CN105044239B - The cold trap trapping gas chromatography/mass spectrometry detection method of nitromethane in a kind of gaseous phase of main stream smoke of cigarette - Google Patents
The cold trap trapping gas chromatography/mass spectrometry detection method of nitromethane in a kind of gaseous phase of main stream smoke of cigarette Download PDFInfo
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- CN105044239B CN105044239B CN201510489303.9A CN201510489303A CN105044239B CN 105044239 B CN105044239 B CN 105044239B CN 201510489303 A CN201510489303 A CN 201510489303A CN 105044239 B CN105044239 B CN 105044239B
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Abstract
The invention discloses the method for nitromethane content in a kind of cold trap trapping Gc/ms Analyser detection gaseous phase of main stream smoke of cigarette.The method is accurate to add nitromethane d using nitromethane in isopropanol dry ice under cryogenic (≤70 DEG C) methanol solvate cold trap trapping gaseous phase of main stream smoke of cigarette3Internal standard, sample it is hand it is uniform after, detected using gas chromatograph/mass spectrometer, retention time and abundance of ions are than qualitative, and characteristic ion is quantitative.The present invention is using nitromethane content in gas chromatograph/mass spectrometer accurate quantitative analysis gaseous phase of main stream smoke of cigarette, method is reproducible, and method pre-treatment is simple, easily operation, the rate of recovery is high, is capable of achieving the Accurate Determining to nitromethane content in gaseous phase of main stream smoke of cigarette.
Description
Technical field
The invention belongs to cigarette smoke chemical index detection field, and in particular to nitro in a kind of gaseous phase of main stream smoke of cigarette
The cold trap trapping of methane-gas chromatography/mass spectrometry detection method.
Background technology
It is colourless liquid under nitromethane normal temperature, is heated volatile, liver kidney, central lesion can be caused, for a long time
Contact can cause slow poisoning, and international cancer research institution is classified as the 2B class materials that the mankind may be allowed carcinogenic.In China
Cosmetic industry has formulated maximum limitation requirement and corresponding regulation, and it is dense that air quality monitoring aspect also specify short contact permission
The monitoring rule such as degree and limit value.In recent years, smoking is received significant attention with health problem, in March, 2012 U.S.'s food and medicine prison
The HPHCs lists during office (FDA) has issued new tobacco product and tobacco smoke are superintended and directed, nitromethane is listed in wherein；Nitro first
Alkane is one of cigarette VOC, and wherein nitromethane is the important composition material in Hoffman inventories in 2001.
The analysis method of nitromethane in a kind of reproducible, rate of recovery cigarette smoke high is hence set up, for monitoring cigarette smoke
The burst size of middle nitromethane, more overall scientific ground evaluating cigarette flue gas security have important realistic meaning.
The text using nitromethane in cold trap trapping-gas chromatography/mass spectrometry detection cigarette mainstream flue gas is there is no at present
Report and patent are offered, the present invention uses methyl alcohol cold solvent cold trap trapping method and gas chromatography/mass spectrometry, using Supelco
The special capillary columns of VOCOL, realize the good separation of nitromethane, the use of nitromethane-d3 are interior scalar quantity, preferably solve
Sample detection poor reproducibility, complex operation, the quantitative defect such as inaccurate can accurately and quickly determine gaseous phase of main stream smoke of cigarette
Middle nitromethane content.For safety cigarette evaluation provides technical support.
The content of the invention
It is an object of the invention to provide it is a kind of while and accurately in gaseous phase of main stream smoke of cigarette nitromethane cold-trap
Trapping-gas chromatography/mass spectrometry detection method, with nitromethane-d3 as internal standard compound, using the inspection of gas chromatography combined with mass spectrometry
Survey method.With cambridge filter trap gaseous phase of main stream smoke of cigarette in granule phase substance, connect after smoking machine trap two series connection
Absorption bottle, absorption bottle is equipped with Chromatographic Pure Methanol solution, the nitre in trapping gaseous phase of main stream smoke of cigarette thing under the conditions of cryotrap
Methylmethane；After cigarette smoking is finished, merge absorbing liquid, accurate quantitative analysis add inner mark solution, it is hand it is uniform after, enter gas-chromatography-
Mass spectral analysis；Under selection ion monitoring mode, using retention time and abundance of ions than qualitative, characteristic ion is quantitative, internal standard method
Determine the content of the nitromethane in gaseous phase of main stream smoke of cigarette.The method is simple to operate, reproducible, and the rate of recovery is high, can be real
Now to the Accurate Determining of nitromethane content in gaseous phase of main stream smoke of cigarette, the present invention establishes a kind of gaseous phase of main stream smoke of cigarette
The cold trap trapping of middle nitromethane-gas chromatography/mass spectrometry detection method, is nitro first in monitoring gaseous phase of main stream smoke of cigarette
The burst size of alkane provides technical support.
To realize the purpose of the present invention, it is achieved through the following technical solutions：
The cold trap trapping of nitromethane in a kind of gaseous phase of main stream smoke of cigarette-gas chromatography/mass spectrometry detection method,
It comprises the following steps：
With cambridge filter trap gaseous phase of main stream smoke of cigarette in granule phase substance, connect after smoking machine trap two series connection
Absorption bottle, absorption bottle is equipped with Chromatographic Pure Methanol solution, the nitre in trapping gaseous phase of main stream smoke of cigarette thing under the conditions of cryotrap
Methylmethane；After cigarette smoking is finished, merge absorbing liquid, accurate quantitative analysis add inner mark solution, it is hand it is uniform after, enter gas-chromatography-
Mass spectral analysis；Selection ion monitoring mode, legal using retention time and Standard entertion, characteristic ion is quantitative, and internal standard method is surveyed
Determine the content of the nitromethane in gaseous phase of main stream smoke of cigarette.
Further, the internal standard compound is preferably nitromethane-d3。
Optimal technical scheme of the present invention is comprised the following steps：
1. the balance of cigarette and suction：Sample cigarette is balanced and selected according to tobacco business GB GB/T 5606.1-2004,
Two respectively absorption bottles equipped with methyl alcohol of series connection are connected after smoking machine trap, absorption bottle is placed in the cold-trap of isopropanol-dry ice
In (≤- 70 DEG C), according to tobacco business GB GB/T 19609-2004 regulation aspirate 10 cigarette, cambridge filter trapping volume
The granule phase substance of cigarette main flume, nitromethane in methyl alcohol cold solvent trapping gaseous phase of main stream smoke of cigarette.
2. sample pre-treatments and analysis：Cigarette smoking merges absorbing liquid after finishing, add nitromethane-d3 inner mark solutions,
It is hand it is uniform after, directly enter gas chromatograph/mass spectrometer and detected, characteristic ion peak qualitative using retention time, selection ion
Response is quantitative, using nitromethane content in deuterated internal standard method Accurate Determining gaseous phase of main stream smoke of cigarette.
Most preferred technique scheme of the present invention is comprised the following steps：
(1), the balance of cigarette and suction：Sample cigarette is balanced and selected according to tobacco business GB GB/T 5606.1-2004
Branch, connects two respectively absorption bottles equipped with 15mL methyl alcohol of series connection after smoking machine trap, and absorption bottle is placed in isopropanol-dry ice
, in -70 DEG C~-80 DEG C cold-traps of temperature, according to tobacco business GB GB/T 19609-2004 regulation aspirate 10 cigarette,
Cambridge filter traps the granule phase substance of cigarette mainstream flue gas, nitromethane in methyl alcohol cold solvent trapping gaseous phase of main stream smoke of cigarette.
(2), sample pre-treatments and analysis：Cigarette smoking merges absorbing liquid after finishing, and 120 μ L nitromethanes of accurate addition-
D3 inner mark solutions, it is hand it is uniform after, directly enter gas chromatograph/mass spectrometer and detected, determined using retention time, selection ion
Property, characteristic ion peak response is quantified, using nitromethane content in deuterated internal standard method Accurate Determining gaseous phase of main stream smoke of cigarette.
(3), analytical conditions for gas chromatography：
Chromatographic column：Supelco VOCOL capillary columns (60m × 0.32mm × 1.8 μm)；
GC conditions：Injector temperature：180 DEG C, sample size：2.0 μ L, carrier gas：Helium, column flow：1.2mL/
Min, split ratio：5:1, temperature programming：40 DEG C of initial temperature, retains 6min, and 220 DEG C are risen to 20 DEG C/min, retains 6min；
4. Mass Spectrometry Conditions：Ionization voltage：70eV, ion source temperature：230 DEG C, quadrupole rod temperature：150 DEG C, solvent delay：
6min, scan mode：SIM；
Nitromethane and internal standard characteristic ion：Nitromethane quota ion is 61, nitromethane-d3 quota ions 64；
Technological progress and effect that the present invention is obtained：
1. using the cold-trap technology of isopropanol-dry ice, Chromatographic Pure Methanol is absorbent, can effectively absorb cigarette mainstream flue gas
Nitromethane in gas phase.
2. detection method, equation of linear regression is Y=0.1945X+0.0009, coefficient R2It is 0.9997,
Detect and be limited to 0.02 μ g/ branch, recovery of standard addition, between 91.7~96.6%, precision RSD % is less than 6%.
3. it is internal standard compound that the present invention uses nitromethane-d3, and GC/MS analytical technologies are realized in gaseous phase of main stream smoke of cigarette
The accurate quantitative analysis detection of nitromethane.The method is simple to operate, and favorable reproducibility, the rate of recovery is high.
4. the instrument and equipment that the present invention is used are laboratory conventional analysis and equipment, and inventive method is simple to operate,
Method is easy to implement, and sample throughput is big, is adapted to batch samples detection, is capable of achieving low cost detection.
Brief description of the drawings
The standard sample chromatogram that Fig. 1 is obtained for the embodiment of the present invention
The typical cigarette sample chromatogram figure that Fig. 2 is obtained for the embodiment of the present invention
Specific embodiment
For ease of understanding the present invention, there is provided the present invention is described further for following examples and accompanying drawing, but this reality
It is illustrative to apply the content that example stated, and should not regard limiting the scope of the invention as.
1. test apparatus：6890N/5975 gas chromatograph-mass spectrometers；Electronic analytical balance (sensibility reciprocal 0.1mg)；Supelco
VOCOL capillary columns (60m × 0.32mm × 1.8 μm)；RM20H smoking machines；Absorption bottle.
2. test reagent and solvent are prepared：Methyl alcohol (chromatographically pure), isopropanol (AR)；Dry ice；Nitromethane standard liquid
(100μg/mL)；Nitromethane-d3 standard liquids (100 μ g/mL).
3. cigarette sample：It is purchased in market.
The gas chromatography/mass spectrometry detection method of nitromethane in a kind of gaseous phase of main stream smoke of cigarette of the present invention, including
Following steps：
The making of standard curve：5L, 25 μ L, 125 μ L, 250 μ L, 625 μ L, 1250 μ L nitromethanes are accurately pipetted respectively extremely
25mL volumetric flasks, it is accurate to add 100 μ L nitromethane-d3 internal standard standard liquids, it is quantitative to scale with methyl alcohol, it is configured to concentration point
Not Wei 0.02 μ g/mL, 0.1 μ g/mL, 0.5 μ g/mL, 1 μ g/mL, 2.5 μ g/mL, the standard liquid of 5 μ g/mL, with nitromethane
Peak area carries out linear regression analysis with the ratio between its concentration that compares of the peak area of nitromethane-d3.
The balance of cigarette and suction：Sample cigarette is balanced and selected according to tobacco business GB GB/T 5606.1-2004,
Two respectively absorption bottles equipped with 15mL methyl alcohol of series connection are connected after smoking machine trap, absorption bottle is placed in isopropanol-dry ice
In cold-trap (- 70 DEG C~-80 DEG C of temperature), 10 cigarette, sword are aspirated according to the regulation of tobacco business GB GB/T 19609-2004
Bridge filter disc traps the granule phase substance of cigarette mainstream flue gas, nitromethane in methyl alcohol cold solvent trapping cigarette mainstream flue gas.
Sample pre-treatments and analysis：Cigarette smoking merges absorbing liquid after finishing, accurate to add in 120 μ L nitromethanes-d3
Mark solution, it is hand it is uniform after, directly enter gas chromatograph/mass spectrometer and detected, it is qualitative using retention time, selection ion, it is special
Levy ion peak response to quantify, using nitromethane content in deuterated internal standard method Accurate Determining gaseous phase of main stream smoke of cigarette.
Analytical conditions for gas chromatography：
Chromatographic column：Supelco VOCOL capillary columns (60m × 0.32mm × 1.8 μm)；
GC conditions：Injector temperature：180 DEG C, sample size：2.0 μ L, carrier gas：Helium, column flow：1.2mL/
Min, split ratio：5:1, temperature programming：40 DEG C of initial temperature, retains 6min, and 220 DEG C are risen to 20 DEG C/min, retains 6min；
Mass spectral analysis condition：Ionization voltage：70eV, ion source temperature：230 DEG C, quadrupole rod temperature：150 DEG C, solvent prolongs
Late：6min, scan mode：SIM；
Nitromethane and internal standard characteristic ion：Nitromethane quota ion is 61, nitromethane-d3 quota ions 64；
Method standard curve, linearly dependent coefficient, test limit and quantitative limit：By the standard sample continuous sample introduction of least concentration
10 times, detection limit is drawn with the standard deviation of 3 times of measurement results, and quantitative limit is drawn with the standard deviation of 10 times of measurement results.Knot
Fruit is as shown in table 1.
The range of linearity of this method of table 1, coefficient correlation, test limit and quantitative limit
Method precision and the rate of recovery：To embodiment cigarette parallel determination 6 times, method precision investigation is carried out, and to reality
Applying a cigarette and being separately added into high, medium and low 3 horizontal standard specimens carries out recovery of standard addition investigation.Result is as shown in table 2.
The precision of this method of table 2 and determination of recovery rates result (n=6)
Show that the method precision RSD % is less than 6% from table 1, the result of table 2；Recovery of standard addition 91.7~96.6% it
Between, therefore showing that the method precision is good, the rate of recovery is high, is suitable for the measure of nitromethane in gaseous phase of main stream smoke of cigarette.
Claims (3)
1. in a kind of gaseous phase of main stream smoke of cigarette nitromethane cold trap trapping-gas chromatography/mass spectrometry detection method, it is special
Levy is to comprise the following steps：
（1）, cigarette selection with suction：Balanced according to tobacco business GB GB/T 5606.1-2004 and select sample cigarette,
After smoking machine trap connect two series connection respectively equipped with methyl alcohol absorption bottles, absorption bottle be placed in isopropanol-dry ice ,≤- 70
DEG C cold-trap in, according to tobacco business GB GB/T 19609-2004 regulation aspirate 10 cigarette, cambridge filter trapping cigarette
The granule phase substance of main flume, nitromethane in methyl alcohol cold solvent trapping gaseous phase of main stream smoke of cigarette；
（2）, sample pre-treatments and analysis：Cigarette smoking merges absorbing liquid after finishing, add nitromethane-d3 inner mark solutions, hand
After shaking uniformly, directly enter gas chromatograph/mass spectrometer and detected, qualitative using retention time, selection ion, characteristic ion peak rings
Should quantify, using nitromethane content in deuterated internal standard method Accurate Determining gaseous phase of main stream smoke of cigarette；
Step（1）In the selection and suction of cigarette, two respectively suctions equipped with 15mL methyl alcohol of series connection are connected after smoking machine trap
Bottle is received, absorption bottle is placed in isopropanol-dry ice, -70 DEG C~-80 DEG C of temperature cold-trap；
Step（2）In sample pre-treatments and analysis：Cigarette smoking merges absorbing liquid after finishing, and 120 μ L nitromethanes of accurate addition-
D3 inner mark solutions；
Analytical conditions for gas chromatography is as follows：
Chromatographic column：Supelco VOCOL capillary columns, 60m × 0.32mm × 1.8 μm；
GC conditions：Injector temperature：180 DEG C, sample size：2.0 μ L, carrier gas：Helium, column flow：1.2mL/min, point
Stream ratio：5:1, temperature programming：40 DEG C of initial temperature, retains 6min, and 220 DEG C are risen to 20 DEG C/min, retains 6min.
2. in a kind of gaseous phase of main stream smoke of cigarette according to claim 1 nitromethane cold trap trapping-gas-chromatography/matter
Spectrum combination detection method, it is characterised in that Mass Spectrometry Conditions are as follows：Ionization voltage：70eV, ion source temperature：230 DEG C, quadrupole rod temperature
Degree：150 DEG C, solvent delay：6min, scan mode：SIM.
3. in a kind of gaseous phase of main stream smoke of cigarette according to claim 1 and 2 nitromethane cold trap trapping-gas phase color
Spectrum/mass spectrometry detection method, it is characterised in that：Nitromethane and internal standard characteristic ion：Nitromethane quota ion 61, nitro
Methane-d3 quota ions 64.
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