CN106526006A - Method for detecting volatiles residue in hot-melt adhesive for cigarettes - Google Patents
Method for detecting volatiles residue in hot-melt adhesive for cigarettes Download PDFInfo
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- CN106526006A CN106526006A CN201610935669.9A CN201610935669A CN106526006A CN 106526006 A CN106526006 A CN 106526006A CN 201610935669 A CN201610935669 A CN 201610935669A CN 106526006 A CN106526006 A CN 106526006A
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- isopropanol
- acetone
- methyl acetate
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- 235000019504 cigarettes Nutrition 0.000 title claims abstract description 23
- 239000004831 Hot glue Substances 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 title claims abstract description 16
- 239000003039 volatile agent Substances 0.000 title abstract 5
- 239000004615 ingredient Substances 0.000 claims abstract description 21
- 239000012224 working solution Substances 0.000 claims abstract description 10
- 238000005259 measurement Methods 0.000 claims abstract description 5
- 230000008569 process Effects 0.000 claims abstract description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 66
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 32
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 claims description 23
- KXKVLQRXCPHEJC-UHFFFAOYSA-N acetic acid trimethyl ester Natural products COC(C)=O KXKVLQRXCPHEJC-UHFFFAOYSA-N 0.000 claims description 23
- 238000001514 detection method Methods 0.000 claims description 16
- JMMWKPVZQRWMSS-UHFFFAOYSA-N isopropanol acetate Natural products CC(C)OC(C)=O JMMWKPVZQRWMSS-UHFFFAOYSA-N 0.000 claims description 14
- 239000000126 substance Substances 0.000 claims description 7
- 230000005540 biological transmission Effects 0.000 claims description 6
- 238000011067 equilibration Methods 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 238000002347 injection Methods 0.000 claims description 4
- 239000007924 injection Substances 0.000 claims description 4
- 230000003068 static effect Effects 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000012159 carrier gas Substances 0.000 claims description 3
- 238000004587 chromatography analysis Methods 0.000 claims description 3
- 239000005350 fused silica glass Substances 0.000 claims description 3
- 239000001307 helium Substances 0.000 claims description 3
- 229910052734 helium Inorganic materials 0.000 claims description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 3
- 150000002500 ions Chemical class 0.000 claims description 3
- 238000001819 mass spectrum Methods 0.000 claims description 3
- 238000000465 moulding Methods 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 239000000758 substrate Substances 0.000 claims description 3
- 239000012895 dilution Substances 0.000 claims description 2
- 238000010790 dilution Methods 0.000 claims description 2
- 238000003825 pressing Methods 0.000 claims description 2
- -1 dimethyl formyl Amine Chemical class 0.000 claims 2
- 238000003859 hyphenated technique Methods 0.000 claims 1
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 abstract description 15
- 239000011159 matrix material Substances 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 2
- 238000004949 mass spectrometry Methods 0.000 abstract description 2
- 230000035945 sensitivity Effects 0.000 abstract description 2
- 238000003988 headspace gas chromatography Methods 0.000 abstract 1
- 238000002203 pretreatment Methods 0.000 abstract 1
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- 238000003556 assay Methods 0.000 description 4
- 230000004044 response Effects 0.000 description 4
- URAYPUMNDPQOKB-UHFFFAOYSA-N triacetin Chemical compound CC(=O)OCC(OC(C)=O)COC(C)=O URAYPUMNDPQOKB-UHFFFAOYSA-N 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 3
- 230000001070 adhesive effect Effects 0.000 description 3
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 241000208125 Nicotiana Species 0.000 description 2
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000009514 concussion Effects 0.000 description 2
- 239000001087 glyceryl triacetate Substances 0.000 description 2
- 235000013773 glyceryl triacetate Nutrition 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000012086 standard solution Substances 0.000 description 2
- 229960002622 triacetin Drugs 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 238000004026 adhesive bonding Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 239000012943 hotmelt Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 230000000391 smoking effect Effects 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N2030/042—Standards
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention provides a method for detecting volatiles residue in hot-melt adhesive for cigarettes; the method comprises the steps of (1) preparing a standard working solution for various volatiles; (2) preparing a sample; (3) determining by headspace-gas chromatography/mass spectrometry process; (4) calculating measurement results for various volatiles in the sample. The method is simple and convenient, and ingredient loss due to complex pre-treatment is avoided; dimethyl formamide is selected as a matrix corrective, matrix effect can be relieved, all volatiles to be detected can be dissolved, and the ingredients to be detected can also be detected without influence; the method has the advantages of good operation accuracy, high sensitivity and good repeatability.
Description
Technical field
The invention belongs to Tobacco Analysis technical field, and in particular to the inspection of volatile ingredient residual in a kind of hot-melt adhesive for cigarette
Survey method.
Background technology
In hot-melt adhesive for cigarette volatile ingredient residual, be it is introduced by raw material itself, mainly residual monomer with have
Machine solvent.Hot-melt adhesive for cigarette operating temperature is high, and step is applied under molten condition, is cooled to solid-state and completes to be glued, produces under molten condition
Raw volatile ingredient residual is gathered in cigarette filter, is produced bad smell, is affected cigarette odor-absorbing, reduces cigarette quality.
Secondly, the volatile ingredient such as middle acetone, isopropanol, methyl acetate has larger harm, the safety one of smoking material to human body
It is directly tobacco business focus of attention.Therefore, carry out for volatile ingredient residual in hot-melt adhesive for cigarette effective, quick, accurate
Analyzing detecting method, to ensure cigarette product quality and safety have important meaning.Water base adhesive, glyceryl triacetate and gluing
In the samples such as agent, the assay method of volatility residual has document report, and said method is not suitable for the hot melt of heating and melting feature
The detection of volatile ingredient residual in glue.
At present, static headspace-GC-MS fado is used for the measure of volatility residual in cigarette packaging material, so far also not
See the report detected with static headspace-GC-MS in PUR.
The content of the invention
For above-mentioned the deficiencies in the prior art, the characteristics of the purpose of the present invention is for hot-melt adhesive for cigarette, there is provided Yi Zhongneng
Quickly, accurately, the method that batch detection goes out the volatile ingredients such as hot-melt adhesive for cigarette acetone, isopropanol, methyl acetate.
The technical scheme that the present invention is provided:The detection method of volatile ingredient residual in a kind of hot-melt adhesive for cigarette, including such as
Lower step:
(1) preparation of standard working solution:Acetone, isopropanol and methyl acetate standard substance are weighed, with chromatographically pure dimethyl
Methanamide is substrate correction agent solvent, and Jing stepwise dilutions are configured to hybrid standard working solution;
(2) preparation of sample:PUR is shredded, 0.2000g is weighed and is placed in ml headspace bottle, accurately add 2mL dimethyl
Methanamide, is sealed to be measured immediately;
(3) HS GC mass spectrometric determination:Sample and standard substance are put in Static Headspace instrument and are processed, condition is:
Sample bottle equilibrium temperature:120 DEG C, sample loop temperature:140 DEG C, transmission line temperature:180℃;Sample bottle equilibration time 45min is low
Fast concussion pattern;Sample bottle moulding pressure 138kpa, pressing time 0.20min;Inflationtime:0.20min;Sample loop volume
3.0mL, sample loop equilibration time 0.05min;Sample injection time 1.0min;By sample and standard substance Jing after head space process, pass through
Gas chromatographyMass spectrometry is measured to acetone, isopropanol and methyl acetate;
(4) in sample various volatile ingredient measurement results calculating:According to the measurement result of standard working solution, with third
The peak area of ketone, isopropanol and methyl acetate distinguishes drawing curve to mass concentration, obtains standard working curve, then by sample
Detect in product that the peak area of acetone, isopropanol and methyl acetate substitutes into standard working curve respectively, obtains acetone, isopropanol in sample
With the content of methyl acetate.
Further, in the step (3), the condition of gas chromatogram is:Innowax fused quartz capillary chromatography posts
(30m×0.25mm×0.25μm);Injector temperature:250℃;Temperature programming:50 DEG C of initial temperature, keep 2min, with 4 DEG C/
Min rises to 200 DEG C, keeps 10min;Split sampling, split ratio 10:1;Carrier gas:Helium (purity is 99.999%);Constant current mould
Formula, flow velocity are 2.0mL/min;Sample size:1μL.
Further, in the step (3), mass spectrographic condition is:EI ionizes pattern, ionization energy 70eV;Ion source temperature:
230℃;Transmission line temperature:250℃;150 DEG C of level Four bar temperature;Scanning of the mass spectrum mode:Full scan (SCAN), sweep limitss 30~
350amu。
Further, in step (1) the hybrid standard working solution acetone, isopropanol and methyl acetate mass concentration
It is:1mg/L、2mg/L、4mg/L、8mg/L、16mg/L.
The method of the present invention for PUR operating temperature the characteristics of 100 DEG C -120 DEG C, compared with prior art this
Bright method has following excellent results:
(1) present invention optimizes head space equilibrium temperature, PUR is made to be maintained at molten condition, actual response PUR work
Make the volatilization situation of 3 kinds of compositions such as acetone under state, isopropanol and methyl acetate, method is simple and convenient, it is to avoid complicated front place
Manage and caused ingredients from lossing;In the samples such as water base adhesive, glyceryl triacetate and adhesive, the assay method of volatility residual is put down
Weighing apparatus temperature is relatively low, is not suitable for the detection of volatile ingredient residual in the PUR of heating and melting feature;And formaldehyde in PUR,
The object of the assay method such as benzene and benzene homologues, phenols polyphenoils analysis is different, is not suitable for acetone, isopropanol and acetic acid first
The detection of 3 kinds of volatility residuals such as ester.
(2) dimethylformamide is chosen as substrate correction agent, can reduce matrix effect and dissolve all to be measured waving
The property sent out composition can not disturb the detection of composition to be measured again.
(3) qualitative and detection by quantitative is carried out simultaneously using mass detector, it is to avoid the false positive being likely to occur.
(4) the inventive method has the advantages that to operate accurate, sensitivity high and reproducible.The detection of acetone is limited to
0.05mg/L, is quantitatively limited to 0.15mg/L, and relative standard deviation is 1.47%, and the response rate is between 95.1~102.3%;Isopropyl
The detection of alcohol is limited to 0.06mg/L, is quantitatively limited to 0.19mg/L, and relative standard deviation is 2.17%, the response rate 94.8~
Between 99.2%;The detection of methyl acetate is limited to 0.10mg/L, is quantitatively limited to 0.35mg/L, and relative standard deviation is 3.44%,
The response rate is between 92.4~98.6%.
Description of the drawings
Fig. 1 is the standard working curve of acetone;
Fig. 2 is the standard working curve of isopropanol;
Fig. 3 is the standard working curve of methyl acetate;
Fig. 4 is the gas chromatogram of hot-melt adhesive for cigarette sample A;
Fig. 5 is the gas chromatogram of hot-melt adhesive for cigarette sample B.
Specific embodiment
The present invention will be further described with reference to the accompanying drawings and examples.
Embodiment 1
0.0500g acetone, isopropanol and methyl acetate standard substance are weighed respectively, are placed in 1000mL volumetric flasks, are used chromatograph
Absolute dimethylformamide is settled to scale, and the solution is hybrid standard storing solution.Accurately pipette 2mL, 4mL, 8mL, 16mL,
The 32mL hybrid standard storing solutions, are respectively placed in 100mL volumetric flasks, are settled to scale with chromatograph absolute dimethylformamide, i.e.,
Obtain series standard working solution.The serial mixed standard solution concentration of preparation is:1mg/L、2mg/L、4mg/L、8mg/L、16mg/
L。
PUR sample A is shredded, 0.2000g is weighed and is placed in ml headspace bottle, accurately add 2mL dimethylformamides, Jing
HS GC mass spectrograph is analyzed, and head space condition is:Sample bottle equilibrium temperature:120 DEG C, sample loop temperature:140 DEG C,
Transmission line temperature:180℃;Sample bottle equilibration time 45min, low speed concussion pattern;Sample bottle moulding pressure 138kpa, during pressurization
Between 0.20min;Inflationtime:0.20min;Sample loop volume 3.0mL, sample loop equilibration time 0.05min;Sample injection time
1.0min.GC conditions are:Innowax fused quartz capillary chromatography posts (30m × 0.32mm × 0.25 μm);Injection port
Temperature:250℃;Temperature programming:50 DEG C of initial temperature, keeps 2min, rises to 200 DEG C with 4 DEG C/min, keeps 10min;It is diverted into
Sample, split ratio 10:1;Carrier gas:Helium (purity is 99.999%);Constant current mode, flow velocity are 2.0mL/min;Sample size:1μL.
Mass Spectrometry Conditions are:EI ionizes pattern, ionization energy 70eV;Ion source temperature:230℃;Transmission line temperature:250℃;Level Four bar temperature
150℃;Scanning of the mass spectrum mode:Full scan (SCAN), 30~350amu of sweep limitss.
Every grade of standard solution parallel assay 2 times, averages.The peak area of each component is bent to mass concentration drawing
Line, standard working curve of the accompanying drawing 1 for acetone, standard working curve of the accompanying drawing 2 for isopropanol, mark of the accompanying drawing 3 for methyl acetate
Quasi- working curve, accompanying drawing 4 are hot-melt adhesive for cigarette sample A chromatograms, and each volatile ingredient standard working curve is as shown in table 1:
1 each volatile ingredient standard working curve of table
By the acetone in the sample A measured under the same terms, isopropanol and methyl acetate chromatographic peak area, standard work is substituted into
Make curve, try to achieve the content of the acetone, isopropanol and methyl acetate in sample.Sample determination twice, is averaged, and tries to achieve sample
In A, content of acetone is 15.66mg/L, and isopropanol content is 7.66mg/L, and methyl acetate content is 5.20mg/L.
Embodiment 2
As described in Example 1, another PUR sample B is selected, accompanying drawing 5 is hot-melt adhesive for cigarette sample B chromatograms.Sample is surveyed
Fixed to average twice, it is 12.94mg/L to try to achieve content of acetone in sample B, and isopropanol content is 7.78mg/L, methyl acetate
Content is 9.33mg/L.
The detailed description of specific embodiments of the present invention is the foregoing is only, the present invention is not limited with this, it is all at this
Any modification, equivalent and improvement for being made in the mentality of designing of invention etc., should be included in protection scope of the present invention it
It is interior.
Claims (4)
1. the detection method that volatile ingredient is remained in a kind of hot-melt adhesive for cigarette, it is characterised in that comprise the steps:
(1) preparation of standard working solution:Acetone, isopropanol and methyl acetate standard substance are weighed, with chromatographically pure dimethyl formyl
Amine is substrate correction agent solvent, and Jing stepwise dilutions are configured to hybrid standard working solution;
(2) preparation of sample:PUR is shredded, 0.2000g is weighed and is placed in ml headspace bottle, accurately add 2mL dimethyl formyls
Amine, is sealed to be measured immediately;
(3) HS GC mass spectrometric determination:Sample and standard substance are put in Static Headspace instrument and are processed, condition is:Sample
Bottle equilibrium temperature:120 DEG C, sample loop temperature:140 DEG C, transmission line temperature:180℃;Sample bottle equilibration time 45min, low speed shake
Swing pattern;Sample bottle moulding pressure 138kpa, pressing time 0.20min;Inflationtime:0.20min;Sample loop volume 3.0mL,
Sample loop equilibration time 0.05min;Sample injection time 1.0min;By sample and standard substance Jing after head space process, by gas phase color
Spectrum-mass spectrometric hyphenated technique is measured to acetone, isopropanol and methyl acetate;
(4) in sample various volatile ingredient measurement results calculating:According to the measurement result of standard working solution, with acetone,
The peak area of isopropanol and methyl acetate distinguishes drawing curve to mass concentration, obtains standard working curve, then by sample
Middle detection acetone, the peak area of isopropanol and methyl acetate substitute into standard working curve respectively, obtain acetone in sample, isopropanol and
The content of methyl acetate.
2. the detection method that volatile ingredient is remained in hot-melt adhesive for cigarette according to claim 1, it is characterised in that:It is described
In step (3), the condition of gas chromatogram is:Innowax fused quartz capillary chromatography posts (30m × 0.25mm × 0.25 μm);Enter
Sample mouth temperature:250℃;Temperature programming:50 DEG C of initial temperature, keeps 2min, rises to 200 DEG C with 4 DEG C/min, keeps 10min;Point
Stream sample introduction, split ratio 10:1;Carrier gas:Helium (purity is 99.999%);Constant current mode, flow velocity are 2.0mL/min;Sample size:1
μL。
3. the detection method that volatile ingredient is remained in hot-melt adhesive for cigarette according to claim 1 and 2, it is characterised in that:
In the step (3), mass spectrographic condition is:EI ionizes pattern, ionization energy 70eV;Ion source temperature:230℃;Transmission line temperature:
250℃;150 DEG C of level Four bar temperature;Scanning of the mass spectrum mode:Full scan (SCAN), 30~350amu of sweep limitss.
4. the detection method that volatile ingredient is remained in hot-melt adhesive for cigarette according to claim 1, it is characterised in that:It is described
In step (1) hybrid standard working solution, the mass concentration of acetone, isopropanol and methyl acetate is:1mg/L、2mg/L、4mg/
L、8mg/L、16mg/L。
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CN201610935669.9A CN106526006A (en) | 2016-11-01 | 2016-11-01 | Method for detecting volatiles residue in hot-melt adhesive for cigarettes |
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