CN106645444A - Method for detecting polycyclic aromatic hydrocarbon content in smokeless tobacco products - Google Patents
Method for detecting polycyclic aromatic hydrocarbon content in smokeless tobacco products Download PDFInfo
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- CN106645444A CN106645444A CN201610855952.0A CN201610855952A CN106645444A CN 106645444 A CN106645444 A CN 106645444A CN 201610855952 A CN201610855952 A CN 201610855952A CN 106645444 A CN106645444 A CN 106645444A
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- benzo
- pyrene
- fluoranthene
- anthracene
- aromatic hydrocarbon
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
Abstract
The invention discloses a method for detecting polycyclic aromatic hydrocarbon content in smokeless tobacco products. The method includes the steps: extracting the smokeless tobacco products by the aid of extraction agents; detecting filtered extraction solution by the aid of a GC-MS/MS (gas chromatography-mass spectrometry). The method can simultaneously measure content of indene, naphthalene, 1-methylnaphthalene, 2-methylnaphthalene, acenaphthylene, acenaphthene, fluorine, phenanthrene, anthracene, fluoranthene, pyrene, benzo [a] anthracene, chrysene, benzo [b] fluoranthene, benzo [k] fluoranthene, benzo [j] fluoranthene, benzo [e] pyrene, benzo [a] pyrene, perylene, indene [1, 2, 3-cd] pyrene, diphenyl [a, h] anthracene, benzo [g, h, i] pyrene and the like in the smokeless tobacco products. The method fills in gaps of the prior art and has the advantages that the method is simple, convenient and rapid in sample pretreatment, goof in detection accuracy and repeatability and high in analytical test flux, and the method is applicable to rapid analysis of large-batch samples.
Description
Technical field
The invention belongs to smoke-free tobacco product technical field of analysis and detection simultaneously, and in particular to one kind can be detected smokelessly
22 kinds of multiring aromatic hydrocarbon substances in gas tobacco product, including：Indenes, naphthalene, 1- methyl naphthalenes, 2- methyl naphthalenes, acenaphthylene, acenaphthene, fluorenes, phenanthrene,
Anthracene, fluoranthene, pyrene, benzo [a] anthracene, in the wrong, benzo [b] fluoranthene, benzo [k] fluoranthene, benzo [j] fluoranthene, benzo [e] pyrene, benzo [a]
Bi, perylenes, indeno [1,2,3-cd] pyrene, dibenzo [a, h] anthracene, the method for the content of benzo [g, h, i] pyrene.
Technical background
Smoke-free tobacco product (Smokeless tobacco products, STPs) refer to when using without the need for burning or not
The tobacco product of flue gas is produced, mouth type (Oral STPs) and nose type (Nasal STPs) two can be divided into according to occupation mode
Big type.Mouth type STPs, wherein being its topmost product form containing cigarette, has including chewing tobacco, containing polytypes such as cigarette, molten cigarettes
Snuff and two kinds of Snus, the occupation mode of the two is put between gingiva and lip, entirely different with traditional Folium Nicotianae preparatum.
In recent years, global Tobacco Control dynamics constantly strengthens, under the influence of a series of Tobacco Control laws, policy and action, Nicotiana tabacum L.
Development environment there occurs deep and great change, and tobacco product structure just accelerates adjustment towards variation and smokeless direction.
Tradition burns and sucks the development of formula tobacco product and faces bigger pressure, and consume smoke-free tobacco product will not produce it is " second-hand
The chemical composition that cigarette " and result of combustion of tobacco are generated, therefore, smoke-free tobacco product has been increasingly becoming a kind of important Nicotiana tabacum L. and has disappeared
Fei Pin, and represent the important development trend of international Field of Tobacco.
About 20,000,000,000 dollars of global non-traditional tobacco product sales volume in 2011, account for tobacco product gross sales amount 3% is left
It is right.Though share is shared less, the situation of its rapid growth is placed on traditional cigarette sales volume and declines 2% and above-mentioned Tobacco Control dynamics day
Under the background for becoming severe, smoke-free tobacco product seems that potentiality are unlimited, and situation is noticeable, it is meant that a smoke-free tobacco product is walked
The chance of upper arena of history focus is arrived.
But it is at present, to smoke-free tobacco product composition and its also little containing quantifier elimination, to the standard of its composition detection still
Category is blank.
During polycyclic aromatic hydrocarbon (Polycyclic Aromatic Hydrocarbons, abbreviation PAHs) is smoke-free tobacco product
One type organic matter of generally existing, they are discharged into flue gas and work as along with the imperfect combustion and thermal cracking processes of Organic substance
In, smoker and the healthy of involuntary smoker are caused damage.PAHs can cause human body oxidative stress and DNA damage, and
And the various PAHs of confirmation are studied with stronger toxicity and carcinogenesis.Therefore, detect that the PAHs in smoke-free tobacco product contains
Amount controls cigarette quality significant.
But tobacco business there is presently no multiring aromatic hydrocarbon substance content in any standard guidance smoke-free tobacco product
Detection.
The content of the invention
Present invention aims to the deficiencies in the prior art, there is provided one kind is easy to operate, quick, it is dry by impurity to be difficult
Disturb, testing result accurately, can be while the 22 kinds of multiring aromatic hydrocarbon substances (indenes, naphthalene, the 1- methyl that detect in smoke-free tobacco product
Naphthalene, 2- methyl naphthalenes, acenaphthylene, acenaphthene, fluorenes, phenanthrene, anthracene, fluoranthene, pyrene, benzo [a] anthracene, in the wrong, benzo [b] fluoranthene, benzo [k] fluoranthene, benzene
And [j] fluoranthene, benzo [e] pyrene, benzo [a] Bi, perylenes, indeno [1,2,3-cd] pyrene, dibenzo [a, h] anthracene, benzo [g, h, i]
Pyrene) content method.
The purpose of the present invention is achieved through the following technical solutions.
Unless otherwise stated, percent of the present invention is mass percent.
A kind of method of multiring aromatic hydrocarbon substance content in detection smoke-free tobacco product, it is characterised in that including following step
Suddenly：
(1) sample extraction：
Take smoke-free tobacco product to be placed in collection vessel, add inner mark solution and extractant, after ultrasound or oscillation extraction,
Extract filter membrane, collects the extract after filtering and is placed in chromatogram bottle as sample, to be detected；
Wherein, the internal standard substance in described inner mark solution is the deuterated compound of 22 kinds of multiring aromatic hydrocarbon substances or it is similar
The deuterated compound of thing, by one or more deuterated compound therein hexamethylene, methanol, isopropanol, dichloromethane are dissolved in
Or in chloroform, as inner mark solution；Described extractant is hexamethylene, methanol, isopropanol, dichloromethane or chloroform；Described
22 kinds of multiring aromatic hydrocarbon substances are indenes, naphthalene, 1- methyl naphthalenes, 2- methyl naphthalenes, acenaphthylene, acenaphthene, fluorenes, phenanthrene, anthracene, fluoranthene, pyrene, benzo [a]
Anthracene, in the wrong, benzo [b] fluoranthene, benzo [k] fluoranthene, benzo [j] fluoranthene, benzo [e] pyrene, benzo [a] Bi, perylenes, indeno [1,2,3-
Cd] pyrene, dibenzo [a, h] anthracene and benzo [g, h, i] pyrene；
(2) sample gas chromatography tandem mass spectrometry GC-MS/MS detections：
GC-MS/MS testing conditions：
Chromatography column feed materials mouth temperature：260℃；Sample size：1μL；Input mode：Splitless injecting samples；
By temperature programming, it is sufficiently separated target compound；
Transmission line temperature：280℃；Mass spectrum ionizes mode：EI；Ion source temperature：230 DEG C～280 DEG C；
Scanning of the mass spectrum mode：Multiple-reaction monitoring MRM patterns or dynamic multiple-reaction monitoring dMRM patterns；Collision gas：Nitrogen, stream
Fast 1.5mL/min；Carrier gas：Helium, flow velocity 2.25mL/min；
(3) quantitative analyses：
Absolute quantitation is carried out using internal standard method；
A series of standard working solution of reference materials containing variable concentrations object and internal standard substance is prepared, using GC-
MS/MS methods set up standard working curve, for the detection by quantitative of sample；Multiring aromatic hydrocarbon substance content in sample presses formula (1)
Calculate；
Ci=CI is surveyed*V/m.................................................(1)
In formula, CiIt is the quality of multiring aromatic hydrocarbon substance i in per gram of smoke-free tobacco product to be measured, unit is ng/g, knot
Fruit is accurate to 0.01ng/g；
CI is surveyedThe content of the multiring aromatic hydrocarbon substance i obtained by GC-MS/MS measure, unit is ng/mL；
V is smoke-free tobacco product extraction solvent volume used, and unit is mL；
M is the weight of the smoke-free tobacco product for carrying out this analysis, and unit is g；
The arithmetic mean of instantaneous value of two parallel samples is taken as test result, that is, obtain indenes in smoke-free tobacco product to be measured,
Naphthalene, 1- methyl naphthalenes, 2- methyl naphthalenes, acenaphthylene, acenaphthene, fluorenes, phenanthrene, anthracene, fluoranthene, pyrene, benzo [a] anthracene, in the wrong, benzo [b] fluoranthene, benzo
[k] fluoranthene, benzo [j] fluoranthene, benzo [e] pyrene, benzo [a] Bi, perylenes, indeno [1,2,3-cd] pyrene, dibenzo [a, h] anthracene and benzene
And the content of [g, h, i] pyrene.
In step (1), the amount of weighing of described smoke-free tobacco product is 0.1～10g；Described collection vessel be 25～
The ground conical flask of 100mL；The consumption of extractant is 5～50mL, and extraction time is 10～60min.
In step (1), described internal standard substance is preferably deuterated naphthalene, deuterated benzo [a] pyrene, deuterated benzo [a] anthracene or deuterated
It is luxuriant and rich with fragrance.
In step (1), described filter membrane is organic phase filter membrane, and filter sizes are 0.22 μm or 0.45 μm.Preferably：0.22
μm nylon66 fiber filter membrane.
In step (2), chromatograph detection chromatographic column used is DB-5MS, HP-5MS or HP-5MS UI chromatographic columns.
In step (2), described temperature programming condition is preferred：40 DEG C of initial temperature, keeps 7min, is risen to 20 DEG C/min
100 DEG C, 300 DEG C are risen to 4 DEG C/min, keep 10min.
In step (2), described scanning of the mass spectrum mode is preferably：Dynamic multiple-reaction monitoring dMRM patterns.
In step (2), described ion source temperature is preferably：250 DEG C or 280 DEG C.
In step (3), the concentration of object is 0.1～500ng/mL in described standard working solution.
Further, mass spectrometry parameters optimization, wherein chemical combination are carried out to the reference material and internal standard substance in standard working solution
The design parameter of the parent ion, daughter ion and collision energy CE values of thing is as follows：
Compared with prior art, the inventive method has following features and excellent results：
1st, the present invention has filled up prior art blank, determines 22 in smoke-free tobacco product simultaneously using GC-MS/MS methods
The content of kind of multiring aromatic hydrocarbon substance, specially indenes, naphthalene, 1- methyl naphthalenes, 2- methyl naphthalenes, acenaphthylene, acenaphthene, fluorenes, phenanthrene, anthracene, fluoranthene,
Pyrene, benzo [a] anthracene, in the wrong, benzo [b] fluoranthene, benzo [k] fluoranthene, benzo [j] fluoranthene, benzo [e] pyrene, benzo [a] Bi, perylenes, indenes
And [1,2,3-cd] pyrene, dibenzo [a, h] anthracene, the content of benzo [g, h, i] pyrene；Wherein indenes, acenaphthylene, acenaphthene, fluoranthene, pyrene, benzo
[content of the composition such as e] Bi, perylenes, indeno [1,2,3-cd] pyrene is quantitative in smoke-free tobacco product first for [j] fluoranthene, benzo
Detect；
2nd, GC-MS methods and HPLC methods are compared, the method for the present invention has the sensitivity of more preferable selectivity and Geng Gao, especially
Trace samplings analysis in suitable complex matrices, and the requirement to sample substrate degree of purity is relatively low；
3rd, the present invention is extracted first with extractant to smoke-free tobacco product, and extract is direct Jing after membrane filtration again
Quantitative determined using GC-MS/MS methods so that sample pre-treatments are quick, easy, while with compared with high detection efficiency,
The use of pre-treatment organic reagent is substantially reduced, the pollution to environment is reduced；Significantly improve the analysis throughput of sample, and accurately
It is property, reproducible.
Description of the drawings
Fig. 1 is indenes, naphthalene, 1- methyl naphthalenes, 2- methyl naphthalenes, acenaphthylene, acenaphthene, fluorenes, phenanthrene, anthracene, fluoranthene, pyrene, benzo [a] anthracene, in the wrong, benzene
And [b] fluoranthene, benzo [k] fluoranthene, benzo [j] fluoranthene, benzo [e] pyrene, benzo [a] Bi, perylenes, indeno [1,2,3-cd] pyrene, two
The structural formula of 22 kinds of compounds of benzo [a, h] anthracene and benzo [g, h, i] pyrene；
Fig. 2～Fig. 7 is 22 kinds of multiring aromatic hydrocarbon substance contents in the smoke-free tobacco product sample A of the embodiment of the present invention 1
The chromatogram of measure；
Fig. 8 is the process chart of the inventive method.
Specific embodiment
For a better understanding of the present invention, with reference to the accompanying drawings and examples the present invention is described in further detail,
But drawings and Examples are not limited to the technical solution.
Embodiment 1：
Weigh 3g buccal cigarettes to be placed in 25mL ground conical flasks as sample A, add containing deuterated naphthalene (320ng/mL) and
The μ L of cyclohexane solution 250 of deuterated benzo [a] pyrene (320ng/mL) add 15mL hexamethylene as extraction as internal standard substance
Agent；After by conical flask at room temperature oscillation extraction 40min, by extract by 0.22 μm of nylon66 fiber filter membrane, filtrate is collected in color
In spectrum bottle, treat that GC-MS/MS is analyzed.
GC-MS/MS analysis conditions：
Chromatography column feed materials mouth temperature：260℃；Sample size：1μL；Input mode：Splitless injecting samples；Chromatographic column：HP-5MS UI
(30m*0.32mm*0.25μm)；Temperature programming：40 DEG C of initial temperature, keeps 7min；100 DEG C are risen to 20 DEG C/min；With 4 DEG C/
Min rises to 300 DEG C of holding 10min；Transmission line temperature：280℃；Mass spectrum ionizes mode：EI；Ion source temperature：280℃；Mass spectrum
Scan mode：Dynamic multiple-reaction monitoring dMRM patterns；Collision gas：Nitrogen, flow velocity 1.5mL/min；Carrier gas：Helium, flow velocity
2.25mL/min。
To indenes, naphthalene, 1- methyl naphthalenes, 2- methyl naphthalenes, acenaphthylene, acenaphthene, fluorenes, phenanthrene, anthracene, fluoranthene, pyrene, benzo [a] anthracene, in the wrong, benzo
[b] fluoranthene, benzo [k] fluoranthene, benzo [j] fluoranthene, benzo [e] pyrene, benzo [a] Bi, perylenes, indeno [1,2,3-cd] pyrene, hexichol
And [a, h] anthracene, the reference material of benzo [g, h, i] pyrene and its internal standard compound carry out mass spectrometry parameters optimization, there is related parameter to include changing
The parent ion of compound, daughter ion and collision energy (CE) are as shown in table 1.
The mass spectral analyses parameter of the compound of table 1
Quantitative analyses condition：
In setting up the series of standards working solution of standard working curve, containing indenes, naphthalene, 1- methyl naphthalenes, 2- methyl naphthalenes, acenaphthene
Alkene, acenaphthene, fluorenes, phenanthrene, anthracene, fluoranthene, pyrene, benzo [a] anthracene, in the wrong, benzo [b] fluoranthene, benzo [k] fluoranthene, benzo [j] fluoranthene, benzo
[e] pyrene, benzo [a] Bi, perylenes, indeno [1,2,3-cd] pyrene, dibenzo [a, h] anthracene, the reference material of benzo [g, h, i] pyrene and its interior
Deuterated naphthalene and deuterated benzo [a] pyrene are marked, solvent is hexamethylene.The concentration of each object is identical in standard working solution, concentration according to
It is secondary for 1ng/mL, 2ng/mL, 5ng/mL, 10ng/mL, 20ng/mL, 50ng/mL, 100ng/mL and 500ng/mL；Standard works
Internal standard concentration is 8ng/mL in solution.
Multiring aromatic hydrocarbon substance content in sample is calculated by formula (1)；
Ci=CI is surveyed*V/m.................................................(1)
In formula, CiIt is the quality of multiring aromatic hydrocarbon substance i in per gram of smoke-free tobacco product to be measured, unit is ng/g, knot
Fruit is accurate to 0.01ng；
CI is surveyedThe content of the multiring aromatic hydrocarbon substance i obtained by GC-MS/MS measure, unit is ng/mL；
V is smoke-free tobacco product extraction solvent volume used, and unit is mL；
M is the weight of the smoke-free tobacco product for carrying out this analysis, and unit is g；
When the internal standard concentration (unit is ng/mL) in sample extraction liquid and standard working solution is differed, it can be used
He is calculated general equation.
The arithmetic mean of instantaneous value of two parallel samples is taken as test result.
22 kinds of polycyclic aromatic hydrocarbon compounds are detected simultaneously in sample A, and its GC-MS/MS chromatogram is respectively such as Fig. 2-Fig. 7 institutes
Show.Wherein, Fig. 2 is indenes, deuterated naphthalene, naphthalene, 1- methyl naphthalenes, the chromatogram of 2- methyl naphthalene content determinations in sample；Fig. 3 is in sample
Acenaphthylene, acenaphthene, the chromatogram of fluorenes assay；Fig. 4 is sample China and Philippines, the chromatogram of anthracene assay；Fig. 5 be sample in fluoranthene,
Pyrene, benzo [a] anthracene, the chromatogram for bending assay；Fig. 6 is that benzo [b] fluoranthene, benzo [k] fluoranthene, benzo [j] are glimmering in sample
Anthracene, benzo [e] pyrene, deuterated benzo [a] pyrene, benzo [a] pyrene, the chromatogram of perylene assay；Fig. 7 be sample in indeno [1,2,
3-cd] pyrene, dibenzo [a, h] anthracene, the chromatogram of benzo [g, h, i] pyrene assay.From above-mentioned 6 figure, polycyclic aromatic hydrocarbon
Compound is separated preferably on chromatogram, detection by quantitative credible result.
The testing result of 22 kinds of polycyclic aromatic hydrocarbon contents is specifically as shown in table 2 in sample A.
The testing result of 22 kinds of multiring aromatic hydrocarbon substance contents in the smoke-free tobacco product sample A of table 2
Embodiment 2：
Repeat embodiment 1, there is following difference：
Weigh 10g chewing tobacco to be placed in 100mL ground conical flasks as sample B, add and contain deuterated benzo [a] anthracene
(200ng/mL) and it is deuterated phenanthrene (200ng/mL) the μ L of methanol solution 500 as internal standard substance, add 50mL methanol as extraction
Take agent；After by conical flask at room temperature oscillation extraction 60min, by extract by 0.45 μm of polyether sulfone (PES) filter membrane, filter is collected
Liquid treats that GC-MS/MS is analyzed in chromatogram bottle.
GC-MS/MS analysis conditions：
Chromatography column feed materials mouth temperature：260℃；Sample size：1μL；Input mode：Splitless injecting samples；Chromatographic column：DB-5MS capillarys
Pipe chromatographic column (30m*0.25mm*0.25 μm)；Temperature programming：150 DEG C of initial temperature, with 5 DEG C/min 280 DEG C of holdings are risen to
10min；Transmission line temperature：280℃；Mass spectrum ionizes mode：EI；Ion source temperature：230℃；Scanning of the mass spectrum mode：Many reaction prisons
Survey MRM patterns；Collision gas：Nitrogen, flow velocity 1.5mL/min；Carrier gas：Helium, flow velocity 2.25mL/min.
Quantitative analyses condition：
Set up in the series of standards working solution of standard working curve containing indenes, naphthalene, 1- methyl naphthalenes, 2- methyl naphthalenes, acenaphthylene,
Acenaphthene, fluorenes, phenanthrene, anthracene, fluoranthene, pyrene, benzo [a] anthracene, in the wrong, benzo [b] fluoranthene, benzo [k] fluoranthene, benzo [j] fluoranthene, benzo [e]
Pyrene, benzo [a] Bi, perylenes, indeno [1,2,3-cd] pyrene, dibenzo [a, h] anthracene, the reference material of benzo [g, h, i] pyrene and its internal standard
Deuterated benzo [a] anthracene and deuterated phenanthrene, solvent is methanol.The concentration of each object is identical in standard working solution, and concentration is followed successively by
0.5ng/mL, 1ng/mL, 2ng/mL, 5ng/mL, 10ng/mL, 20ng/mL, 40ng/mL；Internal standard concentration in standard working solution
It is 4ng/mL.
The testing result of 22 kinds of polycyclic aromatic hydrocarbon contents is as shown in table 2 in sample B.
Embodiment 3：
Repeat embodiment 1, there is following difference：
Weigh 10g Folium Nicotianae preparatums to be placed in 50mL ground conical flasks as sample C, add and contain deuterated benzo [a] pyrene (320ng/
ML the μ L of dichloromethane solution 500) add 20mL dichloromethane as extractant as internal standard substance；By conical flask in room
After the lower oscillation extraction 60min of temperature, by extract by 0.22 μm of polyether sulfone (PES) filter membrane, filtrate is collected in chromatogram bottle, treat
GC-MS/MS is analyzed.
GC-MS/MS analysis conditions：
Chromatography column feed materials mouth temperature：260℃；Sample size：1μL；Input mode：Splitless injecting samples；Chromatographic column：HP-5MS capillarys
Pipe chromatographic column (30m*0.25mm*0.25 μm)；Temperature programming：180 DEG C of initial temperature, with 3 DEG C/min 270 DEG C of holdings are risen to
20min；Transmission line temperature：280℃；Mass spectrum ionizes mode：EI；Ion source temperature：250℃；Scanning of the mass spectrum mode：How anti-dynamic is
DMRM patterns should be monitored；Collision gas：Nitrogen, flow velocity 1.5mL/min；Carrier gas：Helium, flow velocity 2.25mL/min.
Quantitative analyses condition：
Set up in the series of standards working solution of standard working curve containing indenes, naphthalene, 1- methyl naphthalenes, 2- methyl naphthalenes, acenaphthylene,
Acenaphthene, fluorenes, phenanthrene, anthracene, fluoranthene, pyrene, benzo [a] anthracene, in the wrong, benzo [b] fluoranthene, benzo [k] fluoranthene, benzo [j] fluoranthene, benzo [e]
Pyrene, benzo [a] Bi, perylenes, indeno [1,2,3-cd] pyrene, dibenzo [a, h] anthracene, the reference material of benzo [g, h, i] pyrene and its internal standard
Deuterated benzo [a] pyrene, solvent is dichloromethane.The concentration of each object is identical in standard working solution, and concentration is followed successively by
0.5ng/mL, 1ng/mL, 2ng/mL, 5ng/mL, 20ng/mL, 50ng/mL, 100ng/mL；Internal standard concentration in standard working solution
It is as 16ng/mL.
The testing result of 22 kinds of polycyclic aromatic hydrocarbon contents is as shown in table 2 in sample C.
By above example, it can be seen that the present invention has sample pre-treatments quick, easy, and accuracy, repeatability
The characteristics of good.The method can simultaneously detect the content of 22 kinds of polycyclic aromatic hydrocarbons in smoke-free tobacco product, and sample pre-treatments are simple,
Substantially increase the analysis throughput of sample.
Claims (10)
1. it is a kind of detection smoke-free tobacco product in multiring aromatic hydrocarbon substance content method, it is characterised in that including following step
Suddenly：
(1) sample extraction：
Take smoke-free tobacco product to be placed in collection vessel, add inner mark solution and extractant, after ultrasound or oscillation extraction, extraction
Liquid filter membrane, collects the extract after filtering and is placed in chromatogram bottle as sample, to be detected；
Wherein, the internal standard substance in described inner mark solution is the deuterated compound or its analog of 22 kinds of multiring aromatic hydrocarbon substances
Deuterated compound, by one or more deuterated compound therein hexamethylene, methanol, isopropanol, dichloromethane or chlorine are dissolved in
In imitative, as inner mark solution；Described extractant is hexamethylene, methanol, isopropanol, dichloromethane or chloroform；Described 22 kinds
Multiring aromatic hydrocarbon substance be indenes, naphthalene, 1- methyl naphthalenes, 2- methyl naphthalenes, acenaphthylene, acenaphthene, fluorenes, phenanthrene, anthracene, fluoranthene, pyrene, benzo [a] anthracene,
In the wrong, benzo [b] fluoranthene, benzo [k] fluoranthene, benzo [j] fluoranthene, benzo [e] pyrene, benzo [a] Bi, perylenes, indeno [1,2,3-cd]
Pyrene, dibenzo [a, h] anthracene and benzo [g, h, i] pyrene；
(2) sample gas chromatography tandem mass spectrometry GC-MS/MS detections：
GC-MS/MS testing conditions：
Chromatography column feed materials mouth temperature：260℃；Sample size：1μL；Input mode：Splitless injecting samples；
By temperature programming, it is sufficiently separated target compound；
Transmission line temperature：280℃；Mass spectrum ionizes mode：EI；Ion source temperature：230 DEG C～280 DEG C；
Scanning of the mass spectrum mode：Multiple-reaction monitoring MRM patterns or dynamic multiple-reaction monitoring dMRM patterns；Collision gas：Nitrogen, flow velocity
1.5mL/min；Carrier gas：Helium, flow velocity 2.25mL/min；
(3) quantitative analyses：
Absolute quantitation is carried out using internal standard method；
A series of standard working solution of reference materials containing variable concentrations object and internal standard substance is prepared, using GC-MS/MS
Method sets up standard working curve, for the detection by quantitative of sample；Multiring aromatic hydrocarbon substance content in sample is calculated by formula (1)；
Ci=CI is surveyeds*V/m.................................................(1)
In formula, CiIt is the quality of multiring aromatic hydrocarbon substance i in per gram of smoke-free tobacco product to be measured, unit is ng/g, as a result accurately
To 0.01ng/g；
CI is surveyedThe content of the multiring aromatic hydrocarbon substance i obtained by GC-MS/MS measure, unit is ng/mL；
V is smoke-free tobacco product extraction solvent volume used, and unit is mL；
M is the weight of the smoke-free tobacco product for carrying out this analysis, and unit is g；
The arithmetic mean of instantaneous value of two parallel samples is taken as test result, that is, obtains indenes, naphthalene, 1- in smoke-free tobacco product to be measured
Methyl naphthalene, 2- methyl naphthalenes, acenaphthylene, acenaphthene, fluorenes, phenanthrene, anthracene, fluoranthene, pyrene, benzo [a] anthracene, in the wrong, benzo [b] fluoranthene, benzo [k] are glimmering
Anthracene, benzo [j] fluoranthene, benzo [e] pyrene, benzo [a] Bi, perylenes, indeno [1,2,3-cd] pyrene, dibenzo [a, h] anthracene and benzo [g,
H, i] pyrene content.
2. detection method according to claim 1, it is characterised in that：In step (1), described smoke-free tobacco product
The amount of weighing is 0.1～10g；Described collection vessel is the ground conical flask of 25～100mL；The consumption of extractant is 5～50mL,
Extraction time is 10～60min.
3. detection method according to claim 1, it is characterised in that：In step (1), described internal standard substance be deuterated naphthalene,
Deuterated benzo [a] pyrene, deuterated benzo [a] anthracene or deuterated phenanthrene.
4. detection method according to claim 1, it is characterised in that：In step (1), described filter membrane is organic faciess filter
Film, filter sizes are 0.22 μm or 0.45 μm.
5. detection method according to claim 1, it is characterised in that：Described filter membrane is filtered for the nylon66 fiber in 0.22 μm of aperture
Film.
6. detection method according to claim 1, it is characterised in that：In step (2), chromatograph detection chromatographic column used is
DB-5MS, HP-5MS or HP-5MS UI chromatographic columns.
7. detection method according to claim 1, it is characterised in that：In step (2), described temperature programming condition is：
40 DEG C of initial temperature, keeps 7min, and with 20 DEG C/min 100 DEG C are risen to, and with 4 DEG C/min 300 DEG C are risen to, and keeps 10min.
8. detection method according to claim 1, it is characterised in that：In step (2), described ion source temperature is：250
DEG C or 280 DEG C.
9. detection method according to claim 1, it is characterised in that：In step (3), mesh in described standard working solution
The concentration of mark thing is 0.1～500ng/mL.
10. detection method according to claim 1, it is characterised in that：Further, to the standard in standard working solution
Thing and internal standard substance carry out mass spectrometry parameters optimization, and wherein the parent ion of compound, daughter ion and collision energy CE values is concrete
Parameter is as follows：
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