CN109580798A - A kind of method of remaining inflating medium in detection pipe tobacco - Google Patents
A kind of method of remaining inflating medium in detection pipe tobacco Download PDFInfo
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Abstract
The present invention provides a kind of method of remaining inflating medium in detection pipe tobacco, comprising: will expanded cut tobacco sample and hexamethylene mix after carry out Static Headspace-gas chromatography-mass spectrography combination detection, analyze the content of KC-2A in expanded cut tobacco sample.The present invention is based on the low boiling point of KC-2A medium, volatile chemical characteristic and Static Headspace-gas-chromatography (static headspace gas chromatography, SHS-GC) the characteristics of technology, it establishes fast and accurately Static Headspace-gas chromatography-mass spectrography and measures the residual of inflating medium in pipe tobacco, to improve use technology and the raising smoking property of cigarette quality of expansible medium KC-2A provide technical support.
Description
Technical field
The present invention relates to the sides for testing and analyzing remaining inflating medium in technical field more particularly to a kind of detection pipe tobacco
Method.
Background technique
In recent years, with the propulsion that tobacco business " reducing tar and reducing harm " and " cost efficiency " work, expanded cut tobacco and stem
Usage amount is also higher and higher, and mainly since expanded cut tobacco or stem have, filling capacity is strong, has good burning performance, reducing tar and reducing harm effect
The advantages that fruit is obvious uses the consumption that can not only reduce cigarette list case pipe tobacco in cigarette composition, but also can reduce the coke of cigarette
Oily burst size, therefore, expanding tobacco technology are always one of important research field of tobacco business, and researchers at home and abroad are numerous and confused
Tobacco expansion process technology and equipment are furtherd investigate, new technology, new process continue to bring out, and become cigarette and manufacture
Important component in journey.
Traditional CFCs tobacco expanding method has been eliminated, and dry-ice expanding method use is the most mature, and there are many more expansibles
Technology such as steam expansion technology, microwave expansion technology.The process for expansion of tobacco used both at home and abroad mainly has: steam, dry ice, liquid nitrogen
And tobacco expanding agent KC-2A of SP series etc..Pipe tobacco bright, posture after inflating medium KC-2A expansion is full, is one
The good tobacco expanding agent of kind.The study found that expansible medium KC-2A is applied in actual production, if technique is not perfect, deposit
The problem of medium remains, since medium residual will have a direct impact on smoking property of cigarette quality, foundation is fast and accurately detected
The remaining analysis method of inflating medium is particularly important in pipe tobacco, to instruct process modification, pipe tobacco medium is remained after reducing expansion.
Currently, to residue detection of the KC-2A as pipe tobacco expansible medium is used, there is not been reported.
Summary of the invention
In view of this, the purpose of the present invention is to provide a kind of methods of remaining inflating medium in detection pipe tobacco.
The present invention provides a kind of methods of remaining inflating medium in detection pipe tobacco, comprising:
Expanded cut tobacco sample and hexamethylene are mixed, mixed liquor is obtained；
Mixed liquor is subjected to Static Headspace-gas chromatography-mass spectrography combination detection, analyzes KC-2A in expanded cut tobacco sample
Content.
In the present invention, the expanded cut tobacco sample the preparation method comprises the following steps:
Unexpanded tobacco sample is immersed in progress microwave heating expansion in inflating medium KC-2A, obtains expanded cut tobacco sample
Product.
The present invention does not have special limitation to the source of the unexpanded pipe tobacco, using it is well known to those skilled in the art not
By the pipe tobacco of expansion process, it can be bought and be obtained by market.
For the present invention by obtained mixed liquor using Static Headspace-gas chromatography-mass spectrography combination detection, specific method is first
Mixed liquor is passed through automatic head space instrument and carries out sample introduction, then by obtained headspace gas using gas chromatograph-mass spectrometer (GC-MS) into
Row detection.
The volatility of the content of each component not only with itself is related but also related with sample substrate in headspace gas, especially
The component of those solubility big (distribution coefficient is big) in sample substrate, matrix effect become apparent, i.e. the composition of headspace gas
Different from the composition in raw sample, this is particularly acute the adverse effect of quantitative analysis.Inventor is on the basis of many experiments
It finds after study, in order to accurately carry out quantitative analysis, selects quantitative analysis sample and standard solution base having the same
Matter can effectively eliminate the matrix effect of sample.
Expanded cut tobacco sample and hexamethylene, as matrix correction agent, are mixed to get mixed liquor using hexamethylene by the present invention.
Inventors discovered through research that methanol, n-hexane, ethyl acetate boiling point are respectively 64.5 DEG C, 68.7 DEG C, 77.0 DEG C, these are molten
Agent appearance time and medium KC-2A are closer to, and are influenced medium and are accurately integrated quantitatively, are not suitable as the matrix of medium KC-2A
Correction agent.The boiling point of hexamethylene is a kind of preferable hydrophilic reagent at 80.0 DEG C, KC-2A medium can be dissolved, so that sample
Product are dispersed in host solvents, to keep quantitative result more accurate, therefore select hexamethylene as matrix correction agent.
In the present invention, the concentration of expanded cut tobacco sample is preferably 0.3~0.7g/mL in the mixed liquor, more preferably
0.4~0.6g/mL, most preferably 0.5g/mL.
Inventor on the basis of many experiments after study, according to the physics and chemistry of the characteristic of head space and target compound
Matter determines that the equilibrium temperature of Static Headspace during Static Headspace-gas chromatography-mass spectrography is combined is preferably 40~80 DEG C, more
Preferably 50~70 DEG C, most preferably 55~65 DEG C, the most preferably 60 DEG C；The equilibration time of Static Headspace is preferably 10~
30min, more preferably 15~25min, most preferably 15min.
In the present invention, the testing conditions of Static Headspace during the Static Headspace-gas chromatography-mass spectrography is combined
Are as follows:
Sample loop temperature is preferably 110~130 DEG C, more preferably 115~125 DEG C, most preferably 120 DEG C；
Transmission line temperature is preferably 130~150 DEG C, more preferably 135~145 DEG C, most preferably 140 DEG C；
Moulding pressure is preferably 30~40psi, more preferably 34~36psi, most preferably 35psi；
Pressing time is preferably 1.8~2.5min, more preferably 1.8~2.2min, most preferably 2min；
Nebulizer gas pressure is preferably 35~45psi, more preferably 38~42psi, most preferably 40psi；
Inflationtime is preferably 0.15~0.25min, more preferably 0.18~0.22min, most preferably 0.2min；
Sample loop equilibration time is preferably 0.04~0.06min, more preferably 0.05min.
In the present invention, it carries out Static Headspace-gas chromatography-mass spectrography and is combined process, when carrying out gas chromatographic detection
Inventor according to analysis object physicochemical property found on the basis of many experiments, preferably select HP-PONA (50m ×
0.2mm × 0.5 μm) capillary column as chromatography column, can make object obtain preferable baseline separation.In the present invention
In, the column flow of chromatographic column is preferably 0.6~1mL/min when gas chromatographic detection, and more preferably 0.7~0.9mL/min is optimal
It is selected as 0.8mL/min.
When carrying out gas chromatographic detection, inventor studies on the basis of many experiments, to furnace temperature and program liter
Temperature optimization, can be completed entire separation process in 21.5min minutes.In the present invention, furnace temperature when gas chromatographic detection
Control is preferred are as follows:
Initial 30~50 DEG C of 3~5min of heat preservation of furnace temperature, rise to 70~90 DEG C with 2~6 DEG C/min, then with 15~25 DEG C/
Min rises to 140~160 DEG C of 4~6min of heat preservation.
More preferably:
35~45 DEG C of 3.5~4.5min of heat preservation of initial furnace temperature, rise to 75~85 DEG C with 3~5 DEG C/min, then with 18~22
DEG C/min rises to 145~155 DEG C of 4.5~5.5min of heat preservation.
Most preferably:
40 DEG C of heat preservation 4min of initial furnace temperature, rise to 80 DEG C with 4 DEG C/min, then rise to 150 DEG C of heat preservations with 20 DEG C/min
5min。
In the present invention, temperature program when gas chromatographic detection is preferred are as follows:
140~160 DEG C of initial temperature, 275~285 DEG C are risen to the heating rate of 4~8 DEG C/min, keeps 3~7min,
290~310 DEG C are risen to the heating rate of 8~12 DEG C/min again, keeps 13~17min.
More preferably:
145~155 DEG C of initial temperature, 278~282 DEG C are risen to the heating rate of 5~7 DEG C/min, keeps 4~6min,
295~305 DEG C are risen to the heating rate of 9~11 DEG C/min again, keeps 14~16min.
Most preferably:
150 DEG C of initial temperature, 280 DEG C are risen to the heating rate of 6 DEG C/min, keeps 5min, then with the liter of 10 DEG C/min
Warm speed rises to 300 DEG C, keeps 15min.
In the present invention, the testing conditions of gas-chromatography during Static Headspace-gas chromatography-mass spectrography is combined are as follows:
Injector temperature is preferably 140~160 DEG C, more preferably 145~155 DEG C, most preferably 150 DEG C；
It is preferred that constant current mode sample introduction, the split ratio during sample introduction is preferably (40~60): 1, more preferably (45~55):
1, most preferably 50:1；
It is preferred that carrier gas argon gas, more preferably high-purity argon gas, purity of argon is preferably >=99.999%.
In the present invention, during Static Headspace-gas chromatography-mass spectrography combination when Mass Spectrometer Method, inventor uses matter
Spectrum obtains the authentication information of medium KC-2A by selection ion scan, and the authentication information of KC-2A is as shown in table 1；A large amount of real
It is carried out on the basis of testing the study found that target compound can obtain when medium KC-2A selects 81 this characteristic ion of monitoring
Preferable chromatogram, as shown in Figure 3.
The authentication information of 1 medium KC-2A of table
In the present invention, mass spectrographic testing conditions during Static Headspace-gas chromatography-mass spectrography combination are as follows:
EI ionizing energy is preferably 60~80eV, more preferably 65~75eV, most preferably 70eV；
Ion source temperature is preferably 220~240 DEG C, more preferably 225~235 DEG C, most preferably 230 DEG C；
Transmission line temperature is preferably 240~260 DEG C, more preferably 245~255 DEG C, most preferably 250 DEG C；
The solvent delay time is preferably 0.1~0.3min, more preferably 0.15~0.25min, most preferably 0.2min；
Scanning mode is preferably full scan, and scanning range is preferably 29-400aeu；
Selection monitoring ion is preferably 81, more preferably 61 and 81.
Important technological problems solved by the invention are: 1) equilibration time in detection method, equilibrium temperature optimization and
The selection of matrix correction agent；2) quantified by external standard method analysis is carried out to the medium KC-2A in sample using SHS-GC/MS, determined swollen
Regression equation and related coefficient, the detection limit of detection method, quantitative limit of swollen medium KC-2A；3) recycling of detection method is measured
Rate and precision.
Inventor is by largely studying, the low boiling point based on KC-2A medium, volatile chemical characteristic and static top
It is the characteristics of sky-gas-chromatography (static headspace gas chromatography, SHS-GC) technology, real by optimization
Condition is tested, the residual of inflating medium in fast and accurately Static Headspace-Gas Chromatography-Mass Spectrometry pipe tobacco is established, is perfect
The use technology and raising smoking property of cigarette quality of expansible medium KC-2A provides technical support.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
The embodiment of invention for those of ordinary skill in the art without creative efforts, can also basis
The attached drawing of offer obtains other attached drawings.
Fig. 1 is influence of the head space equilibration time of the test of the embodiment of the present invention 1 to peak area；
Fig. 2 is influence of the head space equilibrium temperature of the test of the embodiment of the present invention 2 to peak area；
Fig. 3 is the selection chromatography of ions figure of medium KC-2A (a) and expanded cut tobacco sample (b) in the present invention.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
KC-2A used in following embodiment of the present invention is product provided by Beijing Space experimental technique research institute 101.
Unexpanded tobacco sample used is the product that Guizhou Tobacco Industry Co., Ltd's Tongren cigar mill provides.
The preparation method of expanded cut tobacco sample used are as follows:
Unexpanded tobacco sample is impregnated using inflating medium KC-2A, carries out microwave heating expansion then to get expanded cut tobacco
Sample.
The equipment that SHS-GC/MS (Static Headspace-gas chromatography-mass spectrum) detection uses is gas chromatograph-mass spectrometer (GC-MS)
With automatic head space instrument.
Embodiment 1
The expanded cut tobacco sample of 0.5g (being accurate to 0.001g) is weighed in the ml headspace bottle of 20mL, 1mL hexamethylene is added, it is fast
The tight bottle cap of ram compression is put into the head-space sampler of automatic head space instrument, obtained headspace gas is then passed through gas chromatography-mass spectrum
Combined instrument is measured.
External standard method is carried out to inflating medium KC-2A in pipe tobacco using SHS-GC/MS (Static Headspace-gas chromatography-mass spectrum)
Quantitative analysis detection, testing conditions are as follows:
Static Headspace detection:
Sample equilibration temperature: 60 DEG C；Sample loop temperature: 120 DEG C；Transmission line temperature: l40 DEG C；Sample equilibration time:
15min；Sample bottle moulding pressure: 35psi；Nebulizer gas pressure: 40psi；Pressing time: 2.0min；Inflationtime: 0.20min；Sample
Product ring equilibration time: 0.05min；Sample injection time: 0.1min.
Gas chromatographic detection:
Chromatographic column: HP-PONA capillary column (50m × 0.2mm × 0.5 μm)；Furnace temperature: initial 40 DEG C of heat preservations 4min, with 4
DEG C/min rises to 80 DEG C, 150 DEG C of heat preservation 5min are then risen to 20 DEG C/min；Injector temperature: 150 DEG C, split ratio: 50:1；
Carrier gas: high-purity helium, purity >=99.999%；Constant current mode, column flow: 0.8mL/min.
It detects temperature program: 150 DEG C of initial temperature, rising to 280 DEG C with the heating rate of 6 DEG C/min, keep 5min, then with
The heating rate of 10 DEG C/min rises to 300 DEG C, keeps 15min.
Mass Spectrometer Method:
EI ionizing energy: 70eV；Ion source temperature: 230 DEG C, transmission line temperature: 250 DEG C, solvent delay: 0.2min is swept
Retouch mode: full scan, scanning range 29-400aeu；Salbutamol Selected Ion Monitoring (SIM), monitoring ion are 61 and 81.
The residual quantity that the testing result that the method that the embodiment of the present invention 1 provides obtains is KC-2A is 5.28 μ g/g, the present invention
The method of offer is suitble to detect the residual of tobacco expanding medium KC-2.
Embodiment 2
The KC-2A medium standards solution of 70 μ g/mL is added in unpuffed pipe tobacco, equilibrium temperature is to distinguish at 60 DEG C
The measurement of 10min, 15min, 20min and 30min equilibration time is carried out, other testing conditions are the same as embodiment 1.Measurement result is as schemed
Shown in 1.As shown in Figure 1, medium KC-2A responds chromatogram peak area equilibration time 10min to 15min and slightly rises, and 15min is arrived
It is declined slightly between 20min, substantially indifference between 20min to 30min.Since medium KC-2A boiling point is lower volatile, because
This relative equilibrium time effects is smaller, to balance sample to be tested sufficiently, selects 15min equilibration time best.
Embodiment 3
The KC-2A medium standards solution of 70 μ g/mL is added in unpuffed pipe tobacco, is divided at equilibration time 15min
It is not measured under 40 DEG C, 50 DEG C, 60 DEG C and 80 DEG C of equilibrium temperature, other testing conditions are the same as embodiment 1.Testing result is such as
Shown in Fig. 2, as shown in Figure 2, with the raising of equilibrium temperature, KC-2A medium peak area is gradually increased, 40~60 DEG C of speedups slightly
It is small, and it is obvious in 60~80 DEG C of speedups, usually detect the residual quantity of inflating medium KC-2A in expanded cut tobacco under room temperature, and medium
KC-2A low boiling point, take into account sample media KC-2A abundant volatilization and improvement method sensitivity and reduce sample substrate interference
Requirement, select 60 DEG C of equilibrium temperature best.
The measurement of 4 working curve of embodiment and detection limit
The preparation of KC-2A medium standards solution:
The KC-2A medium of 10 μ L is measured in 10mL cyclohexane solvent, medium is weighed as 7.0mg, concentration 0.7mg/
mL。
KC-2A media operation curve:
The KC-2A medium standards solution of 5 μ L, 10 μ L, 20 μ L, 50 μ L, 100 μ L, 150 μ L are measured respectively in 1mL hexamethylene
Series standard solution is prepared in solvent, mass concentration is respectively 3.5 μ g/mL, 7.0 μ g/mL, 14 μ g/mL, 35 μ g/mL, 70 μ
G/mL, 105 μ g/mL, and it is separately added into the unpuffed pipe tobacco of 0.5g.
Respectively to the standard solution of this 7 various concentrations according to method described in embodiment 1 progress analysis detection, and with
KC-2A medium chromatographic peak area is ordinate and its corrresponding quality concentration X (μ g/mL) is that abscissa carries out regression analysis, must be returned
Return equation Y=1741.89X (r2=0.9999).Detection, which is calculated, with 3 times of signal-to-noise ratio (S/N >=3) is limited to 0.03 μ g/mL.
The rate of recovery and repeatability of 5 detection method of embodiment
The unexpanded pipe tobacco of 0.5g (medium KC-2A content is 0.0 μ g) is weighed, 1mL concentration is separately added into are as follows: 5.0 μ g/mL,
The standard solution containing KC-2A of 10.0 μ g/mL, 20.0 μ g/mL carry out analysis detection, each concentration as described in Example 1
Parallel test 6 times, and the rate of recovery is calculated according to measured quantity, scalar quantity and former content.
Testing result is as shown in table 2, and table 2 is the rate of recovery and again for the KC-2A that method provided in an embodiment of the present invention obtains
Renaturation.
The rate of recovery and repeatability (n=6) for the KC-2A that the method provided in an embodiment of the present invention of table 2 obtains
As shown in Table 2, detection method sample pre-treatments provided by the invention are easy to operate, quick, reproducible, accuracy
It is high.Method provided by the invention can accurately detect the residual of tobacco expanding medium KC-2, and easy, quick.
As seen from the above embodiment, the present invention provides a kind of method for detecting remaining inflating medium in pipe tobacco, comprising: will
Static Headspace-gas chromatography-mass spectrography combination detection is carried out after expanded cut tobacco sample and hexamethylene mixing, analyzes expanded cut tobacco sample
The content of KC-2A in product.The present invention is based on the low boiling point of KC-2A medium, volatile chemical characteristic and Static Headspace-gas phase colors
The characteristics of (static headspace gas chromatography, SHS-GC) technology of composing, establishes fast and accurately static
HS GC-mass spectrography measures the residual of inflating medium in pipe tobacco, for the use for improving expansible medium KC-2A
Technology and raising smoking property of cigarette quality provide technical support.
Claims (10)
1. a kind of method of remaining inflating medium in detection pipe tobacco, comprising:
Expanded cut tobacco sample and hexamethylene are mixed, mixed liquor is obtained；
Mixed liquor is subjected to Static Headspace-gas chromatography-mass spectrography combination detection, KC-2A's contains in analysis expanded cut tobacco sample
Amount.
2. the method according to claim 1, wherein the expanded cut tobacco sample the preparation method comprises the following steps:
Unexpanded tobacco sample is immersed in progress microwave heating expansion in inflating medium KC-2A, obtains expanded cut tobacco sample.
3. the method according to claim 1, wherein the concentration of expanded cut tobacco sample is 0.3 in the mixed liquor
~0.7g/mL.
4. the method according to claim 1, wherein the Static Headspace-gas chromatography-mass spectrography is combined process
The testing conditions of middle Static Headspace are as follows:
Equilibrium temperature is 40~80 DEG C；
Equilibration time is 10~30min.
5. the method according to claim 1, wherein the Static Headspace-gas chromatography-mass spectrography is combined process
The testing conditions of middle Static Headspace are as follows:
Transmission line temperature is l30~150 DEG C；
Moulding pressure is 30~40psi；
Pressing time is 1.5~2.5min.
6. the method according to claim 1, wherein the Static Headspace-gas chromatography-mass spectrography is combined process
The testing conditions of middle Static Headspace are as follows:
Nebulizer gas pressure is 35~45psi；
Inflationtime is 0.15~0.25min；
Sample injection time: 0.05~0.15min.
7. the method according to claim 1, wherein the Static Headspace-gas chromatography-mass spectrography is combined process
The testing conditions of middle gas-chromatography are as follows:
Chromatographic column is HP-PONA capillary column, and column flow is 0.6~1mL/min；
Control for Kiln Temperature are as follows: be warming up to 70~90 DEG C after 3~5min of initial 35~45 DEG C of heat preservations with 3~5 DEG C/min, then with 15~
25 DEG C/min is warming up to 140~160 DEG C of 4~6min of heat preservation；
Injector temperature is 140~160 DEG C.
8. the method according to claim 1, wherein the Static Headspace-gas chromatography-mass spectrography is combined process
The temperature program of middle gas chromatographic detection are as follows:
140~160 DEG C of initial temperature, 275~285 DEG C are risen to the heating rate of 5~7 DEG C/min, keeps the temperature 4~6min, then with 8
The heating rate of~12 DEG C/min rises to 295~305 DEG C, keeps the temperature 14~16min.
9. the method according to claim 1, wherein the Static Headspace-gas chromatography-mass spectrography is combined process
In mass spectrographic testing conditions are as follows:
EI ionizing energy is 65~75eV；
Ion source temperature is 220~240 DEG C,
Transmission line temperature is 240~260 DEG C.
10. the method according to claim 1, wherein the Static Headspace-gas chromatography-mass spectrography was combined
Mass spectrographic testing conditions in journey are as follows:
The solvent delay time is 0.1~0.3min；
Scanning mode is full scan, and scanning range is 29~400aeu；
Selecting monitoring ion is 61 and 81.
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| CN114113391A (en) * | 2021-11-24 | 2022-03-01 | 贵州中烟工业有限责任公司 | Method for detecting content of expansion medium |
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| CN114113391B (en) * | 2021-11-24 | 2024-03-26 | 贵州中烟工业有限责任公司 | Method for detecting content of expansion medium |
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