CN106918663A - The efficient liquid phase tandem mass spectrum detection method of bactericide interception in cigarette mainstream flue gas - Google Patents
The efficient liquid phase tandem mass spectrum detection method of bactericide interception in cigarette mainstream flue gas Download PDFInfo
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- G01N30/02—Column chromatography
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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
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Abstract
The invention discloses a kind of efficient liquid phase tandem mass spectrum detection method of bactericide interception in cigarette mainstream flue gas, comprise the following steps：(1) cigarette is aspirated, mainstream smoke total particulate matter is trapped with cambridge filter；(2) it is put into centrifuge tube after cambridge filter is shredded, adds acetonitrile and internal standard solution, vibration makes infiltration；(3) SPE reagent, centrifugation after vibration are added；(4) take supernatant liquor to purify centrifuge tube in, centrifugation after vibration；(5) supernatant liquor is taken to be analyzed using efficient liquid phase tandem mass spectrometry；Condition is：Chromatographic column：C18 liquid-phase chromatographic analysis posts；Column temperature：25℃；Sample size：10μL；Flowing phase composition is that the gradient mixture of water and acetonitrile, flow velocity are 200uL/min；Scan mode：Cation is scanned；Monitoring mode：Multiple-reaction monitoring；Electron spray voltage：5500V；Atomization gas pressure：0.414MPa；Ion source temperature：500℃.
Description
Technical field
The invention belongs to technical field of tobacco chemical analysis, bactericide interception in one cigarette mainstream flue gas of specific offer
Efficient liquid phase-tandem mass spectrum detection method.
Background technology
Bactericide is the class agricultural chemicals for preventing and treating the plant disease caused by various pathogenic microorganisms, is referred generally to antifungal
Agent.But in the world, typically as the general name of the medicament for preventing and treating all kinds of pathogenic microorganisms.Come from the angle of control crop disease
Say, the total demand that current bactericide has the irreplaceable effect of other materials, bactericide is continuing to increase, global bactericide
Growth rate reaches nearly 8%, and triazole bactericidal agent will be leading role.Bitten to prevent tobacco leaf from being invaded for pest and disease damage, it is ensured that tobacco leaf is produced
Amount, bactericide has also inevitably been used in the planting process of tobacco leaf.
At present, the problem of tobacco Pesticide Residues has increasingly caused the concern of tobacco circle and the whole society.Tobacco conduct
A kind of special consumer goods, are to enter human consumption after cigarette is burnt and to form flue gas, and the agricultural chemicals in this process pipe tobacco is residual
Stay and be transferred in flue gas with certain mobility.Therefore, cigarette smoke is judged with the Pesticide Residue in tobacco leaf merely
Residues of pesticides security be inaccurate, it is necessary to clear and definite tobacco leaf Pesticide Residues are to the migration situation in main flume, ability
The more security of accurate evaluation cigarette smoke residues of pesticides.Therefore, bactericide migration amount in a kind of cigarette mainstream flue gas is set up
Detection method, to bactericide during research cigarette smoking to the migration amount and mobility important in inhibiting in main flume.
At present, the common assay method of the bactericide that is used in tobacco has gas chromatography, liquid chromatography or gas
Matter, gas-chromatography electron capture detector and mass spectrometry detection method, gas chromatographic flame photometric detector detection method, liquid matter connection
Usage etc., but evaluate accuracy have much room for improvement.
The content of the invention
The present invention traps Smoke Particulate using cambridge filter, is purified through Dispersive solid phase extraction, with superelevation liquid phase color
Spectrum-tandem mass spectrum combination method determines the migration amount of bactericide in Smoke Particulate.Through literature search, do not find and present invention
The open report of same document.
It is an object of the invention to provide a kind of detection method of bactericide migration amount in cigarette mainstream smoke total particulate matter,
To study tobacco leaf Pesticide Residues to the migration situation in total particulate matter in mainstream smoke.
Efficient liquid phase-tandem mass spectrum detection side that bactericide interception in a kind of cigarette mainstream flue gas is provided of the invention
Method, comprises the following steps：
(1) cigarette is aspirated on smoking machine, mainstream smoke total particulate matter is trapped with cambridge filter；
(2) cambridge filter of step (1) is removed, is put into centrifuge tube after cambridge filter is shredded, add acetonitrile and internal standard
Liquid, vibration makes to sample to infiltrate；
(3) SPE reagent, centrifugation after vibration are added；
(4) take step (3) centrifugation after supernatant liquor to purify centrifuge tube in, centrifugation after vibration；
(5) supernatant liquor after step (4) centrifugation is taken to be analyzed using efficient liquid phase-tandem mass spectrometry；
(6) condition of step (5) efficient liquid phase-tandem mass spectrum is：Chromatographic column：C18 liquid-phase chromatographic analysis posts；Post
Temperature：25℃；Sample size：10μL；Flowing phase composition is that the gradient mixture of water and acetonitrile, flow velocity are 200uL/min；Scanning side
Formula：Cation is scanned；Monitoring mode：Multiple-reaction monitoring；Electron spray voltage：5500V；Atomization gas pressure：0.414MPa；Ion gun
Temperature：500℃.
Preferably, the internal standard solution described in step (2) is the EPTC methanol solution of 1ug/1000mL.
Preferably, the frequency 2500r/min of step (2), (3) and (4) described vibration, the time is 6min.
Preferably, step (3) and the rotating speed of (4) described centrifugation are 4000r/min, and centrifugation time is 10min.
Preferably, step (3) the SPE reagent is that mass ratio is 2:1:8:2 sodium citrate, hydrogen citrate two
The mixture of sodium, anhydrous magnesium sulfate and sodium chloride.
Preferably, it is 1 to contain mass ratio in step (4) the purification centrifuge tube:1:2 N- propyl group ethylenediamine, graphitization
Carbon and anhydrous slufuric acid magnesium compound.
Preferably, the gradient mixture of step (6) water and acetonitrile is volume ratio 90:10,50:50,50:50,40:
60,20:80,5:95,5:98,90:10,90:10.
The advantage of the invention is that：The extract solution of the TPM on cambridge filter is purified with dispersive solid-phase extraction, is used
Efficient liquid phase-tandem mass spectrometry is analyzed, and realizes the detection of bactericide migration amount in smoke's total particulate matter.So as to be to investigate not
With cigarette, bactericide lays the first stone to the migration amount and mobility in main flume in combustion.The accuracy of evaluation is
Improve.
Brief description of the drawings
Nothing.
Specific embodiment：
The efficient liquid phase of bactericide interception-tandem mass spectrum detection method in cigarette mainstream flue gas of the invention, specific step
It is rapid as follows：
A. cigarette to be measured is loaded onto on smoking machine, is defined and is marked with smoking machine according to GB/T 16450-2004 conventional analyses
Floating screed part, arrange parameter (pumping volume：35ml, puff duration：2s, suction period：60s), 20 cigarette are aspirated altogether, are used
Cambridge filter traps mainstream smoke total particulate matter；
B. after cigarette smoking is finished, removing trapping has the cambridge filter of mainstream smoke total particulate matter, and is torn up, and is put into
In 50mL centrifuge tubes, plus acetonitrile 15mL, 100uL internal standard solution, 2500r/min vibrates 6min and is fully infiltrated by acetonitrile to sample；
C. add SPE reagent, SPE reagent be 1.0g sodium citrates, 0.5g DisodiumHydrogen Citrates, 4.0g without
Water magnesium sulfate, 1.0g sodium chloride；2500r/min vibrates, and 6min is sufficiently mixed rear 4000r/m centrifugations 10min；
D. centrifuged supernatant 2mL is pipetted into purifying centrifuge tube (U.S. Agilent Products), is contained in purification centrifuge tube
The N- propyl group ethylenediamine of 50mg, 50mg graphitized carbons, 100mg anhydrous magnesium sulfates.2500r/min vibrates 6min, then 4000r/m
Centrifugation 10min, takes supernatant 1mL through 0.22 μm of membrane filtration, is divided using superelevation Liquid Chromatography-Tandem Mass Spectrometry afterwards
Analysis.
E. the condition of efficient liquid phase-tandem mass spectrum is：Chromatographic column：C18 liquid-phase chromatographic analysis posts；Column temperature：25℃；Sample introduction
Amount：10μL；Flowing phase composition is that the gradient mixture of water and acetonitrile, flow velocity are 200uL/min；Scan mode：Cation is scanned；
Monitoring mode：Multiple-reaction monitoring；Electron spray voltage：5500V；Atomization gas pressure：0.414MPa；Ion source temperature：500℃.
1st, instrument and reagent
Waters Acquity UPLC Ultra Performance Liquid Chromatography instruments (Waters, US), AB 3200QTrap connect
Mass spectrograph (American AB Sciex companies), Talboys multitube vortexs mixed instrument (Talboys companies of the U.S.), Millipore is ultrapure
Water dispenser (Millipore companies of the U.S.), the desk centrifuges of Eppendorf 5804 (German Eppendorf companies).Acetonitrile, first
Alcohol：Chromatographic grade, purchased from Tiade companies of the U.S.；Pesticide standard material EPTC, as internal standard substance, purity >=95%：It is purchased from
Dr.Ehrenstorfer companies；Dispersive solid phase extraction kit：Extracts reagent includes 1.0g sodium citrates, 0.5g lemons
Sour disodium hydrogen, 4.0g anhydrous magnesium sulfates, 1.0g sodium chloride；N- propyl group ethylenediamine, 50mg graphitization of the purification centrifuge tube containing 50mg
Carbon, 100mg anhydrous magnesium sulfates are purchased from Agilent companies of the U.S..
2. specific experiment step
By commercial cigarettes to be measured, the air of the tobacco specified in GB/T 16447-2004 and tobacco product regulation and test
Balance 48h under environmental condition, it is sorted after, with the smoking machine for meeting the requirements of ISO 30008, in conventional analysis smoking machine standard
Aspirated under condition (1 mouthful/minute, 2 seconds/mouthful, 35.0mL/ mouthfuls).After cigarette smoking is finished, removing trapping has the total grain phase of main flume
The cambridge filter of thing, and torn up to 0.5cm long, 0.2cm wide, it is put into 50mL centrifuge tubes, plus acetonitrile 30mL, in 100uL
Standard liquid, 2500r/min vibration 6min to sample are fully infiltrated by acetonitrile, extract.
Purified with SPE reagent.Add SPE reagent to be sufficiently mixed (to be placed on whirlpool mixing shaker
6min is vibrated with 2500r/min), 10min is then centrifuged with 4000r/min；Centrifuged supernatant 2mL is pipetted to purifying centrifuge tube
In, in 6min is vibrated with 2500r/min on whirlpool mixing shaker, 10min is then centrifuged with 4000r/m, take supernatant 1mL warps
0.22 μm of membrane filtration, obtains liquid to be detected.
3rd, condition determination
--- chromatographic column：C-sC18 liquid-phase chromatographic analysis post (column length 150mm, internal diameter 2.1.i mm, fixing phase particle diameter 3p μ
M) or quite person；
--- column temperature：25℃；
--- sample size：10uμL；
--- flowing phase composition, flow velocity and graded, it is shown in Table 1；
--- scan mode：Cation is scanned；
--- monitoring mode：Multiple-reaction monitoring；
--- electron spray voltage：5 500V；
--- atomization gas pressure：0.414MPa；
--- ion source temperature：500℃；
The liquid chromatogram mobile phase of table 1 composition, flow velocity and graded
| Time (min) | Flow velocity (uL/min) | Water (%) | Acetonitrile (%) |
| 0.00 | 200 | 90 | 10 |
| 1.00 | 200 | 50 | 50 |
| 5.00 | 200 | 50 | 50 |
| 16.00 | 200 | 40 | 60 |
| 25.00 | 200 | 20 | 80 |
| 30.00 | 200 | 5 | 95 |
| 40.00 | 200 | 5 | 98 |
| 40.01 | 200 | 90 | 10 |
| 45.00 | 200 | 90 | 10 |
Standard working curve makes
The Tandem Mass Spectrometry Analysis of high performance liquid chromatography one are carried out to standard working solution, obtain each agricultural chemicals target compound with
The ratio between interior target peak area and the ratio between concentration, check whether the response of mass detector is linear by linear fit.Work as phase
Close coefficients R2>=0.99, can be using the hybrid standard working curve of single level.Single horizontal hybrid standard working curve should
Made using the hybrid standard working solution of intermediate concentration.
Experiment every time all should make hybrid standard working curve, per sample introduction 10 times after should add a mixing for intermediate concentration
Standard working solution, if measured value differs by more than 10% with initial value, should re-start the making of hybrid standard working curve.
Sample determination
Sample is analyzed, measured value is calculated by standard working curve according to internal standard method.It is parallel to carry out sample twice
Product are determined, using the average value of parallel determinations twice as final measurement result.Parallel determinations is relatively average twice
Deviation should be less than 10%.
Embodiment 1
Commercially available domestic cigarette sample is chosen, bactericide in cigarette mainstream smoke total particulate matter is carried out according to above-mentioned method of testing
The measure of migration amount, the results are shown in Table 1.In cigarette mainstream smoke total particulate matter no detection thiophanate-methyl, carbendazim, Propamocarb,
The Fungicide residues such as dimethachlon.Wherein：The rejection (wt%) of filter tip=(residual in pipe tobacco before interception/cigarette smoking in filter tip
Allowance) × 100wt%.
Bactericide migration amount testing result in the cigarette mainstream smoke total particulate matter of table 1
Note：In table/represent do not detect.
Embodiment 2
Due to not detecting above-mentioned bactericide in commercial cigarettes mainstream smoke total particulate matter, using additional injection various concentrations
Bactericide (thiophanate-methyl, carbendazim and Propamocarb), injects 1ug/20 branch, 4ug/20 branch, 20ug/20 branch and 80ug/ respectively
20 in cigarette, according to above-mentioned method of testing to thiophanate-methyl, carbendazim in cigarette mainstream smoke total particulate matter after suction
It is measured with Propamocarb.
Result shows：The thiophanate-methyl amount in cigarette is applied in 1.0ug/20 branch and 4.0ug/20 branch, in cigarette
Thiophanate-methyl and its metabolin carbendazim are not detected by total particulate matter in mainstream smoke；It is applied to the thiophanate-methyl amount in cigarette
In 20ug/20 branch and 80ug/20 branch, trimethyl thiophanate is detected in cigarette mainstream smoke condensate and its metabolin is more
Bacterium spirit, and with the migration amount for increasing thiophanate-methyl and its metabolin carbendazim in Smoke Particulate, the migration of outer dosage
Rate is raised.
The Propamocarb amount in cigarette is applied in 1.0ug/20 branch and 4.0ug/20 branch, in cigarette mainstream smoke condensate
In be not detected by Propamocarb；The Propamocarb amount in cigarette is applied in 20ug/20 branch and 80ug/20 branch, in cigarette main flue
Propamocarb is detected in gas granule phase substance, and with Propamocarb migration amount, mobility liter in the increase Smoke Particulate of outer dosage
It is high.The results are shown in Table 2.Wherein：The rejection (wt%) of filter tip=(in filter tip before interception/cigarette smoking in pipe tobacco residual quantity) ×
100wt%.
Therefore the method can be used to detect the content of bactericide in cigarette mainstream smoke condensate.
Migration amount/rate testing result after the additional thiophanate-methyl of table 2 and Propamocarb in cigarette granule phase substance
Note：In table/represent do not detect.
Claims (7)
1. in a kind of cigarette mainstream flue gas bactericide interception efficient liquid phase-tandem mass spectrum detection method, it is characterised in that bag
Include following steps：
(1) cigarette is aspirated on smoking machine, mainstream smoke total particulate matter is trapped with cambridge filter；
(2) cambridge filter of step (1) is removed, is put into centrifuge tube after cambridge filter is shredded, add acetonitrile and internal standard solution, shaken
Swinging makes to sample to infiltrate；
(3) SPE reagent, centrifugation after vibration are added；
(4) take step (3) centrifugation after supernatant liquor to purify centrifuge tube in, centrifugation after vibration；
(5) supernatant liquor after step (4) centrifugation is taken to be analyzed using efficient liquid phase-tandem mass spectrometry；
(6) condition of step (5) efficient liquid phase-tandem mass spectrum is：Chromatographic column：C18 liquid-phase chromatographic analysis posts；Column temperature：25
℃；Sample size：10μL；Flowing phase composition is that the gradient mixture of water and acetonitrile, flow velocity are 200uL/min；Scan mode：Just from
Son scanning；Monitoring mode：Multiple-reaction monitoring；Electron spray voltage：5500V；Atomization gas pressure：0.414MPa；Ion source temperature：
500℃。
2. method according to claim 1, it is characterised in that the internal standard solution described in step (2) is the EPTC of 1ug/1000mL
Methanol solution.
3. method according to claim 1, it is characterised in that the frequency 2500r/min of step (2), (3) and (4) described vibration,
Time is 6min.
4. method according to claim 1, it is characterised in that step (3) and the rotating speed of (4) described centrifugation are 4000r/
Min, centrifugation time is 10min.
5. method according to claim 1, it is characterised in that step (3) the SPE reagent is that mass ratio is 2:1:8:2
Sodium citrate, DisodiumHydrogen Citrate, the mixture of anhydrous magnesium sulfate and sodium chloride.
6. method according to claim 1, it is characterised in that containing mass ratio be 1 in step (4) the purification centrifuge tube:1:2
N- propyl group ethylenediamine, graphitized carbon and anhydrous slufuric acid magnesium compound.
7. method according to claim 1, it is characterised in that the gradient mixture of step (6) water and acetonitrile is volume ratio
90:10,50:50,50:50,40:60,20:80,5:95,5:98,90:10,90:10.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113984467A (en) * | 2021-10-20 | 2022-01-28 | 国家烟草质量监督检验中心 | Preparation method of aerosol trapping material of tobacco product, obtained aerosol trapping material and application thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113984467A (en) * | 2021-10-20 | 2022-01-28 | 国家烟草质量监督检验中心 | Preparation method of aerosol trapping material of tobacco product, obtained aerosol trapping material and application thereof |
| CN113984467B (en) * | 2021-10-20 | 2024-02-09 | 国家烟草质量监督检验中心 | Preparation method of tobacco product aerosol trapping object, obtained aerosol trapping object and application thereof |
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Application publication date: 20170704 |