CN109738548A - A kind of heating does not burn in cigarette peppermint Alkanol isomer by mouth rate of transform measuring method - Google Patents
A kind of heating does not burn in cigarette peppermint Alkanol isomer by mouth rate of transform measuring method Download PDFInfo
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Abstract
The present invention relates to a kind of heating not to burn in cigarette peppermint Alkanol isomer by mouth rate of transform measuring method, includes the following steps: that sample extraction, heating are not burnt the suction and flue gas trapping, the extraction of cambridge filter, the processing of trapping solution, the calculating of menthol isomer separation and measurement and the rate of transform of cigarette.The present invention, which can not only be precisely separating and measure, heats peppermint Alkanol isomer in the cigarette that do not burn, the isomers of menthol is separated and is able to highly sensitive detection, to realize detection of the peppermint Alkanol isomer to flue gas gas gas-phase objects and granule phase substance by the mouth rate of transform, measurement is accurate and reliable, whole operation is simple and efficient, has application value.
Description
Technical field
The present invention relates to a kind of peppermint Alkanol isomers by mouth rate of transform measuring method, specifically a kind of to heat the cigarette that do not burn
Middle peppermint Alkanol isomer belongs to analytical chemistry field by mouth rate of transform measuring method.
Background technique
It heats the cigarette (heat not burn) that do not burn and contains Alevaire ingredient tobacco and tobacco system using external heat
Product generate flue gas under non-burning state, suck for consumer, and wherein mint type taste is a weight for heating the cigarette that do not burn
Want classification.The refrigerant feature of uniqueness of mint type wiredrawn edge taste is mainly derived from menthol, thin in cigarette in cigarette heating process
Lotus alcohol can be shifted into main flume, and the size and release stability of cool taste feature are determined by the height of the mouth rate of transform.
Menthol has 8 stereoisomers, respectively l-menthol, D- menthol, L- neomenthol, D- neomenthol,
L- isomenthol, D- isomenthol, L- neoisomenthol and D- neoisomenthol, they are in that fragrance matter is different, and L- is thin
Lotus alcohol has the function of peppermint fragrance and has refrigerant, is effect ingredient that the heating of mint type taste is not burnt in cigarette.It is other
Isomers is without refrigerant effect or even irritating effect.The menthol added in the cigarette that do not burn is heated other than l-menthol, also
There may be other isomer compositions, these isomers can also shift to flue gas and bring negative effect to flue gas.Measurement heating
Different peppermint Alkanol isomers are not burnt in cigarette to the rate of transform of flue gas, and menthol can be instructed not burn in cigarette-opening hair in heating
Application.But it only reported transfer of the l-menthol to flue gas at present, the method for having no measures other peppermint Alkanol isomers to flue gas
Transfer.
Against the above deficiency, a kind of peppermint Alkanol isomer that accurately and reliably heats in the cigarette that do not burn is developed by the mouth rate of transform
Measuring method it is very necessary.
Summary of the invention
In order to solve the above technical problem, the present invention provides a kind of heating peppermint Alkanol isomers that do not burn in cigarette to turn by mouth
Shifting rate measuring method, this method, which can not only be precisely separating and measure, heats peppermint Alkanol isomer in the cigarette that do not burn, additionally it is possible to
Quickly analysis heating does not burn in cigarette peppermint Alkanol isomer by the mouth rate of transform.The technical solution adopted by the present invention is specific as follows:
A kind of heating does not burn in cigarette peppermint Alkanol isomer by mouth rate of transform measuring method, comprising the following steps:
Step (1), sample extraction:
The position that menthol is added in the cigarette sample that do not burn will be heated as sample, precise certain mass sample is in taper
In bottle, the extractant of containing the internal standard solution is added, is extracted after capping on vortex oscillation instrument, wherein the use of extractant
Amount and the ratio of sample quality are 20:1 ~ 200:1, and mL:g, inner mark solution concentration is 10 ~ 1000 mg/L；
Step (2), the suction for heating the cigarette that do not burn and flue gas trapping:
It separately takes the heating of a certain amount of addition menthol not burn cigarette, aspirates the heating using smoking machine and do not burn cigarette, lead to
Cambridge filter trapping is crossed by mouth Smoke Particulate, is trapped by trapping solvent by mouth flue gas gas gas-phase objects, wherein trapping solution volume
For 10 ~ 30mL；
The extraction of step (3), cambridge filter:
Cambridge filter after trapping is placed in conical flask, the extractant of containing the internal standard solution is added, is shaken after capping in being vortexed
It swings and is extracted on instrument, wherein the dosage of extractant is 15 ~ 50mL, and inner mark solution concentration is 10 ~ 500 mg/L；
The processing of step (4), trapping solution:
The trapping solution of step (2) is transferred in volumetric flask, internal standard is added, inner mark solution concentration is 10 ~ 500 mg/L after constant volume；
Step (5), menthol isomer separation and measurement:
Respectively by step (1), the trapping solution sample introduction of the extract liquor of (3) and step (4), is separated, passed through by gas-chromatography
Mass spectrography detects isolated peppermint Alkanol isomer, inner mark method ration, calculates separately heating not according to standard curve calculating
Burn cigarette in each menthol content of isomer, by menthol Isomers content in mouth granule phase substance and by each thin in mouth gas gas-phase objects
Lotus Alkanol isomer content, wherein the chromatographic column of gas-chromatography is two chiral elastic capillary-column series connection, and the first root chromatogram column is logical
Capillary column connection special joint is crossed to be connected with the second root chromatogram column；
The calculating of step (6), the rate of transform:
By menthol Isomers content in mouth granule phase substance divided by heating do not burn in cigarette each menthol content of isomer to get
To each peppermint Alkanol isomer to the rate of transform of Smoke Particulate；By menthol content of isomer each in mouth gas gas-phase objects divided by heating not
Burn cigarette in each menthol content of isomer to get arrive the rate of transform of each peppermint Alkanol isomer to Smoke Particulate.
Further, in step (1), the weighing quality of sample is 0.1 ~ 0.5g.
Further, in step (1) and (3), extractant is methanol, ethyl alcohol, isopropanol or normal propyl alcohol.
Further, in step (1) and (3), the revolving speed of vortex oscillation is 500 ~ 2000 rpm, and the time of vortex oscillation is
5~20min。
Further, in step (2), the trapping solution of flue gas gas gas-phase objects is methanol or ethyl alcohol.
Further, in step (2), the suction method of smoking machine is cigarette suction after preheating equipped with the smoking set of cigarette
First suction channel of end insertion, aspirates the 1st mouthful of flue gas using the 1st channel, the 2nd duct is moved to after suction, use
The 2nd mouthful of flue gas is aspirated in 2nd channel, and so on every cigarette altogether aspirate 8 ~ 12 mouthfuls, 2 ~ 20 heating of continuous sucking are non-ignitable
Burn cigarette.
Further, in step (5), GC conditions are as follows:
Injector temperature: 200 DEG C；Carrier gas: helium, column flow: constant current 1.5mL/min；Sample volume: 1 μ L；Split sampling shunts
Than 5:1 ~ 50:1；Temperature program: 100 DEG C of initial temperature, 120 DEG C then are warming up to the rate of 5 DEG C/min, and keep 20
Min is finally warming up to 200 DEG C with the rate of 10 DEG C/min, keeps 5min；
Mass Spectrometry Conditions are as follows:
Electron bombardment ionization source EI；Transmission line temperature: 200 DEG C；Ion source temperature: 180 DEG C；Ionizing energy: 70 eV；Solvent delay:
15 min；Scan pattern is Salbutamol Selected Ion Monitoring mode, and qualitative, the quota ion of 8 menthols are 71/81/95, acetic acid benzene
Ethyl ester is qualitative, quota ion is 43/91/104.
Further, in step (5), the first root chromatogram column stationary phase is 20% tert-butyl chloro-silicane-β-ring paste
Essence is dissolved in BGB-15, and specification is 0.25 mm id of length 30m × internal diameter × 0.25 μm of film thickness df.
Further, in step (5), the second root chromatogram column stationary phase is 30% 7-(2, the 3- bis- tertiary fourths of-O- methyl-6-O-
Base dimethyl silicon substrate)-beta-cyclodextrin is dissolved in DB-1701, and specification is 30 m of length × internal diameter, 0.25 mm id × film thickness 0.25
μm df.The phenyl that BGB-15 is 15% replaces and 85% methyl substituted polysiloxanes.
Further, in step (5), Specification Curve of Increasing method is as follows: preparing 8 peppermint Alkanol isomers with extractant
Mixed standard solution, concentration range are as follows: 0.5mg/L ~ 2000mg/L, series standard solution be added internal standard compound, internal standard compound concentration
It is identical as internal standard concentration in sample extraction liquid, gas chromatograph-mass spectrometer (GC-MS) analysis is carried out to series standard solution, according to each object
The ratio of matter quota ion peak area and internal standard compound quota ion peak area is ordinate, with each material concentration and internal standard compound concentration
Ratio is abscissa, makees the standard curve of each measurement substance.
Compared with prior art, the present invention having the beneficial effect that
(1) present invention can be achieved heating and not burn the trapping by mouth of menthol in cigarette smoke granule phase substance and gas gas-phase objects.
(2) by the tandem compound of two chiral chromatographic columns, it can be achieved that 8 peppermint Alkanol isomers are kept completely separate, thus real
Now heat the detection respectively of 8 peppermint Alkanol isomers in the cigarette that do not burn, Smoke Particulate and flue gas gas gas-phase objects；
(3) method detection sensitivity is high, and precision is good, accurately and reliably.
Generally speaking, 8 isomers of menthol can be separated and be obtained by chiral column serial connection technology by this method
With highly sensitive detection, to realize detection of 8 peppermint Alkanol isomers to flue gas gas gas-phase objects and granule phase substance by the mouth rate of transform, measurement
Accurately and reliably, whole operation is simple and efficient, has application value.
Detailed description of the invention
General introduction described above for technical solution of the present invention, in order to better understand technological means of the invention, and can
It is implemented in accordance with the contents of the specification, and in order to make above and other objects of the present invention, feature and advantage brighter
Show understandable, existing special act preferred embodiment, and cooperate attached drawing, detailed description are as follows.
Fig. 1 is the gas chromatography-mass spectrum figure of 8 kinds of peppermint Alkanol isomer standard solution measurement；
Fig. 2 is that the gas chromatography-mass spectrum figure that peppermint Alkanol isomer measures in the cigarette that do not burn is heated in embodiment 1；
Fig. 3 is that the gas chromatography-mass spectrum that peppermint Alkanol isomer measures in the cigarette smoke granule phase substance that do not burn is heated in embodiment 1
Figure；
Fig. 4 is that the gas chromatography-mass spectrum that peppermint Alkanol isomer measures in the components in cigarette smoke gas phase object that do not burn is heated in embodiment 1
Figure.
Specific embodiment
Below with reference to embodiment, the present invention is described in further detail, but it is not intended to limit the present invention.
It will be understood to those of skill in the art that the following example is merely to illustrate the present invention, and it should not be regarded as limiting this hair
Bright range.In the examples where no specific technique or condition is specified, described technology or conditions according to the literature in the art
Or it is carried out according to product description.Reagents or instruments used without specified manufacturer is that can be obtained by purchase
Conventional products.
Embodiment 1
The heating of the present embodiment does not burn in cigarette core substrate peppermint Alkanol isomer by mouth rate of transform measuring method, including following step
It is rapid:
The heating of the present embodiment does not burn cigarette sample to be added to 8 kinds of peppermint Alkanol isomers in core substrate, and additive amount is
2mg/g。
Step (1), sample extraction:
The core substrate for adding menthol in the cigarette that do not burn will be heated to remove, shred and be uniformly mixed, 0.1 g core base of precise
Methanol solution of the 20mL containing the phenethyl acetate that concentration is 100mg/L is added in conical flask in material, and capping is placed on vortex oscillation
Be vortexed under 500 rpm revolving speeds 10min on instrument.
Step (2), the suction for heating the cigarette that do not burn and flue gas trapping:
Separately the heating for being added to 8 kinds of peppermint Alkanol isomers in 2 core branch substrates is taken not burn cigarette.
The cigarette that do not burn is heated using the suction of linear type multi-pore channel smoking machine, selects Canadian depth suction mode, suction
Method are as follows:
After the smoking set preheating equipped with cigarette, cigarette aspiration end is inserted into first suction channel, using the 1st channel suction the 1st
Mouthful flue gas, moves to the 2nd duct, aspirates the 2nd mouthful of flue gas using the 2nd channel after suction, and so on every cigarette one
8 mouthfuls are aspirated altogether, and continuous sucking above-mentioned 2 are heated the cigarette that do not burn, and are trapped by cambridge filter by mouth Smoke Particulate, are being trapped
The trapping of 20 mL methanol is added in device by mouth flue gas gas gas-phase objects.
The extraction of step (3), cambridge filter:
Cambridge filter after trapping is placed in conical flask, 30 mL are added containing the phenethyl acetate that concentration is 100 mg/L
Methanol solution, capping are placed on vortex oscillation instrument under 500 rpm revolving speeds 5 min that are vortexed.
The processing of step (4), trapping solution:
The trapping solution of step (2) is transferred in volumetric flask, phenethyl acetate internal standard is added, phenethyl acetate concentration is after constant volume
500 mg/L；
Step (5), menthol isomer separation and measurement:
Respectively by step (1), the trapping solution sample introduction of the extract liquor of (3) and step (4), is separated, passed through by gas-chromatography
Mass spectrography detects isolated peppermint Alkanol isomer, inner mark method ration, calculates separately heating not according to standard curve calculating
Burn cigarette in each menthol content of isomer, by menthol Isomers content in mouth granule phase substance and by each thin in mouth gas gas-phase objects
Lotus Alkanol isomer content.
Wherein, GC conditions are as follows:
Chromatographic column is two chiral elastic capillary-columns series connection, and the first root chromatogram column passes through capillary column connection special joint and the
Two root chromatogram columns are connected.
First root chromatogram column stationary phase is that 20% tert-butyl chloro-silicane-beta-cyclodextrin is dissolved in BGB-15(15%
Phenyl, 85% methyl polysiloxane), specification is 0.25 mm id of length 30m × internal diameter × 0.25 μm of film thickness df.
Second root chromatogram column stationary phase is 30% 7-(bis--O- methyl-6-O- t-Butyldimethylsilyl of 2,3-)-β-ring
Dextrin is dissolved in DB-1701((14%- cyanogen propyl-phenyl) methyl polysiloxane), specification is length 30m × internal diameter 0.25
Mm id × 0.25 μm of film thickness df.
Injector temperature: 200 DEG C；Carrier gas: helium (purity >=99.999 %), column flow: constant current 1.5mL/min；Sample introduction
Amount: 1 μ L；Split sampling, split ratio 5:1；Temperature program: it 100 DEG C of initial temperature, is then warming up to the rate of 5 DEG C/min
120 DEG C, and 20 min are kept, 200 DEG C finally are warming up to the rate of 10 DEG C/min, keeps 5min.
Mass Spectrometry Conditions are as follows:
Electron bombardment ionization source (EI)；Transmission line temperature: 200 DEG C；Ion source temperature: 180 DEG C；Ionizing energy: 70 eV；Solvent prolongs
It is slow: 15 min；Scan pattern is Salbutamol Selected Ion Monitoring mode, and qualitative, the quota ion of 8 menthols are 71/81/95, second
Sour phenethyl ester is qualitative, quota ion is 43/91/104.
Specification Curve of Increasing method is as follows: the mixed standard solution of 8 peppermint Alkanol isomers, concentration are prepared with extractant
Range are as follows: internal standard compound, internal standard in internal standard compound concentration and sample extraction liquid is added in the mg/L of 0.5mg/L ~ 2000, series standard solution
Concentration is identical, to series standard solution carry out gas chromatograph-mass spectrometer (GC-MS) analysis, according to each substance quota ion peak area with
The ratio of internal standard compound quota ion peak area is ordinate, using each material concentration and internal standard compound concentration proportion as abscissa, is made each
Measure the standard curve of substance.
Fig. 1 is the gas chromatography-mass spectrum figure of 8 kinds of peppermint Alkanol isomer standard solution measurement, and 9 peaks from left to right divide in figure
Not Wei D- neomenthol, L- neomenthol, L- neoisomenthol, D- menthol, l-menthol, L- isomenthol, D- it is strange thin
Lotus alcohol, D- isomenthol, phenethyl acetate, 8 menthol isomer separations are all right.
It heats in the cigarette core substrate that do not burn, heat in the cigarette smoke granule phase substance that do not burn and heat the cigarette smoke that do not burn
The gas chromatography-mass spectrum figure that peppermint Alkanol isomer measures in gas gas-phase objects is shown in Fig. 2, Fig. 3 and Fig. 4 respectively.
The calculating of step (6), the rate of transform:
The content of each peppermint Alkanol isomer in core substrate is obtained according to standard curve, is contained by menthol Isomers in mouth granule phase substance
It measures, by menthol Isomers content in mouth gas gas-phase objects, further calculates to obtain and heat each peppermint in the cigarette core substrate that do not burn
Alkanol isomer into Smoke Particulate and flue gas gas gas-phase objects by the mouth rate of transform.
It does not burn each menthol content of isomer in cigarette by menthol Isomers content in mouth granule phase substance divided by heating,
Obtain the rate of transform of each peppermint Alkanol isomer to Smoke Particulate；By menthol content of isomer each in mouth gas gas-phase objects divided by adding
Heat does not burn in cigarette each menthol content of isomer to get to the rate of transform of each peppermint Alkanol isomer to Smoke Particulate.
As a result it is listed in the table below respectively in 1 and table 2.
Table 1 heat do not burn peppermint Alkanol isomer in cigarette core substrate into Smoke Particulate by the mouth rate of transform
Table 2 heat do not burn peppermint Alkanol isomer in cigarette core substrate into flue gas gas gas-phase objects by the mouth rate of transform
Table 3 is the method evaluation using 8 kinds of peppermint Alkanol isomers in this method measurement cigarette, Smoke Particulate, flue gas gas gas-phase objects
Data give the precision (RSD), detection limit and the rate of recovery of this experimental method, show this method high sensitivity, precision and
Accuracy is good.
3 linearly dependent coefficient of table, precision (RSD), detection limit and the rate of recovery
Embodiment 2
The heating of the present embodiment does not burn in cigarette cigarette paper peppermint Alkanol isomer by mouth rate of transform measuring method, including following step
It is rapid:
The heating of the present embodiment cigarette sample that do not burn is to be added to 4 kinds of peppermint Alkanol isomers in cigarette paper, the wherein new peppermint of D-
Alcohol, L- neomenthol, D- menthol, l-menthol additive amount are respectively 0.3mg/g, 0.4mg/g, 0.3mg/g, 8.1mg/g.
Step (1), sample extraction:
The cigarette paper for adding menthol in the cigarette that do not burn will be heated to remove, shred and be uniformly mixed, precise 0.5g core base
Ethanol solution of 10 mL containing the phenethyl acetate that concentration is 1000 mg/L is added in conical flask in material, and capping is placed on vortex
Be vortexed under 1000 rpm revolving speeds 5min on shaker.
Step (2), the suction for heating the cigarette that do not burn and flue gas trapping:
The heating for adding 4 kinds of peppermint Alkanol isomers in 5 cigarette paper is separately taken not burn cigarette.
The cigarette that do not burn is heated using the suction of linear type multi-pore channel smoking machine, selects ISO suction mode, suction method are as follows:
After the smoking set preheating equipped with cigarette, cigarette aspiration end is inserted into first suction channel, using the 1st channel suction the 1st
Mouthful flue gas, moves to the 2nd duct, aspirates the 2nd mouthful of flue gas using the 2nd channel after suction, and so on every cigarette one
10 mouthfuls are aspirated altogether, and continuous sucking 5 are heated the cigarette that do not burn, and are trapped by cambridge filter by mouth Smoke Particulate, are passed through trapping
The trapping of 10 mL ethyl alcohol is added in device by mouth flue gas gas gas-phase objects.
The extraction of step (3), cambridge filter:
The cambridge filter of trapping is placed in conical flask, and it is molten that ethyl alcohol of the 15mL containing the phenethyl acetate that concentration is 500 mg/L is added
Liquid, capping are placed on vortex oscillation instrument under 1000 rpm revolving speeds the 10min that is vortexed.
The processing of step (4), trapping solution:
The trapping solution of step (2) is transferred in volumetric flask, phenethyl acetate internal standard is added, phenethyl acetate concentration is after constant volume
10 mg/L；
Step (5), menthol isomer separation and measurement:
Respectively by step (1), the trapping solution sample introduction of the extract liquor of (3) and step (4), is separated, passed through by gas-chromatography
Mass spectrography detects isolated peppermint Alkanol isomer, inner mark method ration, calculates separately heating not according to standard curve calculating
Burn cigarette in each menthol content of isomer, by menthol Isomers content in mouth granule phase substance and by each thin in mouth gas gas-phase objects
Lotus Alkanol isomer content.
GC conditions are as follows:
Chromatographic column is two chiral elastic capillary-columns series connection, and the first root chromatogram column passes through capillary column connection special joint and the
Two root chromatogram columns are connected.
First root chromatogram column stationary phase is that 20% tert-butyl chloro-silicane-beta-cyclodextrin is dissolved in BGB-15(15%
Phenyl, 85% methyl polysiloxane), specification is 0.25 mm id of length 30m × internal diameter × 0.25 μm of film thickness df.
Second root chromatogram column stationary phase is 30% 7-(bis--O- methyl-6-O- t-Butyldimethylsilyl of 2,3-)-β-ring
Dextrin is dissolved in DB-1701((14%- cyanogen propyl-phenyl) methyl polysiloxane), specification is length 30m × internal diameter 0.25
Mm id × 0.25 μm of film thickness df.
Injector temperature: 200 DEG C；Carrier gas: helium (purity >=99.999 %), column flow: constant current 1.5mL/min；Sample introduction
Amount: 1 μ L；Split sampling, split ratio 20:1；Temperature program: it 100 DEG C of initial temperature, is then warming up to the rate of 5 DEG C/min
120 DEG C, and 20 min are kept, 200 DEG C finally are warming up to the rate of 10 DEG C/min, keeps 5min.
Mass Spectrometry Conditions are as follows:
Electron bombardment ionization source (EI)；Transmission line temperature: 200 DEG C；Ion source temperature: 180 DEG C；Ionizing energy: 70 eV；Solvent prolongs
It is slow: 15 min；Scan pattern is Salbutamol Selected Ion Monitoring mode, and qualitative, the quota ion of 8 menthols are 71/81/95, second
Sour phenethyl ester is qualitative, quota ion is 43/91/104.
The calculating of step (6), the rate of transform:
The content of each peppermint Alkanol isomer in cigarette paper is obtained according to standard curve, is contained by menthol Isomers in mouth granule phase substance
It measures, by menthol Isomers content in mouth gas gas-phase objects, further calculates to obtain and heat each peppermint in the cigarette cigarette paper that do not burn
Alkanol isomer into Smoke Particulate and flue gas gas gas-phase objects by the mouth rate of transform, be as a result listed in the table below respectively in 4 and table 5, the party
Method is easy to operate, accurately and reliably.
Table 4 heat do not burn peppermint Alkanol isomer in cigarette cigarette paper into Smoke Particulate by the mouth rate of transform
Table 5 heat do not burn peppermint Alkanol isomer in cigarette cigarette paper into flue gas gas gas-phase objects by the mouth rate of transform
Remaining is same as Example 1.
Embodiment 3
The heating of the present embodiment does not burn in cigarette filter tow peppermint Alkanol isomer by mouth rate of transform measuring method, including following
Step:
The heating of the present embodiment does not burn cigarette to add 4 kinds of peppermint Alkanol isomers in filter tow, and wherein D- menthol, L- are thin
Lotus alcohol, L- isomenthol, D- isomenthol additive amount are respectively 0.8mg/g, 12.6mg/g, 0.9mg/g, 0.4mg/g.
Step (1), sample extraction:
The filter tow for adding menthol in the cigarette that do not burn will be heated to remove, shred and be uniformly mixed, precise 0.2g core
Normal propyl alcohol solution of 10 mL containing the phenethyl acetate that concentration is 10 mg/L is added in conical flask in substrate, and capping is placed on whirlpool
Be vortexed under 2000 rpm revolving speeds 20min on rotation shaker.
Step (2), the suction for heating the cigarette that do not burn and flue gas trapping:
The heating for adding 4 kinds of peppermint Alkanol isomers in 20 filter tows is separately taken not burn cigarette.
The cigarette that do not burn is heated using the suction of linear type multi-pore channel smoking machine, selects Canadian depth suction mode, suction
Method are as follows:
After the smoking set preheating equipped with cigarette, cigarette aspiration end is inserted into first suction channel, using the 1st channel suction the 1st
Mouthful flue gas, moves to the 2nd duct, aspirates the 2nd mouthful of flue gas using the 2nd channel after suction, and so on every cigarette one
12 mouthfuls are aspirated altogether, and continuous sucking 20 are heated the cigarette that do not burn, and are trapped by cambridge filter by mouth Smoke Particulate, are passed through trapping
The trapping of 30mL methanol is added in device by mouth flue gas gas gas-phase objects.
The extraction of step (3), cambridge filter:
The cambridge filter of trapping is placed in conical flask, and normal propyl alcohol of the 50mL containing the phenethyl acetate that concentration is 10 mg/L is added
Solution, capping are placed on vortex oscillation instrument under 2000 rpm revolving speeds 20 min that are vortexed.
The processing of step (4), trapping solution:
The trapping solution of step (2) is transferred in volumetric flask, phenethyl acetate internal standard is added, phenethyl acetate concentration is after constant volume
100mg/L。
Step (5), menthol isomer separation and measurement:
Respectively by step (1), the trapping solution sample introduction of the extract liquor of (3) and step (4), is separated, passed through by gas-chromatography
Mass spectrography detects isolated peppermint Alkanol isomer, inner mark method ration, calculates separately heating not according to standard curve calculating
Burn cigarette in each menthol content of isomer, by menthol Isomers content in mouth granule phase substance and by each thin in mouth gas gas-phase objects
Lotus Alkanol isomer content.
Wherein, GC conditions are as follows:
Chromatographic column is two chiral elastic capillary-columns series connection, and the first root chromatogram column passes through capillary column connection special joint and the
Two root chromatogram columns are connected.
First root chromatogram column stationary phase is that 20% tert-butyl chloro-silicane-beta-cyclodextrin is dissolved in BGB-15(15%
Phenyl, 85% methyl polysiloxane), specification is 0.25 mm id of length 30m × internal diameter × 0.25 μm of film thickness df.
Second root chromatogram column stationary phase is 30% 7-(bis--O- methyl-6-O- t-Butyldimethylsilyl of 2,3-)-β-ring
Dextrin is dissolved in DB-1701((14%- cyanogen propvl-phenvl) methyl polysiloxane), specification is length 30m × 0.25 mm of internal diameter
0.25 μm of df of id × film thickness.
Injector temperature: 200 DEG C；Carrier gas: helium (purity >=99.999 %), column flow: constant current 1.5mL/min；Sample introduction
Amount: 1 μ L；Split sampling, split ratio 50:1；Temperature program: it 100 DEG C of initial temperature, is then warming up to the rate of 5 DEG C/min
120 DEG C, and 20 min are kept, 200 DEG C finally are warming up to the rate of 10 DEG C/min, keeps 5min.
Mass Spectrometry Conditions are as follows:
Electron bombardment ionization source (EI)；Transmission line temperature: 200 DEG C；Ion source temperature: 180 DEG C；Ionizing energy: 70 eV；Solvent prolongs
It is slow: 15 min；Scan pattern is Salbutamol Selected Ion Monitoring mode, and qualitative, the quota ion of 8 menthols are 71/81/95, second
Sour phenethyl ester is qualitative, quota ion is 43/91/104.
The calculating of step (6), the rate of transform:
The content of each peppermint Alkanol isomer in filter tow is obtained, by menthol Isomers in mouth granule phase substance according to standard curve
Content, by menthol Isomers content in mouth gas gas-phase objects, further calculate to obtain and heat in the cigarette core filter tow that do not burn
Each peppermint Alkanol isomer into Smoke Particulate and flue gas gas gas-phase objects by the mouth rate of transform, be as a result listed in the table below 6 and table 7 respectively
In, this method is easy to operate, and accuracy is high.
Table 6 heat do not burn peppermint Alkanol isomer in cigarette filter tow into Smoke Particulate by the mouth rate of transform
Table 7 heat do not burn peppermint Alkanol isomer in cigarette filter tow into flue gas gas gas-phase objects by the mouth rate of transform
Remaining is same as Example 1.
The basic principles, main features and advantages of the present invention have been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (10)
1. a kind of heating is not burnt in cigarette, peppermint Alkanol isomer is by mouth rate of transform measuring method, it is characterised in that including following step
It is rapid:
Step (1), sample extraction:
The position that menthol is added in the cigarette sample that do not burn will be heated as sample, precise certain mass sample is in taper
In bottle, the extractant of containing the internal standard solution is added, is extracted after capping on vortex oscillation instrument, wherein the use of extractant
Amount and the ratio of sample quality are 20:1 ~ 200:1, and mL:g, inner mark solution concentration is 10 ~ 1000 mg/L；
Step (2), the suction for heating the cigarette that do not burn and flue gas trapping:
It separately takes the heating of a certain amount of addition menthol not burn cigarette, aspirates the heating using smoking machine and do not burn cigarette, lead to
Cambridge filter trapping is crossed by mouth Smoke Particulate, is trapped by trapping solvent by mouth flue gas gas gas-phase objects, wherein trapping solution volume
For 10 ~ 30mL；
The extraction of step (3), cambridge filter:
Cambridge filter after trapping is placed in conical flask, the extractant of containing the internal standard solution is added, is shaken after capping in being vortexed
It swings and is extracted on instrument, wherein the dosage of extractant is 15 ~ 50mL, and inner mark solution concentration is 10 ~ 500 mg/L；
The processing of step (4), trapping solution:
The trapping solution of step (2) is transferred in volumetric flask, internal standard is added, inner mark solution concentration is 10 ~ 500 mg/L after constant volume；
Step (5), menthol isomer separation and measurement:
Respectively by step (1), the trapping solution sample introduction of the extract liquor of (3) and step (4), is separated, passed through by gas-chromatography
Mass spectrography detects isolated peppermint Alkanol isomer, inner mark method ration, calculates separately heating not according to standard curve calculating
Burn cigarette in each menthol content of isomer, by menthol Isomers content in mouth granule phase substance and by each thin in mouth gas gas-phase objects
Lotus Alkanol isomer content, wherein the chromatographic column of gas-chromatography is two chiral elastic capillary-column series connection, and the first root chromatogram column is logical
Capillary column connection special joint is crossed to be connected with the second root chromatogram column；
The calculating of step (6), the rate of transform:
By menthol Isomers content in mouth granule phase substance divided by heating do not burn in cigarette each menthol content of isomer to get
To each peppermint Alkanol isomer to the rate of transform of Smoke Particulate；By menthol content of isomer each in mouth gas gas-phase objects divided by heating not
Burn cigarette in each menthol content of isomer to get arrive the rate of transform of each peppermint Alkanol isomer to Smoke Particulate.
2. heating according to claim 1 is not burnt, peppermint Alkanol isomer is special by mouth rate of transform measuring method in cigarette
Sign is: in step (1), the weighing quality of sample is 0.1 ~ 0.5g.
3. heating according to claim 1 is not burnt, peppermint Alkanol isomer is special by mouth rate of transform measuring method in cigarette
Sign is: in step (1) and (3), extractant is methanol, ethyl alcohol, isopropanol or normal propyl alcohol.
4. heating according to claim 1 is not burnt, peppermint Alkanol isomer is special by mouth rate of transform measuring method in cigarette
Sign is: in step (1) and (3), the revolving speed of vortex oscillation is 500 ~ 2000 rpm, and the time of vortex oscillation is 5 ~ 20min.
5. heating according to claim 1 is not burnt, peppermint Alkanol isomer is special by mouth rate of transform measuring method in cigarette
Sign is: in step (2), the trapping solution of flue gas gas gas-phase objects is methanol or ethyl alcohol.
6. heating according to claim 1 is not burnt, peppermint Alkanol isomer is special by mouth rate of transform measuring method in cigarette
Sign is: in step (2), the suction method of smoking machine is cigarette aspiration end insertion first after preheating equipped with the smoking set of cigarette
A suction channel aspirates the 1st mouthful of flue gas using the 1st channel, the 2nd duct is moved to after suction, is taken out using the 2nd channel
Inhale the 2nd mouthful of flue gas, and so on every cigarette aspirate 8 ~ 12 mouthfuls altogether, continuous sucking 2 ~ 20 heating are not burnt cigarette.
7. heating according to claim 1 is not burnt, peppermint Alkanol isomer is special by mouth rate of transform measuring method in cigarette
Sign is: in step (5), GC conditions are as follows:
Injector temperature: 200 DEG C；Carrier gas: helium, column flow: constant current 1.5mL/min；Sample volume: 1 μ L；Split sampling shunts
Than 5:1 ~ 50:1；Temperature program: 100 DEG C of initial temperature, 120 DEG C then are warming up to the rate of 5 DEG C/min, and keep 20
Min is finally warming up to 200 DEG C with the rate of 10 DEG C/min, keeps 5min；
Mass Spectrometry Conditions are as follows:
Electron bombardment ionization source EI；Transmission line temperature: 200 DEG C；Ion source temperature: 180 DEG C；Ionizing energy: 70 eV；Solvent delay:
15 min；Scan pattern is Salbutamol Selected Ion Monitoring mode, and qualitative, the quota ion of 8 menthols are 71/81/95, acetic acid benzene
Ethyl ester is qualitative, quota ion is 43/91/104.
8. heating according to claim 1 is not burnt, peppermint Alkanol isomer is special by mouth rate of transform measuring method in cigarette
Sign is: in step (5), the first root chromatogram column stationary phase is that 20% tert-butyl chloro-silicane-beta-cyclodextrin is dissolved in
BGB-15, specification are 0.25 mm id of length 30m × internal diameter × 0.25 μm of film thickness df.
9. heating according to claim 1 is not burnt, peppermint Alkanol isomer is special by mouth rate of transform measuring method in cigarette
Sign is: in step (5), the second root chromatogram column stationary phase is 30% 7-(2,3- bis--O- methyl-6-O- tert-butyldimethyl silyls
Base)-beta-cyclodextrin is dissolved in DB-1701, and specification is 30 m of length × internal diameter, 0.25 mm id × 0.25 μm of film thickness df.
10. heating according to claim 1 is not burnt, peppermint Alkanol isomer is special by mouth rate of transform measuring method in cigarette
Sign is: in step (5), Specification Curve of Increasing method is as follows: the hybrid standard of 8 peppermint Alkanol isomers is prepared with extractant
Solution, concentration range are as follows: internal standard compound, internal standard compound concentration and sample extraction is added in 0.5mg/L ~ 2000mg/L, series standard solution
Internal standard concentration is identical in liquid, gas chromatograph-mass spectrometer (GC-MS) analysis is carried out to series standard solution, according to each substance quota ion
The ratio of peak area and internal standard compound quota ion peak area is ordinate, with each material concentration and internal standard compound concentration proportion for horizontal seat
Mark makees the standard curve of each measurement substance.
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| CN112798716A (en) * | 2021-02-08 | 2021-05-14 | 国家烟草质量监督检验中心 | Method for measuring migration rates of growth regulator and pyrethroid pesticide in cigarette without burning by heating |
| CN113671063A (en) * | 2021-07-12 | 2021-11-19 | 河南中烟工业有限责任公司 | Method for measuring ester transfer rate in heated cigarette |
| CN115097054A (en) * | 2022-06-22 | 2022-09-23 | 云南中烟工业有限责任公司 | Method for simultaneously separating and detecting terpene ketone analogue and chiral enantiomer thereof |
| US11519865B2 (en) | 2020-02-28 | 2022-12-06 | Disco Corporation | Crack detection method |
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- 2019-02-20 CN CN201910127465.6A patent/CN109738548A/en not_active Withdrawn
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US11519865B2 (en) | 2020-02-28 | 2022-12-06 | Disco Corporation | Crack detection method |
| CN112798716A (en) * | 2021-02-08 | 2021-05-14 | 国家烟草质量监督检验中心 | Method for measuring migration rates of growth regulator and pyrethroid pesticide in cigarette without burning by heating |
| CN113671063A (en) * | 2021-07-12 | 2021-11-19 | 河南中烟工业有限责任公司 | Method for measuring ester transfer rate in heated cigarette |
| CN115097054A (en) * | 2022-06-22 | 2022-09-23 | 云南中烟工业有限责任公司 | Method for simultaneously separating and detecting terpene ketone analogue and chiral enantiomer thereof |
| CN115097054B (en) * | 2022-06-22 | 2024-06-04 | 云南中烟工业有限责任公司 | Method for simultaneously separating and detecting terpene ketone analogue and chiral enantiomer thereof |
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