CN109580798B - Method for detecting residual expanding medium in cut tobacco - Google Patents
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- CN109580798B CN109580798B CN201710904817.5A CN201710904817A CN109580798B CN 109580798 B CN109580798 B CN 109580798B CN 201710904817 A CN201710904817 A CN 201710904817A CN 109580798 B CN109580798 B CN 109580798B
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Abstract
The invention provides a method for detecting residual expansion media in cut tobacco, which comprises the following steps: and mixing the expanded tobacco shred sample with cyclohexane, and performing static headspace-gas chromatography-mass spectrometry combined detection to analyze the KC-2A content in the expanded tobacco shred sample. Based on the low boiling point and volatile chemical characteristics of a KC-2A medium and the characteristics of static headspace-gas chromatography (SHS-GC) technology, the invention establishes a rapid and accurate static headspace-gas chromatography-mass spectrometry method to determine the residue of an expansion medium in tobacco shreds, and provides technical support for perfecting the use process technology of a novel expansion medium KC-2A and improving the smoking quality of cigarettes.
Description
Technical Field
The invention relates to the technical field of detection and analysis, in particular to a method for detecting a residual expanding medium in cut tobacco.
Background
In recent years, with the advance of the work of tar and harm reduction and cost reduction and efficiency improvement in the tobacco industry, the usage amount of expanded cut tobacco and cut stems is higher and higher, mainly because the expanded cut tobacco or the cut stems have the advantages of strong filling capacity, good combustion performance, obvious tar and harm reduction effects and the like, the consumption amount of the cut tobacco in a single box of cigarettes can be reduced and the tar release amount of the cigarettes can be reduced when the expanded cut tobacco or the cut stems are used in a cigarette formula, so that the tobacco expansion technology is always one of the important research fields of the tobacco industry, researchers at home and abroad increasingly carry out deep research on tobacco expansion technology and equipment, and new technology are continuously developed to become an important component part in the cigarette manufacturing process.
The traditional CFCs tobacco shred expansion method is eliminated, the dry ice expansion method is used most mature, and a plurality of novel expansion technologies such as steam expansion technology and microwave expansion technology are provided. The tobacco expansion method used at home and abroad mainly comprises the following steps: steam, dry ice, liquid nitrogen, SP series cut tobacco expanding agent KC-2A and the like. The tobacco shreds expanded by the expansion medium KC-2A have bright color and full body state, and are a good tobacco shred expansion agent. Researches find that when the novel expansion medium KC-2A is applied to actual production, if the process is incomplete, the problem of medium residue exists, and the medium residue can directly influence the smoking quality of cigarettes, so that the establishment of a rapid and accurate analysis method for detecting the expansion medium residue in tobacco shreds is particularly important, thereby guiding the process improvement and reducing the expanded tobacco shred medium residue. At present, the residue detection of KC-2A serving as a novel expansion medium of tobacco shreds is not reported.
Disclosure of Invention
In view of this, the present invention provides a method for detecting the residual swelling medium in the cut tobacco.
The invention provides a method for detecting residual expansion media in cut tobacco, which comprises the following steps:
mixing the expanded tobacco shred sample with cyclohexane to obtain a mixed solution;
and (3) carrying out static headspace-gas chromatography-mass spectrometry combined detection on the mixed solution, and analyzing the content of KC-2A in the expanded tobacco shred sample.
In the invention, the preparation method of the expanded cut tobacco sample comprises the following steps:
and soaking the unexpanded cut tobacco sample in an expansion medium KC-2A for microwave heating expansion to obtain an expanded cut tobacco sample.
The source of the unexpanded cut tobacco is not particularly limited in the present invention, and cut tobacco which is not subjected to expansion treatment and is well known to those skilled in the art can be used, and can be obtained commercially.
The method comprises the steps of introducing the mixed solution into an automatic headspace analyzer for sample injection, and detecting the obtained headspace gas by using a gas chromatography-mass spectrometer.
The content of each component in the headspace gas is related to the volatility of the headspace gas and the sample matrix, especially the components with high solubility (large distribution coefficient) in the sample matrix, and the matrix effect is more obvious, namely the composition of the headspace gas is different from that in the original sample, which has serious adverse effect on quantitative analysis. The inventor researches on a large number of experiments to find that the matrix effect of a sample can be effectively eliminated by selecting a matrix which is the same as that of a standard solution in a quantitative analysis sample so as to accurately perform the quantitative analysis.
The method adopts cyclohexane as a matrix correction agent, and mixes the expanded tobacco shred sample and the cyclohexane to obtain a mixed solution. The inventor finds that the boiling points of methanol, n-hexane and ethyl acetate are 64.5 ℃, 68.7 ℃ and 77.0 ℃ respectively, the peak emergence time of the solvents is closer to the medium KC-2A, the accurate integral quantification of the medium is influenced, and the solvents are not suitable for being used as the matrix correction agent of the medium KC-2A. Cyclohexane has a boiling point of 80.0 ℃, is a better hydrophilic reagent, can dissolve KC-2A medium, enables a sample to be uniformly dispersed in a matrix solvent, and enables a quantitative result to be more accurate, so cyclohexane is selected as a matrix correcting agent.
In the present invention, the concentration of the expanded tobacco sample in the mixed solution is preferably 0.3 to 0.7g/mL, more preferably 0.4 to 0.6g/mL, and most preferably 0.5g/mL.
The inventor conducts research on the basis of a large number of experiments, and determines that the equilibrium temperature of the static headspace in the process of combining the static headspace with the gas chromatography-mass spectrometry is preferably 40-80 ℃, more preferably 50-70 ℃, most preferably 55-65 ℃ and most preferably 60 ℃ according to the characteristics of the headspace and the physicochemical property of a target compound; the equilibration time for the static headspace is preferably 10 to 30min, more preferably 15 to 25min, most preferably 15min.
In the invention, the detection conditions of the static headspace in the process of combining the static headspace with the gas chromatography-mass spectrometry are as follows:
the temperature of the sample ring is preferably 110-130 ℃, more preferably 115-125 ℃, and most preferably 120 ℃;
the temperature of the transmission line is preferably 130 to 150 ℃, more preferably 135 to 145 ℃, and most preferably 140 ℃;
the pressurization pressure is preferably 30 to 40psi, more preferably 34 to 36psi, most preferably 35psi;
the pressurizing time is preferably 1.8 to 2.5min, more preferably 1.8 to 2.2min, and most preferably 2min;
the carrier gas pressure is preferably 35 to 45psi, more preferably 38 to 42psi, most preferably 40psi;
the aeration time is preferably 0.15 to 0.25min, more preferably 0.18 to 0.22min, and most preferably 0.2min;
the sample loop equilibration time is preferably 0.04 to 0.06min, more preferably 0.05min.
In the invention, a static headspace-gas chromatography-mass spectrometry combined process is carried out, and the inventor finds that an HP-PONA (50 m multiplied by 0.2mm multiplied by 0.5 mu m) capillary column is preferably selected as a chromatographic separation column according to the physicochemical properties of an analysis target object in the gas chromatography detection process on the basis of a large number of experiments, so that the target object can be well separated from a base line. In the present invention, the column flow rate of the column in the gas chromatography detection is preferably 0.6 to 1mL/min, more preferably 0.7 to 0.9mL/min, and most preferably 0.8mL/min.
During gas chromatography detection, the inventor conducts research on the basis of a large number of experiments, and optimizes the furnace temperature and the programmed temperature, so that the whole separation process can be completed within 21.5 min. In the present invention, the furnace temperature control at the time of gas chromatography detection is preferably:
the initial furnace temperature is kept at 30-50 ℃ for 3-5 min, the temperature is increased to 70-90 ℃ at 2-6 ℃/min, and then the temperature is increased to 140-160 ℃ at 15-25 ℃/min, and the temperature is kept for 4-6 min.
More preferably:
the initial furnace temperature is kept at 35-45 ℃ for 3.5-4.5 min, the temperature is increased to 75-85 ℃ at 3-5 ℃/min, and then the temperature is increased to 145-155 ℃ at 18-22 ℃/min, and the temperature is kept for 4.5-5.5 min.
Most preferably:
the initial furnace temperature is kept at 40 ℃ for 4min, the temperature is increased to 80 ℃ at 4 ℃/min, and then the temperature is increased to 150 ℃ at 20 ℃/min for 5min.
In the present invention, the temperature raising procedure at the time of gas chromatography detection is preferably:
the initial temperature is 140-160 ℃, the temperature is raised to 275-285 ℃ at the heating rate of 4-8 ℃/min, the temperature is kept for 3-7 min, the temperature is raised to 290-310 ℃ at the heating rate of 8-12 ℃/min, and the temperature is kept for 13-17 min.
More preferably:
the initial temperature is 145-155 ℃, the temperature is increased to 278-282 ℃ at the temperature rising speed of 5-7 ℃/min, the temperature is kept for 4-6 min, the temperature is increased to 295-305 ℃ at the temperature rising speed of 9-11 ℃/min, and the temperature is kept for 14-16 min.
Most preferably:
the initial temperature is 150 ℃, the temperature is increased to 280 ℃ at the heating rate of 6 ℃/min, the temperature is maintained for 5min, the temperature is increased to 300 ℃ at the heating rate of 10 ℃/min, and the temperature is maintained for 15min.
In the invention, the detection conditions of the gas chromatography in the process of combining the static headspace-gas chromatography-mass spectrometry are as follows:
the injection port temperature is preferably 140-160 ℃, more preferably 145-155 ℃, and most preferably 150 ℃;
the constant-flow mode is preferred for sample injection, and the split ratio in the sample injection process is preferably (40-60): 1, more preferably (45-55): 1, most preferably 50;
preferably, the carrier gas is argon gas, more preferably high-purity argon gas, and the purity of the argon gas is preferably more than or equal to 99.999 percent.
In the invention, when mass spectrometry is detected in the process of combining static headspace-gas chromatography-mass spectrometry, the inventors adopt mass spectrometry to obtain identification information of a medium KC-2A by selecting ion scanning, wherein the identification information of KC-2A is shown in Table 1; research is carried out on the basis of a large number of experiments, and the target compound can obtain a better chromatogram when the medium KC-2A selectively monitors 81 characteristic ions, as shown in figure 3.
TABLE 1 authentication information for media KC-2A
In the invention, the detection conditions of the mass spectrum in the process of combining the static headspace-gas chromatography-mass spectrometry are as follows:
EI ionization energy is preferably 60-80 eV, more preferably 65-75 eV, and most preferably 70eV;
the ion source temperature is preferably 220 to 240 ℃, more preferably 225 to 235 ℃, and most preferably 230 ℃;
the temperature of the transmission line is preferably 240-260 ℃, more preferably 245-255 ℃ and most preferably 250 ℃;
the solvent delay time is preferably 0.1 to 0.3min, more preferably 0.15 to 0.25min, and most preferably 0.2min;
the scanning mode is preferably full scanning, and the scanning range is preferably 29-400aeu;
the selection of the monitor ion is preferably 81, more preferably 61 and 81.
The invention solves the important technical problems that: 1) Optimizing the balance time and the balance temperature and selecting a matrix correction agent in the detection method; 2) Performing external standard quantitative analysis on the medium KC-2A in the sample by using SHS-GC/MS, and determining a regression equation and a correlation coefficient of the expansion medium KC-2A, and a detection limit and a quantification limit of a detection method; 3) And (4) determining the recovery rate and precision of the detection method.
Through a large amount of researches, based on the characteristics of the KC-2A medium, such as low boiling point and volatile chemical characteristics and static headspace-gas chromatography (SHS-GC) technology, the residue of the expansion medium in the cut tobacco is determined by optimizing experimental conditions and establishing a rapid and accurate static headspace-gas chromatography-mass spectrometry method, so that technical support is provided for perfecting the use process technology of the novel expansion medium KC-2A and improving the smoking quality of cigarettes.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the embodiments or the prior art descriptions will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
FIG. 1 is a graph showing the effect of headspace equilibration time on peak area as tested in example 1 of the present invention;
FIG. 2 is a graph showing the effect of headspace equilibrium temperature on peak area as measured in example 2 of the present invention;
FIG. 3 is a selective ion chromatogram of medium KC-2A (a) and expanded tobacco sample (b) in the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The KC-2A used in the following examples of the invention is a product provided by the Peking institute for aerospace testing and technology 101.
The unexpanded cut tobacco sample used was a product provided by cupren cigarette factory, a company limited in the tobacco industry, guizhou.
The method for obtaining the used expanded cut tobacco sample comprises the following steps:
and soaking the unexpanded tobacco shred sample by adopting an expansion medium KC-2A, and then performing microwave heating expansion to obtain the expanded tobacco shred sample.
The SHS-GC/MS (static headspace-gas chromatography-mass spectrometry) detection equipment is a gas chromatography-mass spectrometer and an automatic headspace instrument.
Example 1
Weighing 0.5g (accurate to 0.001 g) of expanded tobacco shred sample into a 20mL headspace bottle, adding 1mL cyclohexane, quickly pressing the bottle cap, putting into a headspace sample injector of an automatic headspace instrument, and measuring the obtained headspace gas by a gas chromatography-mass spectrometer.
Performing quantitative analysis and detection on an expansion medium KC-2A in tobacco shreds by using an SHS-GC/MS (static headspace-gas chromatography-mass spectrometry) through an external standard method, wherein the detection conditions are as follows:
static headspace detection:
sample equilibrium temperature: 60 ℃; sample ring temperature: 120 ℃; transmission line temperature: l40 ℃; sample equilibration time: 15min; sample bottle pressurization pressure: 35psi; carrier gas pressure: 40psi; pressurizing time: 2.0min; and (3) inflating time: 0.20min; sample loop equilibration time: 0.05min; sample introduction time: 0.1min.
Gas chromatography detection:
and (3) chromatographic column: HP-PONA capillary columns (50 m.times.0.2 mm. Times.0.5 μm); furnace temperature: preserving the heat for 4min at the initial temperature of 40 ℃, raising the temperature to 80 ℃ at the speed of 4 ℃/min, and then raising the temperature to 150 ℃ at the speed of 20 ℃/min and preserving the heat for 5min; sample inlet temperature: 150 ℃, split ratio: 50; carrier gas: high-purity helium with the purity more than or equal to 99.999 percent; constant flow mode, column flow: 0.8mL/min.
Detecting a temperature rise program: the initial temperature is 150 ℃, the temperature is increased to 280 ℃ at the heating rate of 6 ℃/min, the temperature is kept for 5min, the temperature is increased to 300 ℃ at the heating rate of 10 ℃/min, and the temperature is kept for 15min.
Mass spectrum detection:
EI ionization energy: 70eV; ion source temperature: 230 ℃, transmission line temperature: 250 ℃, solvent retardation: 0.2min, scanning mode: full scan, scan range 29-400aeu; ion Monitoring (SIM) was selected, monitoring ions 61 and 81.
The detection result obtained by the method provided by the embodiment 1 of the invention is that the residue of KC-2A is 5.28 mug/g, and the method provided by the invention is suitable for detecting the residue of the tobacco shred expansion medium KC-2.
Example 2
Adding 70 mu g/mL KC-2A medium standard solution into unexpanded tobacco shred, and measuring the balance time at the balance temperature of 60 ℃ for 10min, 15min, 20min and 30min respectively under the same other detection conditions as in example 1. The measurement results are shown in FIG. 1. As can be seen from FIG. 1, the peak area equilibrium time of the medium KC-2A response chromatogram is slightly increased from 10min to 15min, slightly decreased from 15min to 20min, and basically no difference exists between 20min and 30 min. As the medium KC-2A has a low boiling point and is volatile, the influence of the relative balance time is small, and the balance time of 15min is selected to be optimal for fully balancing the sample to be detected.
Example 3
KC-2A medium standard solution of 70 mu g/mL is added into unexpanded cut tobacco, and the measurement is carried out at the equilibrium temperature of 40 ℃, 50 ℃, 60 ℃ and 80 ℃ respectively under the equilibrium time of 15min, and other detection conditions are the same as those in example 1. The detection result is shown in figure 2, and as can be seen from figure 2, with the increase of the equilibrium temperature, the peak area of the KC-2A medium is gradually increased, the acceleration is slightly small at 40-60 ℃, the acceleration is obvious at 60-80 ℃, the residual quantity of the expansion medium KC-2A in the expanded tobacco shred at normal temperature is usually detected, the boiling point of the medium KC-2A is low, the requirements of sufficient volatilization of the sample medium KC-2A are considered, the sensitivity of the method is improved, the sample matrix interference is reduced, and the equilibrium temperature of 60 ℃ is selected to be optimal.
EXAMPLE 4 determination of working curves and detection limits
Preparing a KC-2A medium standard solution:
10 μ L of KC-2A medium was measured in 10mL of cyclohexane solvent, the medium weighed 7.0mg, and the concentration was 0.7mg/mL.
KC-2A medium working curve:
respectively measuring 5 mu L, 10 mu L, 20 mu L, 50 mu L, 100 mu L and 150 mu L KC-2A medium standard solutions to prepare a series of standard solutions in 1mL cyclohexane solvent, wherein the mass concentrations are respectively 3.5 mu g/mL, 7.0 mu g/mL, 14 mu g/mL, 35 mu g/mL, 70 mu g/mL and 105 mu g/mL, and respectively adding 0.5g of unexpanded tobacco shreds.
The 7 standard solutions with different concentrations are analyzed and detected according to the method described in example 1, and regression analysis is carried out by taking the KC-2A medium chromatographic peak area as the ordinate and the corresponding mass concentration X (mu g/mL) as the abscissa to obtain the regression equation Y =1741.89X (r is the equation R) 2 = 0.9999). The detection limit was calculated to be 0.03. Mu.g/mL with a signal-to-noise ratio of 3 times (S/N. Gtoreq.3).
Example 5 recovery and reproducibility of the detection method
0.5g of unexpanded tobacco (medium KC-2A content of 0.0 μ g) was weighed out, and 1mL of the mixture was added: 5.0. Mu.g/mL, 10.0. Mu.g/mL, 20.0. Mu.g/mL of a standard solution containing KC-2A was assayed in parallel 6 times per concentration by the method of example 1, and the recovery rate was calculated from the amount measured, the amount of addition, and the original content.
The detection results are shown in table 2, and table 2 shows the recovery rate and repeatability of KC-2A obtained by the method provided by the embodiment of the invention.
TABLE 2 recovery and reproducibility of KC-2A obtained by the method provided in the examples of the present invention (n = 6)
As can be seen from Table 2, the detection method provided by the invention has the advantages of simple and convenient sample pretreatment operation, rapidness, good repeatability and high accuracy. The method provided by the invention can accurately detect the residue of the tobacco shred expansion medium KC-2, and is simple, convenient and rapid.
As can be seen from the above embodiments, the present invention provides a method for detecting a residual swelling medium in tobacco shreds, including: and mixing the expanded tobacco shred sample with cyclohexane, and performing static headspace-gas chromatography-mass spectrometry combined detection to analyze the KC-2A content in the expanded tobacco shred sample. Based on the low boiling point and volatile chemical characteristics of a KC-2A medium and the characteristics of static headspace-gas chromatography (SHS-GC) technology, the invention establishes a rapid and accurate static headspace-gas chromatography-mass spectrometry method to determine the residue of an expansion medium in tobacco shreds, and provides technical support for perfecting the use process technology of a novel expansion medium KC-2A and improving the smoking quality of cigarettes.
Claims (5)
1. A method of detecting residual swelling medium in cut tobacco, comprising:
mixing the expanded tobacco shred sample with cyclohexane to obtain a mixed solution;
performing static headspace-gas chromatography-mass spectrometry combined detection on the mixed solution, and analyzing the content of KC-2A in the expanded tobacco shred sample;
the detection conditions of the static headspace in the process of the static headspace-gas chromatography-mass spectrometry are as follows:
the equilibrium temperature is 40-80 ℃;
the balance time is 10-30 min;
the detection conditions of the gas chromatography in the static headspace-gas chromatography-mass spectrometry combined process are as follows:
the chromatographic column is an HP-PONA capillary column, and the flow rate of the chromatographic column is 0.6-1 mL/min;
the furnace temperature is controlled as follows: the temperature is initially kept at 35-45 ℃ for 3-5 min, then the temperature is raised to 70-90 ℃ at 3-5 ℃/min, and then the temperature is raised to 140-160 ℃ at 15-25 ℃/min, and the temperature is kept for 4-6 min;
the sample introduction temperature is 140-160 ℃;
the detection conditions of the mass spectrum in the static headspace-gas chromatography-mass spectrometry combined process are as follows:
EI ionization energy is 65-75 eV;
the temperature of the ion source is 220-240 ℃,
the temperature of the transmission line is 240-260 ℃;
the solvent delay time is 0.1-0.3 min;
the scanning mode is full scanning, and the scanning range is 29-400aeu;
the monitor ions were selected to be 61 and 81.
2. The method according to claim 1, wherein the expanded cut tobacco sample is prepared by:
and soaking the unexpanded tobacco shred sample in an expansion medium KC-2A for microwave heating expansion to obtain an expanded tobacco shred sample.
3. The method according to claim 1, wherein the concentration of the expanded tobacco sample in the mixed solution is 0.3-0.7 g/mL.
4. The method of claim 1, wherein the detection conditions for the static headspace during the static headspace-gas chromatography-mass spectrometry combination are:
the temperature of the transmission line is l 30-150 ℃;
the pressurizing pressure is 30-40 psi;
the pressurizing time is 1.5-2.5 min.
5. The method of claim 1, wherein the detection conditions for the static headspace during the static headspace-gas chromatography-mass spectrometry combination are:
the pressure of the carrier gas is 35-45 psi;
the aeration time is 0.15-0.25 min;
sample introduction time: 0.05-0.15 min.
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