CN106442753B - A kind of method of TSNAs content in measurement cigarette mainstream flue gas - Google Patents
A kind of method of TSNAs content in measurement cigarette mainstream flue gas Download PDFInfo
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- CN106442753B CN106442753B CN201610764923.3A CN201610764923A CN106442753B CN 106442753 B CN106442753 B CN 106442753B CN 201610764923 A CN201610764923 A CN 201610764923A CN 106442753 B CN106442753 B CN 106442753B
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Abstract
The present invention discloses a kind of method for measuring tobacco-specific nitrosamine content in cigarette mainstream flue gas, comprising the following steps: the step of flue gas trapping, the preparation for extracting object, purification, standard reserving solution and standard working solution and ultra performance liquid chromatography-tandem mass spectrum measure.The present invention and traditional GC-TEA Comparison between detecting methods, are extracted, vortex oscillation using ammonium acetate, filter the mode of sample introduction, simplify pretreatment process, improve sensitivity for analysis.Compared with existing LC-MS/MS method, the present invention is significantly shorter than ultrasonic extraction or oscillation extraction with vortex oscillation method duration of oscillation, and extraction efficiency increases, and duration of oscillation shortens 6 times.The present invention has the advantages that easy to operate, quick, accurate, sensitivity and reproducible.
Description
Technical field
The invention belongs to cigarette smoke analysis technical fields, and in particular to the inspection of cigarette smoke harmful components, especially
The measuring method of peculiar TSNAs content in cigarette mainstream flue gas.
Background technique
The peculiar TSNAs of tobacco (TSNAs) mainly includes N- nitrosonornicotine (NNN), 4- (methyl TSNAs yl) -1- (3-
Pyridyl group) -1- butanone (NNK), N- nitroso anabasine (NAB) and N- nitrosoanabasine (NAT) etc..International cancer research
Mechanism (IARC), Hecht research team etc., in Canadian government list harmful components toxicity assessment the result shows that, and have foot
Enough cards are it is thought that the NNK in TSNAs has carcinogenicity to laboratory animal.In recent years, State Tobacco Monopoly Bureau organizes and implements
" cigarette harmfulness Research on Index System " project also indicates that, under the actual environment of cigarette smoke, 7 kinds maximum to body effect
In harmful chemical component index, NNK is one of them.
Currently, in cigarette mainstream flue gas the detection method of TSNAs mainly have gas-chromatography-thermal energy analytic approach (GC-TEA),
Gas chromatography mass spectrometry method (GC-MS) and Liquid Chromatography-Tandem Mass Spectrometry combination method (LC-MS/MS).GC-TEA method is recommended as CORESTA
The detection method of TSNAs in main flume, what is used is the most extensive.But the sample pretreatment process of GC-TEA method is complicated,
Selectivity is poor.Existing LC-MS/MS method the most popular generally chooses ammonium acetate aqueous solution extraction, then direct loading analysis,
Method is simple, but the measurement of Chinese style flue-cured tobacco type cigarette lower for TSNAs content is more difficult, and especially content is minimum
NAB, measurement are more difficult.
Summary of the invention
In consideration of it, that it is an object of that present invention to provide a kind of pre-treatments is relatively easy, sensitivity is higher, analysis is fireballing
TSNAs detection method of content, this method are exclusively used in TSNAs content in analysis cigarette mainstream flue gas.
In order to solve the above technical problems, technical solution provided by the invention is to provide in a kind of measurement cigarette mainstream flue gas
The method of tobacco-specific nitrosamine content, comprising the following steps:
Step a) flue gas trapping
It chooses glass fiber filter and traps cigarette mainstream flue gas；
Step b) extracts object
The filter disc for trapping main flume is put into extracting tube, extract liquor and internal standard is added, the first centrifuge tube is placed in the
One vortex oscillation instrument, vortex oscillation are stood；The extracting tube is centrifuge tube；
Step c) purification
Ceramics proton, magnesium sulfate and N- propyl ethylenediamine is added in the second centrifuge tube in Aspirate supernatant, by the second centrifugation
Pipe is placed in the second vortex oscillation instrument, vortex oscillation, centrifugation；Supernatant is filtered through organic phase filter membrane, and filtrate is to be measured；
The preparation of step d) standard reserving solution and standard working solution
TSNAs standard reserving solution is configured with methanol, is stored in Brown Glass Brown glass bottles and jars only, cryo-conservation；Measure stock solution first
Alcohol dilutes constant volume, and TSNAs working solution is made；
TSNAs-d4 internal standard stock solution is accurately configured with methanol, prepares internal standard working solution with internal standard stock solution, and be stored in
In Brown Glass Brown glass bottles and jars only；All stock solution cryo-conservations, restore it room temperature before use；
The TSNAs standard working solution of various concentration is prepared with extract liquor；
Step e) ultra performance liquid chromatography-tandem mass spectrum measurement
Draw the TSNAs standard working solution of prepared various concentration, inject UPLC-MS/MS system, by internal standard method with
Calculated by peak area goes out TSNAs content in sample prepare liquid.
An embodiment of the method for tobacco-specific nitrosamine content in cigarette mainstream flue gas, institute are measured according to the present invention
It states in step a), the filter disc diameter for trapping main flume is 44mm.
An embodiment of the method for tobacco-specific nitrosamine content in cigarette mainstream flue gas, institute are measured according to the present invention
It states in step b), the first centrifuge tube is 50mL, and extract liquor 15mL and 1 μ g/mL the mixing 150 μ L of internal standard of 100mmol/L is added；Institute
Stating extract liquor is ammonium acetate aqueous solution.
An embodiment of the method for tobacco-specific nitrosamine content in cigarette mainstream flue gas, institute are measured according to the present invention
It states in step b), the vortex oscillation time of the first vortex oscillation instrument is 5min, and vortex oscillation revolving speed is 2000 turns/min.
An embodiment of the method for tobacco-specific nitrosamine content in cigarette mainstream flue gas, institute are measured according to the present invention
It states in step c), the second centrifuge tube is 2mL, and the supernatant pipetted is 1mL, and ceramics two, proton, the anhydrous sulphur of addition is added
Sour magnesium and N- propyl ethylenediamine are respectively 150mg and 25mg.
An embodiment of the method for tobacco-specific nitrosamine content in cigarette mainstream flue gas, institute are measured according to the present invention
It states in step c), the vortex oscillation time of the second vortex concussion instrument is 2min, and vortex oscillation revolving speed is 2000 turns/min.
An embodiment of the method for tobacco-specific nitrosamine content in cigarette mainstream flue gas, institute are measured according to the present invention
It states in step c), centrifugation time 4min, centrifuge speed is 6000 turns/min.
An embodiment of the method for tobacco-specific nitrosamine content in cigarette mainstream flue gas, institute are measured according to the present invention
State step e) concrete operations are as follows: draw the TSNAs standard working solution of prepared various concentration, inject UPLC-MS/MS system
System, draws the equation of linear regression of TSNAs, is measured to the sample prepare liquid after purifying dilution, measures analyte and internal standard
The ratio of peak area substitutes into unary linear regression equation, acquires the content of analyte in sample prepare liquid.
An embodiment of the method for tobacco-specific nitrosamine content in cigarette mainstream flue gas, institute are measured according to the present invention
State in step d), the chromatographic condition of UPLC-MS/MS system: selection chromatographic column be C18, specification be 100mm × 2.1mm, 1.7 μm；
Mobile phase A: 0.1% formic acid water and Mobile phase B: methanol；Condition of gradient elution are as follows: 0~0.5min, 80%A~80%A；0.5~
1.0min, 80%A~10%A；1.0~2.9min, 10%A~10%A；2.9~3.5min, 10%A~80%A；3.51~
5.0min, 80%A~80%A；Flow rate of mobile phase is 0.6mL/min.
An embodiment of the method for tobacco-specific nitrosamine content in cigarette mainstream flue gas, institute are measured according to the present invention
It states in step d), the condition of tandem mass spectrum detection are as follows: electric spray ion source, spray voltage (IS) 3.0kV；Ionization temperature 450
℃；Atomization gas flow 800L/Hr；Taper hole throughput 50L/Hr；Collision gas is argon gas, flow 0.15ml/min；Remaining gas is
Nitrogen；Residence time is 100msec, cation MRM type collection.
Compared with prior art, a technical solution in above-mentioned technical proposal has the advantages that
1, it with traditional GC-TEA Comparison between detecting methods, is extracted using ammonium acetate, vortex oscillation, filters the mode of sample introduction,
Pretreatment process is simplified, sensitivity for analysis is improved.
2, compared with existing LC-MS/MS method, it is significantly shorter than ultrasonic extraction or oscillation with vortex oscillation method duration of oscillation
Extraction, extraction efficiency increase, and duration of oscillation shortens 6 times.
3, compared with existing LC-MS/MS method, dispersive solid-phase extraction purification main flume sample is had chosen, is conducive to
The measurement of the Virginian-type cigarette of low TSNAs content.
4, the present invention has chosen ultra performance liquid chromatography column, so that the separating degree of pillar significantly improves, analysis time is significant
Shorten, improves detection flux.Tandem mass spectrum uses the selectivity for making method and sensitivity to improve, and is more advantageous to smoker master
Flow the measurement of low content TSNAs in flue gas.
5, it is designated as deuterated internal standard in use of the present invention, using deuterated interior scalar quantity, effectively eliminates matrix interference and pre-treatment
Caused error in the process.
6, the present invention has the advantages that easy to operate, quick, accurate, sensitivity and reproducible.
Detailed description of the invention
Fig. 1 is the selection ion stream chromatogram that oscillation extraction-LC-MS/MS method detects TSNAs in No. 1 flue-cured tobacco sample.
Fig. 2 is the selection ion stream chromatogram of TSNAs in the present invention No. 1 flue-cured tobacco sample of detection.
Specific embodiment
It is described further below in conjunction with specific example.
The present embodiment instrument and reagent are as follows: the Waters Xevo TQ ultra performance liquid chromatography-tandem mass spectrometer (U.S.
Waters company), it is equipped with electrospray ionisation source (ESI)；VtexMixer 230VeU oscillator (Labnet company, the U.S.).
Formic acid is HPLC grades (concentration 49-51%, German Sigma company)；Acetonitrile, methanol are the chromatographically pure (U.S.
Thermo-Fisher company)；TSNAs, TSNAs-d4(purity: 98%；Isotopic purity: 99%, Toronto Research
Chemicals Inc.), water is ultrapure water.
The present invention uses ammonium acetate aqueous solution for extract liquor, vortex oscillation extraction, the purification of matrix dispersion extraction, deuterated internal standard
It is quantitative, UPLC-MS/MS measurement and etc. TSNAs in main flume is measured, can quickly, it is accurate, detect mainstream simultaneously
The content of 4 kinds of TSNAs in flue gas, i.e. N- nitrosonornicotine (NNN), 4- (methyl TSNAs yl) -1- (3- pyridyl group) -1- fourth
The content of ketone (NNK), N- nitroso anabasine (NAB) and N- nitrosoanabasine (NAT).
1, main flume traps
Sample cigarette is chosen according to " cigarette: sampling " (ISO 8243:2006), according to " tobacco and tobacco product are adjusted
With test atmosphere " (ISO 3402:1999) Lai Pingheng cigarette；Using " conventional analysis cigarette smoking machine definition and standard bar
Part " (ISO 3308:2000) trap cigarette mainstream flue gas.
2, the analyte in main flume is extracted
The filter disc for trapping cigarette mainstream flue gas is taken, 50mL tool plug centrifuge tube is put into, 15mL 100mmol/L acetic acid is added
Ammonium extract liquor, and the deuterated mixing internal standard of 150 μ L, 1 μ g/mL is added, vortex oscillation 5min under conditions of 2000 revs/min takes
In 2mL spiral cover centrifuge tube 150mg anhydrous magnesium sulfate and 25mgPSA is added, under conditions of 2000 revs/min in 1mL supernatant
Vortex oscillation 2min is centrifuged 4min under conditions of 6000 revs/min.Supernatant crosses 0.22 μm of organic phase filter membrane, takes 5 μ L filtrates
Introduce LC-MS/MS separation analysis.
3, UPLC-MS/MS is measured
(1) UPLC-MS/MS condition:
Chromatographic condition: Atiantis UPLC BEH C18 (100mm × 2.1mm, 1.7 μm, Waters, US)；Stream
Dynamic phase A:0.1% formic acid water and Mobile phase B: methanol；Condition of gradient elution are as follows: 0~0.5min, 80%A~80%A；0.5~
1.0min, 80%A~10%A；1.0~2.9min, 10%A~10%A；2.9~3.5min, 10%A~80%A；3.51~
5.0min, 80%A~80%A；Flow rate of mobile phase is 0.6mL/min.
Mass Spectrometry Conditions: electric spray ion source, spray voltage (IS) 3.0kV；450 DEG C of ionization temperature；Atomization gas flow
800L/Hr；Taper hole gas (cone) flow 50L/Hr；Collision gas flow is 0.15ml/min；Collision gas is argon gas, and remaining gas is
Nitrogen；Residence time is 100msec, and cation MRM type collection, monitors ion pair and its corresponding collision energy (CE) is shown in Table
1。
The peculiar TSNAs of the lower four kinds of tobaccos of 1 multiple-reaction monitoring pattern of table and its deuterated interior target part mass spectrometry parameters
* quota ion pair.
(2) preparation of standard reserving solution
The preparation of stock solution and working solution: accurately preparing 11.00 μ g/mL NNN, 11.20 μ g/mL NNK with methanol,
10.14 μ g/mL NAB, 5.00 μ g/mL NAT standard reserving solutions are stored in Brown Glass Brown glass bottles and jars only, -20 DEG C of preservations.Measure eachization
It closes object stock solution to be mixed, preparation obtains 1 μ g/mL TSNAs mixed standard solution.
100 μ g/mL NNN-d are prepared with methanol4, 50 μ g/mL NAT-d4, 100 μ g/mL NAB-d4With 250 μ g/mL
NNK-d4Internal standard stock solution, be stored in Brown Glass Brown glass bottles and jars only, -20 DEG C preservation.Each internal standard stock solution accurately measured, after mixing
It is made into 1 μ g/mL mixing inner mark solution.
(3) measurement of TSNAs content:
Each 5 μ L of hybrid standard working solution of the TSNAs of prepared various concentration is drawn, UPLC-MS/MS is injected；
The equation of linear regression of TSNAs is shown in Table 2, and y represents the ratio of analyte Yu internal standard peak area in equation, and x is indicated in main flume
The concentration of target analytes.Same method detects actual sample, acquires the content of TSNAs in actual sample.
(4) range of linearity and detection limit of this method
The present embodiment pipettes 1 μ g/mL standard reserving solution 0 μ L, 10 μ L with blank flue-cured tobacco substrate preparation standard curve respectively,
For 20 μ L, 50 μ L, 100 μ L, 200 μ L, 500 μ L and 800 μ L in 8 10mL brown volumetric flasks, each volumetric flask moves into 100 μ L 1
The deuterated mixing internal standard working solution of μ g/mL, with methanol constant volume to 10mL.The concentration of each standard working solution is respectively 0ng/mL,
1ng/mL, 2ng/mL, 5ng/mL, 10ng/mL, 20ng/mL, 50ng/mL and 80ng/mL.To each standard specimen peak area and interior target
The ratio (y) of peak area and its concentration (x) carry out linear regression analysis, obtain standard curve, the results are shown in Table 2.Various compounds
Good (the correlation coefficient r of linear relationship2>=0.99) needs of quantitative analysis, be can satisfy.The inspection of method is determined with 3 times of signal-to-noise ratio
Rising limit, see Table 2 for details.
The range of linearity, related coefficient, detection limit and the retention time of 2 TSNAs of table
(5) repeatability and recovery of standard addition of the method for the present invention:
A certain amount of TSNAs standard solution is added during main flume sample extraction, is then extracted, is measured, calculates
The rate of recovery.This experiment selects the recovery testu of high, medium and low 3 kinds of various concentrations to investigate the accuracy of method, in addition to lower
The rate of recovery of the NAB of content when additional amount is 10.1ng be except 82.5%, the rate of recovery of other points all 90%-95% it
Between.The precision of method is evaluated with the relative standard deviation (RSD) of the rate of recovery, is measured in parallel 5 times to same sample, 3 kinds of changes
The RSD range for closing the object rate of recovery is 4.9%~9.8%, the results are shown in Table 3.
The rate of recovery of TSNAs and precision (n=5) in 3 main flume of table
(6) the method for the present invention is compared with traditional ultrasonic extraction method:
The TSNAs of traditional LC-MS/MS measurement main flume mainly chooses cyclotron oscillation or ultrasonic extraction 30min,
We have chosen four samples, and two fire-cured tobacco type samples, two mixed type samples, box mark tar content range is 3mg-11mg, point
It is not compared with traditional ultrasonic extraction method and vortex oscillation Dispersive solid phase extraction method of the invention, each sample
Measurement 6
It is a parallel, show that NNN, NNK, NAB and the NAT related coefficient of two methods are respectively 0.983 by regression analysis,
0.930,0.835 and 0.996, four indexs are all significant related (P < 0.001), and measurement result is shown in Table 4, the correlation of two methods
Analysis the results are shown in Table 5.Oscillation extraction-measurement LC-MS/MS measure the selection of TSNAs in No. 1 Virginian-type cigarette main flume from
Subflow chromatogram is as shown in Figure 1, using the selection ion stream color of the TSNAs of this method processing measurement main flume in same sample
Spectrogram as shown in Fig. 2, it can be seen from the figure that the present invention since simple purifying step is added after, the response of target analytes
Enhancing, chaff interferent are substantially reduced.Table 4 measures the inspection of four kinds of cigarette using the LC-MS/MS method and the method for the present invention of oscillation extraction
Measured data
Note: A, B are Virginian-type cigarette, and C, D are blended type cigarette.
The regression analysis of table 5 oscillation extraction-LC-MS/MS method and the method for the present invention determination data
The above is only the preferred embodiment of the present invention, it is noted that above-mentioned preferred embodiment is not construed as pair
Limitation of the invention, protection scope of the present invention should be defined by the scope defined by the claims..For the art
For those of ordinary skill, without departing from the spirit and scope of the present invention, several improvements and modifications can also be made, these change
It also should be regarded as protection scope of the present invention into retouching.
Claims (8)
1. a kind of method of TSNAs content in measurement cigarette mainstream flue gas, the TSNAs includes N- nitrosonornicotine, 4-(first
Base TSNAs yl) -1-(3- pyridyl group) -1- butanone, N- nitroso anabasine and N- nitrosoanabasine, which is characterized in that packet
Include following steps:
Step a) flue gas trapping
It chooses glass fiber filter and traps cigarette mainstream flue gas；
Step b) extracts object
The filter disc for trapping main flume is put into extracting tube, extract liquor and internal standard is added, the first centrifuge tube is placed in the first whirlpool
Shaker is revolved, vortex oscillation is stood；The extracting tube is centrifuge tube；The extract liquor is ammonium acetate aqueous solution；
Step c) purification
Aspirate supernatant is added ceramics proton, magnesium sulfate and N- propyl ethylenediamine, the second centrifuge tube is set in the second centrifuge tube
In the second vortex oscillation instrument, vortex oscillation, centrifugation；Supernatant is filtered through organic phase filter membrane, and filtrate is to be measured；
The preparation of step d) standard reserving solution and standard working solution
TSNAs standard reserving solution is configured with methanol, is stored in Brown Glass Brown glass bottles and jars only, -20 DEG C of preservations；It is dilute to measure stock solution methanol
Constant volume is released, TSNAs working solution is made；
TSNAs-d is accurately configured with methanol4Internal standard stock solution prepares internal standard working solution with internal standard stock solution, and is stored in brown glass
In glass bottle；- 20 DEG C of stock solution all preservations, restore it room temperature before use；
The TSNAs standard working solution of various concentration is prepared with extract liquor；
Step e) ultra performance liquid chromatography-tandem mass spectrum measurement
The TSNAs standard working solution of prepared various concentration is drawn, UPLC-MS/MS system is injected, by internal standard method with peak face
Product calculates TSNAs content in sample prepare liquid；
The chromatographic condition of UPLC-MS/MS system: selection chromatographic column be Atiantis UPLC BEH C18, specification be 100 mm ×
2.1mm, 1.7 μm；Mobile phase A: 0.1% formic acid water and Mobile phase B: methanol；Condition of gradient elution are as follows: 0 ~ 0.5min, 80%A ~ 80%
A；0.5 ~ 1.0min, 80%A ~ 10%A；1.0 ~ 2.9min, 10%A ~ 10%A；2.9 ~ 3.5min, 10%A ~ 80%A；3.51 ~ 5.0min,
80%A~80%A；Flow rate of mobile phase is 0.6 mL/min；
The condition of tandem mass spectrum detection are as follows: electric spray ion source, spray voltage 3.0kV；450 DEG C of ionization temperature；Atomization air flow
Measure 800L/Hr；Taper hole throughput 50L/Hr；Collision gas is argon gas, flow 0.15ml/min；Remaining gas is nitrogen；When resident
Between be 100msec, cation MRM type collection.
2. the method for TSNAs content in measurement cigarette mainstream flue gas according to claim 1, which is characterized in that the step
It is rapid a) in, trap main flume filter disc diameter be 44 mm.
3. the method for TSNAs content in measurement cigarette mainstream flue gas according to claim 1, which is characterized in that the step
It is rapid b) in, the first centrifuge tube be 50mL, be added 100mmol/L extract liquor 15mL and 1 μ g/mL mixing 150 μ L of internal standard.
4. the method for TSNAs content in measurement cigarette mainstream flue gas according to claim 1 or 2, in the step b), institute
The vortex oscillation time for stating the first vortex oscillation instrument is 5min, and vortex oscillation revolving speed is 2000 turns/min.
5. the method for TSNAs content in measurement cigarette mainstream flue gas according to claim 1, in the step c), second
Centrifuge tube is 2 mL, and the supernatant pipetted is 1mL, and ceramics two, proton, the anhydrous magnesium sulfate and N- propyl second of addition is added
Diamines is respectively 150mg and 25mg.
6. the method for measuring TSNAs content in cigarette mainstream flue gas according to claim 1 or 5, in the step c), institute
The vortex oscillation time for stating the second vortex concussion instrument is 2min, and vortex oscillation revolving speed is 2000 turns/min.
7. the method for measuring TSNAs content in cigarette mainstream flue gas according to claim 1 or 5, in the step c), from
The heart time is 4min, and centrifuge speed is 6000 turns/min.
8. the method for TSNAs content, the step e) concrete operations in measurement cigarette mainstream flue gas according to claim 1
Are as follows: the TSNAs standard working solution of prepared various concentration is drawn, UPLC-MS/MS system is injected, draws the linear of TSNAs
Regression equation is measured the sample prepare liquid after purifying dilution, measures the ratio of analyte Yu internal standard peak area, substitutes into one
First equation of linear regression acquires the content of analyte in sample prepare liquid.
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| CN109975447A (en) * | 2017-12-28 | 2019-07-05 | 贵州中烟工业有限责任公司 | The measuring method of Alkaloid and nitrosamine in a kind of cigarette filter |
| CN109975444A (en) * | 2017-12-28 | 2019-07-05 | 贵州中烟工业有限责任公司 | The measuring method of Alkaloid and nitrosamine in a kind of buccal cigarette |
| CN109781875A (en) * | 2019-01-11 | 2019-05-21 | 云南中烟工业有限责任公司 | A method of utilizing TSNAs in the Soxhlet extraction device detection smoker urine with Solid Phase Extraction function |
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| CN103293245B (en) * | 2013-06-08 | 2015-02-18 | 国家烟草质量监督检验中心 | GC-MS (Gas Chromatography-Mass Spectrometer)/MS (Mass Spectrometer) method for simultaneously analyzing four tobacco-specific nitrosamines (TSNAs) in main stream smoke of cigarette |
| CN104749310B (en) * | 2015-04-13 | 2016-06-29 | 中国烟草总公司四川省公司 | A kind of measure the method for content of nitrosamines in cigarette filter |
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