CN102507773B - Method for selectively determining residual vinyl acetate in white latex for cigarette through static headspace gas and chromatography mass spectrometry - Google Patents
Method for selectively determining residual vinyl acetate in white latex for cigarette through static headspace gas and chromatography mass spectrometry Download PDFInfo
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Abstract
The invention relates to a method for selectively determining residual vinyl acetate in white latex for cigarette through static headspace and gas chromatography mass spectrometry, belonging to the technical field of physical and chemical inspection of materials for the cigarette, and provides a quantitative selected ion determining method through the static headspace and gas chromatography mass spectrometry, aiming at selectively determining the residual vinyl acetate in white latex for the cigarette. A sample of the white latex for the cigarette after static headspace at 80 DEG C for 15 minutes is detected by taking 2-hexanone as an internal standard through HP-INNOWAX column in a GC-MS/SIM (Gas Chromatography Mass Spectrometry/Selected Ion Monitoring) mode, and is quantified through an internal standard method. According to the method for selectively determining the residual vinyl acetate in the white latex for the cigarette through the static headspace gas chromatography mass spectrometry, disclosed by the invention, detection limit, labeling recovery ratio and RSD (Relative Standard Deviation) of the method are respectively 0.63mg/kg, 104-107% and 2.5-4.9%; in addition, the method disclosed by the invention has the characteristics of simpleness, fastness, accuracy, sensitiveness and the like, and is especially suitable for quantitative analysis on the residual vinyl acetate in the white latex for the cigarette.
Description
Technical field
The method that the present invention relates to a kind of Static Headspace-gaschromatographic mass spectrometry selective determination cigarette residual vinyl acetate in white latex, belongs to the physical and chemical inspection technical field of rolling up smoking material.
Background technology
At present, the tackifier using in domestic production of cigarettes is taking vinyl acetate as the synthetic a kind of thermoplasticity white glue with vinyl of primary raw material mostly, wherein residual vinyl acetate monomer had both been unfavorable for the stability of emulsion, can bring being an unpleasant jar to nerves property smell to product again, thereby have a strong impact on the aesthetic quality of cigarette product, international cancer research association has been classified as 2B class carcinogen.Therefore, analyze and monitor cigarette, with vinyl acetate residual in white glue with vinyl, the security of sucking of cigarette is had to important meaning.Cigarette mainly contains Near-Infrared Absorption Method, titrimetry, iodimetric titration etc. with the residual traditional analysis of vinyl acetate in white glue with vinyl, but is subject to the restriction of its preci-sion and accuracy, and these methods can not meet the needs of analysis.Some new methods are just attempted for relevant analysis and research as head space-gas chromatography and By Gas Chromatography-mass Spectrometry.Static Headspace is analyzed (static headspace, SHS) be a kind of method that the head space gas of liquid or solid sample in the closed container in reaching balance is analyzed, it is directly got head space gas the volatile ingredient in sample is analyzed, without complicated sample pretreatment process, can effectively get rid of sample substrate to the interference of analyzing, mensuration process is easy, quick, is widely applied in recent years at multiple analysis fields such as food security, medicine analysis, industrial products.The present invention is the deficiency with vinyl acetate residue analysis method in white glue with vinyl to existing cigarette, by SHS and gas chromatography-mass spectrum (GC-MS) combination, to set up a kind of easy, accurate, fast detecting cigarette residual SHS-GC-MS method of vinyl acetate in glue.
Summary of the invention
The object of this invention is to provide the method for a kind of Static Headspace-gaschromatographic mass spectrometry selective determination cigarette residual vinyl acetate in white latex.The present invention is directed to the deficiency of existing cigarette residual vinyl acetate in white latex analytical approach, by Static Headspace SHS and gaschromatographic mass spectrometry (GC/MS) combination, set up a kind of easy, accurate, fast selective and detect the SHS-GC/MS method of cigarette residual vinyl acetate in white latex.
The method of residual vinyl acetate in white latex for Static Headspace-gaschromatographic mass spectrometry selective determination cigarette of the present invention, taking methyl-n-butyl ketone as internal standard compound, adopt Static Headspace balance, gas chromatography-mass spectrum choice ion pattern to measure the content of cigarette residual vinyl acetate in white latex, wherein, gas chromatography adopts HP-INNOWAX chromatographic column, and assay adopts inner mark method ration.
The method of residual vinyl acetate in white latex for described Static Headspace-gaschromatographic mass spectrometry selective determination cigarette, specifically comprises the steps:
(1) preparation of vinyl acetate standard solution: accurately take the pure material of vinyl acetate, be made into standard solution with DMF;
(2) be added with the preparation of interior target matrix correction agent: accurately take internal standard compound methyl-n-butyl ketone, be made into the DMF solution of methyl-n-butyl ketone with DMF, obtain and be added with interior target matrix correction agent, and for subsequent use as matrix solvent;
(3) detection of vinyl acetate standard solution and the drafting of typical curve: many parts of the standard solution that accurately removing step (1) obtains, the matrix solvent that adds respectively a certain amount of step (2) to obtain, and with N, dinethylformamide constant volume obtains the vinyl acetate standard solution of a series of variable concentrations gradients, respectively the vinyl acetate standard solution of these a series of variable concentrations gradients is carried out after Static Headspace balance, put into respectively head-space sampler and carry out SHS-GC/MS detection; Taking the chromatographic peak area of vinyl acetate and interior mark peak area ratio Y as ordinate, its respective quality concentration X (μ g/mL) draws the typical curve of vinyl acetate as horizontal ordinate, calculates the regression equation of vinyl acetate typical curve;
(4) the Static Headspace processing of sample: cigarette is placed in to head space bottle with white glue with vinyl sample, adds prepared matrix solvent, the testing sample solution of acquisition is sealed rapidly, carry out after Static Headspace balance to be measured;
(5) assay of residual vinyl acetate in white glue with vinyl sample for cigarette: the testing sample solution after Static Headspace balance is put into head-space sampler and carry out SHS-GC/MS detection, by in regression equation described in the ratio substitution of the peak area of the vinyl acetate obtaining and the peak area of interior mark methyl-n-butyl ketone, can obtain the residual content of vinyl acetate in cigarette white glue with vinyl sample.
Preferably, in step (1), in vinyl acetate standard solution, the concentration of vinyl acetate is 5mg/mL-50mg/mL.
Preferably, in step (2), in matrix solvent, the concentration of methyl-n-butyl ketone is 100 μ g/mL-500 μ g/mL.
Preferably, in step (3), the umber of the vinyl acetate standard solution accurately pipetting is 6 parts, and in the vinyl acetate standard solution of a series of variable concentrations gradients that obtain, the concentration of vinyl acetate is respectively 10 μ g/mL, 20 μ g/mL, 40 μ g/mL, 80 μ g/mL, 160 μ g/mL, 400 μ g/mL, the concentration of methyl-n-butyl ketone is 120 μ g/mL.
Preferably, in step (3) neutralization procedure (4), the equilibrium temperature of Static Headspace balance is 80 DEG C, and equilibration time is 10-30min; Be preferably 15min.
Preferably, in step (4), in described testing sample solution, every 0.1g cigarette generally adds 1-5ml to be added with interior target matrix solvent by white glue with vinyl.
Preferably, in step (3) neutralization procedure (5), the Static Headspace condition that SHS-GC/MS detects is:
Sample equilibrium temperature: 80 DEG C; Sample loop temperature: 100 DEG C; Transmission line temperature: 120 DEG C; Sample equilibration time: 15min; Sample bottle moulding pressure: 15psi; Nebulizer gas pressure: 15psi; Pressing time: 0.20min; Inflationtime: 0.20min; Sample loop equilibration time: 0.05min; Sample injection time: 0.5min.
Preferably, in step (3) neutralization procedure (5), the GC/MS condition that SHS-GC/MS detects is:
GC conditions is: chromatographic column: (30m × 0.25mm × 0.25 μ m) for HP-INNOWAX; Injector temperature: 150 DEG C; Carrier gas: high-purity helium, purity >=99.999%; The constant current mode of flow velocity: 1.0mL/min; Split ratio: 10: 1; Heating schedule: 40 DEG C of maintenance 3min of initial temperature, then rise to 180 DEG C with the speed of 10 DEG C/min, and then rise to 200 DEG C with the speed of 20 DEG C/min, keep 1min;
Mass spectrum condition is: transmission line temperature: 250 DEG C; Ion source temperature: 230 DEG C; Quadrupole rod temperature: 150 DEG C; Solvent delay: 3min; Ionization mode: EI source; Ionizing energy: 70eV; Scan mode: select ion monitoring (SIM).
The present invention, according to the special physicochemical property of white glue with vinyl for cigarette, optionally measures cigarette residual vinyl acetate in white latex, has set up the content of Static Headspace-gas chromatography-mass spectrum technology coupling selective determination cigarette residual vinyl acetate in white latex.Sample, after 80 DEG C, 15min Static Headspace, taking methyl-n-butyl ketone as interior mark, adopts HP-INNOWAX post, and gas chromatography-mass spectrum choice ion pattern detects, inner mark method ration.The detection of this assay method is limited to 0.63mg/kg, and recovery of standard addition is 104%～107%, and relative standard deviation (RSD) is 2.5%～4.9%.The features such as it is simple and quick, accurate sensitive that this assay method has, are applied to actual sample detection and have obtained good result.
Assay method of the present invention is directly got head space gas vinyl acetate composition remaining in sample is analyzed, can effectively get rid of sample substrate to the interference of analyzing, without complicated sample pretreatment process, this assay method has been avoided loaded down with trivial details solvent extraction, and has quantitatively made up the not high defect of GC-flame ionization ditector sensitivity by SIM.Experimental result shows: assay method of the present invention has the features such as reproducible, accuracy is high, rapid sensitive, is particularly suitable for the mensuration of cigarette with residual vinyl acetate in white glue with vinyl.
Brief description of the drawings
The affect figure of Fig. 1 head space equilibration time on peak area.
The affect figure of Fig. 2 head space equilibrium temperature on peak area.
Tetra-kinds of matrix of Fig. 3 are proofreaied and correct the selection chromatography of ions figure of solvent for sample determination
A:N, dinethylformamide; B: glyceryl triacetate; C: cyclohexane; D: normal hexane; Wherein in each collection of illustrative plates,
1: vinyl acetate; 2:N, dinethylformamide; 3: cyclohexane; 4: normal hexane.
Selection chromatography of ions Fig. 4 c of white glue with vinyl sample for selection chromatography of ions Fig. 4 a of Fig. 4 methyl-n-butyl ketone, selection chromatography of ions Fig. 4 b of vinyl acetate standard items and cigarette; Wherein, 1: vinyl acetate; 2:2-hexanone; 3:N, dinethylformamide.
Embodiment
Further set forth the present invention below in conjunction with specific embodiment, should be understood that these embodiment are only not used in and limit the scope of the invention for the present invention is described.
Embodiment 1
1 experimental section
1.1 materials, reagent and instrument
White glue with vinyl sample for cigarette (being selected from cigarette enterprise); Glyceryl triacetate (AR, chemical reagent Ltd of traditional Chinese medicines group); Cyclohexane, normal hexane (chromatographically pure, Tianjin great Mao chemical reagent factory); DMF (AR, Chongqing Chuan Dong chemical industry (group) company limited chemical reagent factory); Methyl-n-butyl ketone (interior mark, IS; 99%), vinyl acetate (99%, Sigma company of the U.S.); HP6890/5973 type Gc/ms Analyser, 7694 automatic head space instrument (Agilent company of the U.S.); AG104 type electronic analytical balance (sensibility reciprocal: 0.1mg, Mettler Toledo Inc. of Switzerland).
1.2 sample preparation and analysis
Accurately take 0.25g vinyl acetate in 25mL volumetric flask, use DMF constant volume, obtain 10mg/mL vinyl acetate standard solution.Accurately take 0.3g methyl-n-butyl ketone (IS) in 50mL volumetric flask, use DMF constant volume, obtain 6mg/mL IS solution; Get 2mL IS solution in 100mL volumetric flask, use DMF constant volume, for subsequent use as matrix solvent, its concentration is 120 μ g/mL.Accurately take 0.1g sample, be placed in head space bottle, add the DMF solution of 1mL120 μ g/mL IS, compress rapidly bottle cap, put into head-space sampler and carry out GC-MS detection analysis.Detection analysis condition is:
(1) SHS condition.Sample equilibrium temperature: 80 DEG C; Sample loop temperature: 100 DEG C; Transmission line temperature: 120 DEG C; Sample equilibration time: 15min; Sample bottle moulding pressure: 15psi; Nebulizer gas pressure: 15psi; Pressing time: 0.20min; Inflationtime: 0.20min; Sample loop equilibration time: 0.05min; Sample injection time: 0.5min.
(2) GC/MS condition.(30m × 0.25mm × 0.25 μ m) for chromatographic column: HP-INNOWAX; Injector temperature: 150 DEG C; Carrier gas: high-purity helium, purity>=99.999%; Flow velocity: 1.0mL/min (constant current mode); Split ratio: 10: 1; Heating schedule:
transmission line temperature: 250 DEG C; Ion source temperature: 230 DEG C; Quadrupole rod temperature: 150 DEG C; Solvent delay: 3min; Ionization mode: EI source; Ionizing energy: 70eV; Scan mode: select ion monitoring (SIM).
Retention time is compared in employing, standard specimen addition method is qualitative, inner mark method ration under SIM pattern.The retention time of vinyl acetate and IS and characteristic ion are in table 1.
Table 1 vinyl acetate and and retention time and the qualitative, quantitative ion of IS
2 results and discussion
The selection of 2.1 SHS equilibration times
SHS analyzes the impact that is mainly subject to sample equilibrium temperature, equilibration time and sample substrate, therefore, adopts the mode of single factor experiment to select these influence factors.The vinyl acetate standard solution that is 10 μ g/mL by concentration is placed in head space bottle, under the equilibrium temperature of 80 DEG C to different equilibration times (5,10,15,20, head space gas 30min) is analyzed, and taking the chromatographic peak area of vinyl acetate as index, investigates the impact of different equilibration times on vinyl acetate amount in static headspace gas.Result (seeing Fig. 1) shows, when equilibration time is 10～30min, and basic indifference, when this explanation 10min, the distribution of vinyl acetate has reached dynamic balance state.In order to ensure the abundant balance of sample system, select the SHS equilibration time of 15min as sample.
The selection of 2.2 SHS equilibrium temperatures
Under identical equilibration time, the content of vinyl acetate in the lower static headspace gas of different equilibrium temperatures (45 DEG C, 50 DEG C, 60 DEG C, 80 DEG C, 90 DEG C, 100 DEG C) is compared.Result (seeing Fig. 2) shows, along with the raising of equilibrium temperature, the chromatographic peak area of vinyl acetate increases gradually, and at 45～60 DEG C, speedup is slower, and in the time of 60～90 DEG C, speedup is very fast, eases up subsequently.Due to temperature, more high volatile volatile compound is more, impurity peaks increases, and pollute also larger to ion gun, therefore, consider the effumability (boiling point is 71.8 DEG C) of vinyl acetate and reduce ionogenic pollution and impurity peaks disturbs the factor of two aspects, selecting equilibrium temperature is 80 DEG C.
The selection of 2.3 SHS matrix correction agents
In head space gas, the content of each component is both relevant with the volatility of itself, relevant with sample substrate again, especially the component of those solubleness large (partition factor is large) in sample substrate, matrix effect is more obvious, make analytic sample and standard solution there is identical matrix solvent, can effectively eliminate the matrix effect of sample, thereby improve the accuracy of quantitative test.Therefore, this experiment selects respectively glyceryl triacetate, normal hexane, cyclohexane and 4 kinds of organic solvents of DMF to investigate (seeing Fig. 3) as matrix correction agent for sample determination.Result shows, normal hexane and cyclohexane are because boiling point is relatively low, and solvent appearance time and vinyl acetate approach, and chromatographic resolution degree is bad, causes quantitative accuracy poor, is therefore not suitable as the matrix correction agent of vinyl acetate.Glyceryl triacetate boiling point is higher, is difficult for flowing out at short notice, more consuming time while analysis for lower boiling vinyl acetate.DMF has moderate boiling point, is a kind of good non-proton polar reagent, can dissolve cigarette glue, sample is dispersed in matrix solvent, thereby makes quantitative result more accurate.In sum, select DMF as matrix solvent.
2.4 interior targets are selected
In the time adopting SHS-GC to measure volatile compound, quantitative test adopts external standard method conventionally.Due to head space method, affected by environment and sample substrate larger, makes the quantitative accuracy of external standard method be subject to certain limitation, and internal standard method is attempted for Headspace-Gas Chromatography Analysis quantitative test in recent years.The present invention's experiment selects methyl-n-butyl ketone to analyze as IS.Result (Fig. 4) shows: under same quality level condition, the mass spectrum response of methyl-n-butyl ketone and vinyl acetate component to be measured is comparatively approaching, and (sees Fig. 4 b), therefore selection methyl-n-butyl ketone is internal standard compound IS with the degree of separation of component to be measured is high.
The detectability of 2.5 working curves and method, the recovery, precision
Accurately pipette 10mg/mL vinyl acetate standard solution 25 μ L, 50 μ L, 100 μ L, 200 μ L, 400 μ L, 1000 μ L are in 6 25mL volumetric flasks, adding respectively 500 μ L concentration is 6mg/mL IS solution, and is settled to 25mL with DMF, obtain concentration and be respectively 10,20,40,80,160,400 μ g/mL and IS concentration are the vinyl acetate series standard solution of 6 grades of concentration gradients of 120 μ g/mL.Respectively the standard solution of these 6 grades of gradient concentrations is carried out to SHS-GC-MS analysis, and taking vinyl acetate chromatographic peak area and interior mark peak area ratio Y as ordinate, its respective quality concentration X (μ g/mL) are as horizontal ordinate carries out regretional analysis, obtain regression equation Y=21.039X+1.6013 (R
2=0.9999), calculate detection with 3 times of signal to noise ratio (S/N ratio)s (S/N=3) and be limited to 0.63mg/kg.
In the white glue with vinyl sample of known vinyl acetate content (mean value of measuring for 6 times), add respectively high, normal, basic 3 variable concentrations (40,20,10 μ g/mL) the standard solution of vinyl acetate, adopt SHS-GC-MS method to measure corresponding vinyl acetate content, according to the addition of measurement result and vinyl acetate, calculate the recovery (in table 2) of this assay method.Result (table 2) demonstration, the recovery of vinyl acetate is 104%～107%, shows that the accuracy of this assay method is higher; The relative standard deviation (RSD) of calculating vinyl acetate according to measurement result is 2.5%～4.9%, is less than 5%, illustrates that the repeatability of this assay method is better.
The recovery and the precision (n=6) of vinyl acetate in glue for table 2 cigarette
The mensuration of the vinyl acetate content in white glue with vinyl sample for 2.6 actual cigarettes
In utilizing 1.2 sample preparation in said determination method and analyzing, the preparation steps of each solution and 6 kinds of cigarettes residual quantity of vinyl acetate in white glue with vinyl that determination step uses cigarette enterprise are measured, each sample replicate determination 6 times, result (in table 3) shows: 6 kinds of cigarettes use the residual quantity of vinyl acetate in white glue with vinyl between 72.27～310.09mg/kg, and RSD is 1.6%～4.5%.Wherein, in 6 kinds of cigarette white glue with vinyl sample solutions that configure the corresponding 1ml of the every 0.1g of cigarette white glue with vinyl be added with interior target matrix correction agent, the concentration that is added with methyl-n-butyl ketone in interior target matrix correction agent is 120 μ g/mL.
Testing result and the precision (n=6) of middle vinyl acetate in glue sample for table 3 cigarette
3 conclusions
The present invention has set up the static headspace GC-MS method of selective determination cigarette by vinyl acetate content remaining in white glue with vinyl, this assay method has been avoided loaded down with trivial details solvent extraction, and has quantitatively made up the not high defect of GC-flame ionization ditector sensitivity by SIM.The features such as that this assay method has is reproducible, accuracy is high, rapid sensitive, are suitable for the mensuration of cigarette with residual vinyl acetate in white glue with vinyl.
Claims (3)
1. the method for Static Headspace-gaschromatographic mass spectrometry selective determination cigarette use residual vinyl acetate in white latex, it is characterized in that, taking methyl-n-butyl ketone as internal standard compound, adopt Static Headspace balance, gas chromatography-mass spectrum choice ion pattern to measure the content of cigarette residual vinyl acetate in white latex, wherein, gas chromatography adopts HP-INNOWAX chromatographic column, assay adopts inner mark method ration, and described Static Headspace-gaschromatographic mass spectrometry selective determination cigarette specifically comprises the steps: by the method for residual vinyl acetate in white latex
(1) preparation of vinyl acetate standard solution: accurately take the pure material of vinyl acetate, with N, N – dimethyl formamide is made into standard solution;
(2) be added with the preparation of interior target matrix correction agent: accurately take internal standard compound 2 – hexanones, with N, N – dimethyl formamide is made into the N of 2 – hexanones, N – dimethyl formamide solution obtains and is added with interior target matrix correction agent, and for subsequent use as matrix solvent; In matrix solvent, the concentration of 2 – hexanones is 100 μ g/mL-500 μ g/mL;
(3) detection of vinyl acetate standard solution and the drafting of typical curve: many parts of the standard solution that accurately removing step (1) obtains, the matrix solvent that adds respectively a certain amount of step (2) to obtain, and with N, N – dimethyl formamide constant volume obtains the vinyl acetate standard solution of a series of variable concentrations gradients, respectively the vinyl acetate standard solution of these a series of variable concentrations gradients is carried out after Static Headspace balance, put into respectively head-space sampler and carry out SHS-GC/MS detection; Taking the chromatographic peak area of vinyl acetate and interior mark peak area ratio Y as ordinate, its respective quality concentration X(μ g/mL) draw the typical curve of vinyl acetate as horizontal ordinate, calculate the regression equation of vinyl acetate typical curve;
(4) the Static Headspace processing of sample: cigarette is placed in to head space bottle with white glue with vinyl sample, adds prepared matrix solvent, the testing sample solution of acquisition is sealed rapidly, carry out after Static Headspace balance to be measured; In described testing sample solution, every 0.1g cigarette adds 1-5ml to be added with interior target matrix solvent by white glue with vinyl;
(5) assay of residual vinyl acetate in white glue with vinyl sample for cigarette: the testing sample solution after Static Headspace balance is put into head-space sampler and carry out SHS-GC/MS detection, by in regression equation described in the ratio substitution of the peak area of the vinyl acetate obtaining and the peak area of interior mark 2 – hexanones, obtain the residual content of vinyl acetate in cigarette white glue with vinyl sample;
In described step (3) neutralization procedure (4), the equilibrium temperature of Static Headspace balance is 80 DEG C, and equilibration time is 10-30min;
In described step (3) neutralization procedure (5), the Static Headspace condition that SHS-GC/MS detects is:
Sample equilibrium temperature: 80 DEG C; Sample loop temperature: 100 DEG C; Transmission line temperature: 120 DEG C; Sample equilibration time: 15min; Sample bottle moulding pressure: 15psi; Nebulizer gas pressure: 15psi; Pressing time: 0.20min; Inflationtime: 0.20min; Sample loop equilibration time: 0.05min; Sample injection time: 0.5min;
In step (3) neutralization procedure (5), the GC/MS condition that SHS-GC/MS detects is:
GC conditions: chromatographic column: HP-INNOWAX; Injector temperature: 150 DEG C; Carrier gas: high-purity helium, purity >=99.999%; The constant current mode of flow velocity: 1.0mL/min; Split ratio: 10:1; Heating schedule: 40 DEG C of maintenance 3min of initial temperature, then rise to 180 DEG C with the speed of 10 DEG C/min, and then rise to 200 DEG C with the speed of 20 DEG C/min, keep 1min;
Mass spectrum condition: transmission line temperature: 250 DEG C; Ion source temperature: 230 DEG C; Quadrupole rod temperature: 150 DEG C; Solvent delay: 3min; Ionization mode: EI source; Ionizing energy: 70eV; Scan mode: SIM selects ion monitoring.
2. the method for residual vinyl acetate in white latex for Static Headspace-gaschromatographic mass spectrometry selective determination cigarette as claimed in claim 1, is characterized in that, in step (1), in standard solution, the concentration of vinyl acetate is 5mg/mL-50mg/mL.
3. the method for residual vinyl acetate in white latex for Static Headspace-gaschromatographic mass spectrometry selective determination cigarette as claimed in claim 1, it is characterized in that, in step (3), the umber of the vinyl acetate standard solution accurately pipetting is 6 parts, and in the vinyl acetate standard solution of a series of variable concentrations gradients that obtain, the concentration of vinyl acetate is respectively 10 μ g/mL, 20 μ g/mL, 40 μ g/mL, 80 μ g/mL, 160 μ g/mL, 400 μ g/mL, the concentration of 2 – hexanones is 120 μ g/mL.
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| CN103512994B (en) * | 2013-10-14 | 2015-11-18 | 福建中烟工业有限责任公司 | A kind ofly measure the residual method of volatile ingredient in filter stick for cigarettes |
| CN104198602B (en) * | 2014-09-01 | 2016-04-13 | 云南中烟工业有限责任公司 | The detection method of vinyl acetate in a kind of hot melt adhesive |
| CN106841442B (en) * | 2017-01-25 | 2020-05-05 | 江苏中烟工业有限责任公司 | Method for simultaneously determining vinyl acetate and six benzene series in water-based adhesive |
| CN112557531B (en) * | 2020-11-27 | 2023-05-09 | 衢州康鹏化学有限公司 | Method for detecting residual solvent in vinyl sulfate by headspace gas chromatography |
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