition is composed of pentafluorobutane and decafluoropentane. Chinese patent CN 1199592C discloses a tobacco shred swelling agent which is composed of dichloromonofluoroethane and perfluoropentane or perfluorohexane in a certain proportion, has the characteristics of zero or very low ozone consumption potential, moderate boiling point, safety, low toxicity, incombustibility, easy volatilization and the like, and can replace CFC-11 to be used as the tobacco shred swelling agent in the tobacco industry. Chinese patent CN 101766328A environmental protection tobacco shred expansion agent composition, the composition of the environmental protection tobacco shred expansion agent composition by mass percentage is as follows: 50-99% of fluorinated alkane and 1-50% of alcohol or ether or alkane, wherein the fluorinated alkane is one or any combination of more of pentafluoropropane, pentafluorobutane, decafluoropentane or methoxy heptafluoropropane; preferably 80 to 99 percent of fluorinated alkane and 1 to 20 percent of alcohol or ether or alkane; more preferably 90 to 99% of fluoroalkane, and 1 to 10% of alcohol, ether or alkane. Chinese patent CN 110973684A discloses a tobacco shred expanding agent and a tobacco shred expanding method, wherein the components of the tobacco shred expanding agent comprise hydrochlorofluoroalkane and fluoroalkane, and the mass ratio of the hydrochlorofluoroalkane to the fluoroalkane is 95.0-99.8:0.2-5.0. The hydrogen-containing chlorofluoroalkane comprises at least one of monofluorodichloroethane, difluoromonochloroethane and trifluorodichloroethane; the fluoroalkane includes at least one of pentafluoropropane, pentafluorobutane and decafluoropentane. Chinese patent CN 111264898A discloses a tobacco shred swelling agent, which comprises the following components in percentage by mass: 4 to 98 percent of halogenated olefin; 1 to 50 percent of ester compound; 1 to 20 percent of halogenated ether or halogenated alcohol. Chinese patent CN 101617854B discloses a circulation method for preparing expanded tobacco shred, wherein the liquid expanding agent and the gaseous expanding agent are respectively one or more of alcohol with 2-12 carbon atoms, ketone with 2-12 carbon atoms, halogenated ether with 2-12 carbon atoms, alkane with 2-12 carbon atoms or halogenated alkane with 2-12 carbon atoms. Preferably one or a mixture of two or more of tetrafluoroethane, pentafluoropropane, pentafluorobutane, decafluoropentane or methoxynonafluorobutane. Chinese patent CN 107981408B discloses a novel tobacco shred swelling agent which is characterized by comprising pentafluorobutane, citric acid and butyl hydroxy anisole, and the mass ratio is 75. The alternative tobacco shred swelling agent is the same as CFC-11, and adopts liquid phase swelling method, i.e. the condensed volatile substance is fully soaked with the tobacco shred, then the soaked tobacco shred is heated, the swelling medium is quickly volatilized, the cell wall of the tobacco shred is pushed outwards, and the effect of swelling the tobacco shred is achieved.
In summary, most of the expanding agents used in the freon tobacco shred expansion technology in the prior art are halogenated hydrocarbon compounds or compositions, and the types of the expanding agents are more, and because the tobacco shred expanding agents are additionally added substances, part of the tobacco shred expanding agents are remained in the expanded tobacco shreds, and the remained tobacco shred expanding agents can influence the smoking safety of cigarettes and the quality of the cigarettes. The existing tobacco industry standard does not make relevant regulations on the residue of the expanding agent in the cut tobacco, and the related detection method of the cut tobacco expanding agent at home and abroad is not reported at present. Therefore, how to quickly detect the tobacco shred expanding agent contained in the tobacco shred has important reference and scientific research significance for improving the production technical level of the tobacco shred and exploring the tobacco shred suitable for the production requirement of Chinese style cigarettes.
Disclosure of Invention
The invention aims to provide a method for detecting a tobacco shred swelling agent, which utilizes HS-GC/MS to measure the components of the tobacco shred swelling agent, can carry out rapid analysis, is simple and convenient to operate, does not need pretreatment, has less manual intervention, greatly improves the working efficiency and the analysis accuracy, can meet the rapid analysis of a large amount of tobacco shred raw materials, and provides a new method for the rapid analysis of the chemical components of the tobacco shred swelling agent in the tobacco shreds.
In order to achieve the purpose, the technical scheme adopted by the invention for solving the technical problems is as follows: a detection method of a tobacco shred swelling agent is measured by a headspace-gas chromatography-mass spectrometry combined method, and is characterized by comprising the following steps:
s1: sample treatment: the expanded tobacco shred sample and the headspace bottle are placed under constant temperature and constant humidity to be balanced for 2 hours;
s2: selecting a sample: accurately weighing 0.5-2.0 g of tobacco shred samples, and immediately sealing;
s3: the samples were analyzed by headspace-gas chromatography/mass spectrometer.
Preferably, the tobacco leaf sample and the headspace bottle in the step A are processed under the conditions of temperature 22 +/-2 ℃ and relative humidity 60 +/-5% for balancing for 1 to 3h.
Preferably, the mass of the cut tobacco sample in the step B is 1.0g.
Preferably, the headspace gas chromatography-mass spectrometry conditions in step C are as follows:
and (3) headspace conditions: 3.0mL of sample ring, 110 ℃ of sample ring, 280 ℃ of transmission line, 20min of sample balancing time, 50psi of sample bottle pressurization pressure, 2.0min of pressurization time, 0.5min of aeration time and 0.10min of sample introduction time;
gas chromatography conditions: capillary chromatographic column DB-624 with specification of 30m × 0.32mm × 1.80 μm; the carrier gas is helium with the purity more than or equal to 99.999 percent; the temperature of a sample inlet is 250 ℃; constant flow mode, main flow 1.3mL/min, solvent delay time: 0.5min, sample injection mode: split-flow sample injection, split ratio 20:1; temperature programming conditions: the initial temperature is 40 ℃, the temperature is kept for 2min, the temperature is increased to 220 ℃ at the speed of 10 ℃/min, and the temperature is kept for 5min;
mass spectrum conditions: an ionization mode: EI; ionization voltage: 70eV; full scan, scan range: 30-300amu; ion source temperature: 230 ℃; quadrupole temperature: 150 ℃; transmission line temperature: 280 ℃; searching a spectrogram: the WILEY, NIST08 spectral library was searched.
(1) The detection method of the tobacco shred swelling agent provided by the invention utilizes HS-GC/MS to measure the components of the tobacco shred swelling agent, can be used for carrying out rapid analysis, is simple and convenient to operate, does not need pretreatment, has less manual intervention, and greatly improves the working efficiency and the analysis accuracy.
(2) The detection method of the tobacco shred expanding agent provided by the invention can simulate the volatilization process of the expanding agent after tobacco shreds are expanded, is reasonable in design, accurate in measurement, scientific and reliable, and is suitable for popularization in the industry.
(3) According to the detection method of the tobacco shred expanding agent, the tobacco shred consumption can reach or even exceed the tobacco leaf raw material of 1 cigarette (0.7 g of tobacco shred), the sufficient high content of the tobacco shred expanding agent is ensured, the method is especially suitable for analyzing trace chemical components, and the completion of one-time analysis is ensured. Can meet the requirement of rapid analysis of a large amount of tobacco shred raw materials, and provides a new method for rapid analysis of chemical components of tobacco shred expanding agents in the tobacco shreds.
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FIG. 1 is a chromatogram of a detection method of a tobacco shred swelling agent.
Description of the preferred embodiment
The present invention will be further described with reference to the following examples, but the present invention is not limited to these examples. It will be appreciated by those skilled in the art that the present invention encompasses all alternatives, modifications and equivalents as may be included within the scope of the claims.
1. Instruments and reagents
Headspace autosampler: agilent 7697A, agilent Inc. USA.
Gas chromatography-mass spectrometer: agilent 7890B-5977A, agilent Inc., USA.
Capillary column: agilent DB-624, 30 m.times.0.30 mm.times.1.8 μm, agilent Inc., USA.
Balance: an AL 204 ten-thousandth balance (MEITLER TOLEDO, switzerland).
And (3) vacuum drying oven: DZF-6012, shanghai-Heng scientific instruments, inc.
1, 4-hexafluorobutane: purity 98%, beijing Bailingwei science and technology Co.
1,2,3,4, 5-decafluoropentane: purity 98%, by Beijing Bailingwei science and technology Co.
1, 3-pentafluoropropane: purity 99%, shanghai Yujisaifu science and technology Limited.
Trans-1-chloro-3, 3-trifluoropropene: purity 99%, shanghai Yutesai fluorine science and technology Limited.
Cis-1, 3-tetrafluoropropene: purity 99%, shanghai Yujisaifu science and technology Limited.
Cis-1, 4-hexafluoro-2-butene: purity 99%, shanghai Yujisaifu science and technology Limited.
2. Standard samples: as the tobacco shred swelling agent has more substances in the formula, the halogenated hydrocarbon compounds commonly used in 6 are selected, and a proper amount of the 6 reference substances are accurately weighed in a 10 mL volumetric flask to obtain a standard sample.
3. Checking the performance of the instrument: 1 mu L of 4-bromofluorobenzene (BFB) solution is taken to enter a sample through a GC sample inlet, or is added into a headspace bottle to be injected through a headspace autosampler, and is analyzed by GC/MS, the obtained BFB key ion abundance meets the standard specified in the table 1, otherwise, some parameters of a mass spectrometer need to be adjusted or the ion source needs to be cleaned.
4. Blank test: accurately weighing 1.0g of the expanded tobacco sample, putting the tobacco sample into a ground bottle, placing the ground bottle in a vacuum oven with the opening at 80 ℃ and the vacuum degree higher than 50kPa for more than 180min to prepare a blank sample, placing the prepared blank sample into a sample disc of a headspace automatic sample injector, and measuring according to the reference conditions of the instrument. And (3) determining the prepared blank sample under the working condition of an instrument, wherein the content of the substance to be detected is lower than the detection limit of the method, or repeating the vacuum drying operation.
5. And (3) detection of a low limit: the detection limits of the present method for 1,1,1,4,4,4-hexafluorobutane, 1,1,1,2,3,4,5,5,5-decafluoropentane, 1,1,3,3-pentafluoropropane, trans-1-chloro-3,3,3-trifluoropropene, cis-1,1,1,3-tetrafluoropropene, 1,1,1,4,4-hexafluoro-2-butene are as follows:
quantification of the target compound: and quantifying by using a correction area normalization method.
8. Selection of equilibrium temperature: headspace gases at different equilibrium temperatures (80 ℃, 90 ℃, 100 ℃, 110 ℃, 120 ℃, 130 ℃) were analyzed at the same equilibrium time (20 min) and the effect of the equilibrium temperature on the response value was examined. From the results, it is understood that peak area response values of the target and the internal standard gradually increase with increasing equilibrium temperature, and increase more rapidly and then decrease gradually before 110 ℃. Comprehensively considering that the headspace bottle pressure is too high when the temperature is too high, 110 ℃ is selected as the sample equilibrium temperature.
9. Selection of the equilibration time: the headspace gases at different equilibrium times (5 min,10 min, 15min, 20min, 30min, 40 min) were analyzed at the same temperature time (110 ℃) to examine the influence of the equilibrium time on the response values. Basically, peak area response values of a target compound and an internal standard show a gradual increase trend after 5-40 min, after 25min, the speed increase tends to be gentle, the detection efficiency is comprehensively considered, and 20min is preferably used as the balance time of a sample.
According to the method and the steps, 6 samples of the expanded cut tobacco of the same batch are selected for analysis and determination, and the detection results are shown in the following table:
note: (1) the unit is ug/kg; (2) ND is not detected; (3) Because the variety of the tobacco shred expanding agents contained in the standard sample is more, only a few tobacco shred expanding agents can be used in the actual production due to different formulas.
It should be noted that the above-mentioned preferred embodiments are merely illustrative of the technical concepts and features of the present invention, and are intended to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (6)
1. A detection method of a tobacco shred swelling agent is measured by a headspace-gas chromatography-mass spectrometry combined method, and is characterized by comprising the following steps:
s1: sample treatment: the expanded tobacco shred sample and the headspace bottle are placed at constant temperature and constant humidity and are balanced for 2 hours:
s2: selecting a sample: accurately weighing 0.5-2.0 g of tobacco shred samples, and immediately sealing;
s3: the samples were analyzed by headspace-gas chromatography/mass spectrometer.
2. The method for detecting the tobacco shred swelling agent according to claim 1, wherein the method comprises the following steps: and B, the tobacco shred sample and the headspace bottle in the step A are subjected to balance 1-3h pretreatment under the conditions of the temperature of 22 +/-2 ℃ and the relative humidity of 60 +/-5%.
3. The method for detecting the tobacco shred swelling agent according to claim 1, wherein the method comprises the following steps: and the mass of the tobacco leaf sample in the step B is 1.0g.
4. The method for detecting the tobacco shred swelling agent according to claim 1, wherein the method comprises the following steps: headspace conditions in step C: 3.0mL of sample ring, 110 ℃ of sample ring, 280 ℃ of transmission line, 20min of sample balance time, 50psi of sample bottle pressurization pressure, 2min of pressurization time, 0min of aeration time and 0.10min of sample introduction time.
5. The method for detecting the tobacco shred swelling agent according to claim 1, wherein the method comprises the following steps: gas chromatography conditions in step C: capillary chromatographic column DB-624 with specification of 30m × 0 32mm × 1.80 μm; the carrier gas is helium with the purity more than or equal to 99.999 percent; the temperature of a sample inlet is 250 ℃; constant flow mode, main flow 1.3mL/min, solvent delay time: 0.5min, sample injection mode: split-flow sample injection, split ratio 20:1; temperature programming conditions: the initial temperature was 40 deg.C, held for 2min, ramped to 220 deg.C at 10 deg.C/min, and held for 5min.
6. The method for detecting the tobacco shred swelling agent according to claim 1, wherein the method comprises the following steps: mass spectrometry conditions in step C: an ionization mode: EI; ionization voltage: 70eV; full scan, scan range: 30-300amu; ion source temperature: 230 ℃; quadrupole temperature: 150 ℃; transmission line temperature: 280 ℃; searching a spectrogram: the WILEY, NIST08 spectral library was searched.
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