CN107389811A - The assay method of diisopropyl naphthalene in cigarette tipping paper - Google Patents
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- CN107389811A CN107389811A CN201710541398.3A CN201710541398A CN107389811A CN 107389811 A CN107389811 A CN 107389811A CN 201710541398 A CN201710541398 A CN 201710541398A CN 107389811 A CN107389811 A CN 107389811A
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- G—PHYSICS
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- 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
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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
- G01N30/02—Column chromatography
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- G01N30/06—Preparation
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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
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/025—Gas chromatography
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Abstract
The invention discloses a kind of assay method of diisopropyl naphthalene in cigarette tipping paper, extract is used as using dichloromethane, cigarette tipping paper sample pipettes extract after oscillation extraction, the centrifugal clarification liquid after SPE column purification, again through organic membrane filter, using the diisopropyl naphthalene in gas-chromatography tandem mass spectrum combination method measure cigarette tipping paper.The dilution inner mark method ration of the present invention avoids COMPLEX MIXED objects system Quantitative Separation, the difficulty of purifying, also overcomes the influence of matrix effect；Seven kinds of isomers of object are effectively realized that baseline is kept completely separate using gas-chromatography tandem mass spectrum combined instrument, improve quantitative accuracy, measurement result can accurately reflect the content of object in sample；This method uses direct injected, can quickly, accurately detect the content of diisopropyl naphthalene in cigarette tipping paper, and repeatability and the rate of recovery are good, suitable for the analysis of batch samples.
Description
Technical field
The invention belongs to physical and chemical inspection technical field, and in particular to the assay method of diisopropyl naphthalene in cigarette tipping paper.
Background technology
Diisopropyl naphthalene has outstanding advantages of strong to the solvability of dyestuff, and the dyestuff for being used as NCR is molten
The important compound of agent, it is widely used in paper and food contact packing material etc..Because the material can be contained by intake
Fatty foodstuff enters human body and is enriched with human body, is caused a hidden trouble to consumer health.Cigarette tipping paper is used as and human body is direct
The paper material of contact, its security equally merit attention.
At present, China lacks more perfect this kind of material testing standard, and related technology mainly has following two：（1）State
Family inspection and quarantine professional standard SN/T2831-2011《Export food contact material paper and cardboard diisopropyl naphthalene（DIPN）Survey
Determine gas chromatography-mass spectrography》, because part diisopropyl naphthalene isomers can only be realized complete baseline separation by this method, and simultaneously
2,6- DIPN, 2,7- DIPN, the isomers such as 1,6- DIPN and Isosorbide-5-Nitrae-DIPN can not be realized that baseline is kept completely separate.Therefore,
It is larger to be easily caused quantitative calculating mistiming difference；（2）《The detection method of 2,6- diisopropyl naphthalenes residual quantity in a kind of food》（Publication number
CN 106053694 A）With《The detection method of 2,6- diisopropyl naphthalenes residual quantity in food》（Publication number： CN105301133A）
The only detection to 2,6-DIPN residual quantity in food, testing result can not represent diisopropyl naphthalene other isomeries
Content of the body in food.Therefore, there is larger one-sidedness in its result, and sample treatment cycle length, detection efficiency are low.
The content of the invention
The purpose of the present invention is：A kind of assay method of diisopropyl naphthalene in cigarette tipping paper is provided, Accurate Determining cigarette is used
The content of diisopropyl naphthalene in tipping paper, the quality of cigarette tipping paper is better controled over, reduce product quality risk.
The technical solution of the present invention is that the assay method of diisopropyl naphthalene in the cigarette tipping paper comprises the following steps：
（1）Prepare internal standard working solution：Using anthracene-d10 as internal standard compound, make extractant with dichloromethane, preparation concentration is 50 μ g/mL
Internal standard storing solution；2mL internal standards storing solution accurately is pipetted in 10mL volumetric flasks, dchloromethane and constant volume, obtains the μ g/ of concentration 10
ML internal standard working solutions；
（2）Prepare Standard Stock solutions：Using diisopropyl naphthalene as standard items, make solvent with dichloromethane, preparation concentration is 1000 μ
G/mL Standard Stock solutions；
（3）Configuration standard solution：1mL Standard Stock solutions are pipetted into 100mL volumetric flasks, dchloromethane and constant volume, are obtained
10 μ g/mL standard liquids；
（4）Sample pre-treatments and analysis：The certain cigarette tipping paper sample of precise, add a certain amount of dichloromethane extraction
Agent simultaneously accurately adds quantitative internal standard working solution, oscillation extraction；Part extract is extracted, after SPE column purification, from
Heart scavenging solution, crosses organic membrane filter, and filtrate determines for GC-MS；
（5）The drafting of standard working curve：Accurately pipette 50 μ L respectively, 100 μ L, 200 μ L, 300 μ L, 500 μ L steps（3）Mark
Quasi- solution is separately added into 0.1 μ L internal standard working solutions in 10mL volumetric flasks, and dchloromethane is simultaneously settled to 10mL, entered
Sample is analyzed；After GC-MS is analyzed, using the peak area ratio of seven kinds of isomers peak area sums of diisopropyl naphthalene and internal standard compound as horizontal stroke
Coordinate, linear regression analysis is carried out by ordinate of the concentration of seven kinds of diisopropyl naphthalenes in each standard liquid, tries to achieve standard curve
Equation；
（6）Data processing and detection：Inner mark method ration is carried out by the ratio between component peak area and internal standard peak area.
Further, in step（4）In, cigarette tipping paper shreds into 0.5cm × 0.5cm, and sample size is 1.0 g.
Further, in step（4）In, the addition of internal standard working solution and extract is respectively 100 μ L and 20 mL.
Further, in step（4）In, the time of oscillation extraction is 40 min, and rotating speed is 220 r/min.
Further, in step（4）In, extraction column is that 150mg anhydrous magnesium sulfates and the bonding of 25mg N- propyl group ethylenediamine are solid
Determine phase adsorbent（That is PSA）, organic filter membrane is 0.45 μm of teflon membrane filter.
Further, in step（4）With（5）In, the analysis condition of gas-chromatography is：Chromatographic column is DB-17 vitreous silicas
Elastic capillary-column, column parameter are mm × 0.25 μm of 30 m × 0.25；Carrier gas is helium；Constant flow rate is 1mL/min；Sample introduction
Measure 1.0 μ L；Split ratio 30: 1；280 °C of injector temperature；280 °C of transmission line temperature；Heating schedule is 150 °C of initial temperature,
210 °C are increased to 5 °C/min speed and keeps 1min, then are increased to 280 °C with 20 °C/min speed and are kept
15min。
Further, in step（4）With（5）In, mass spectral analysis condition is：Ionization mode is EI sources；Ionizing energy：70
eV；Mass number scope：35~350amu；Ion source temperature：280°C；Level Four bar temperature：150°C；Solvent delay：2min；Inspection
Survey mode：Ion monitoring（SIM）；The quota ion and retention time of each component be respectively：
The beneficial effects of the invention are as follows：
1st, the instrument and equipment used is laboratory conventional analysis equipment, and method is easy to spread, and testing cost is low；
2nd, using dilution inner mark method ration, COMPLEX MIXED objects system Quantitative Separation, the difficulty of purifying is avoided, also overcomes matrix
The influence of effect；
3rd, effectively seven kinds of isomers of object can be kept completely separate, improved using gas chromatography tandem mass spectrometry combined instrument
Quantitative accuracy, measurement result can accurately reflect the content of object in sample；
4th, present invention firstly provides using diisopropyl naphthalene in gas chromatography tandem mass spectrometry combined instrument measure cigarette tipping paper
Analysis method, analyze speed is fast, and repeatability and the rate of recovery are high, suitable for the analysis of batch samples.
Brief description of the drawings
Fig. 1 is diisopropyl naphthalene and interior target extraction ion flow graph in standard liquid；
Fig. 2 is diisopropyl naphthalene and interior target extraction ion flow graph in sample.
Embodiment
For the ease of being better understood from technical scheme, further illustrate, but can not manage with reference to embodiment
Solve to be the limitation to technical scheme.
Embodiment：Diisopropyl naphthalene in cigarette tipping paper is determined according to following steps
（1）Instrument and reagent, material：U.S.'s Agilent 6890A-5975 gas chromatography tandem mass spectrometry combined instruments（GC-MS）；
Agilent DB-17 chromatographic columns（30 m×0.25 mm×0.25μm）；0.45 μm of micropore filtering film, mechnical oscillator；Dichloro
Methane（Chromatographically pure, lark prestige chemical reagents corporation）, diisopropyl naphthalene standard items（German Dr.Ehrenstorfer GmbH are public
Department）, extraction column：150mg anhydrous magnesium sulfates and 25mg N- propyl group ethylenediamine bonded stationary phase adsorbents（That is PSA）（Town in Shanghai is composed
Scientific instrument Co., Ltd）；
（2）Configure internal standard working solution：Using anthracene-d10 as internal standard compound, make extractant with dichloromethane, preparation concentration is 50 μ g/mL
Internal standard storing solution；2mL internal standards storing solution accurately is pipetted in 10mL volumetric flasks, dchloromethane and constant volume, obtains the μ g/ of concentration 10
ML internal standard working solutions；
（3）Configuration standard solution：1mL Standard Stock solutions are pipetted into 100mL volumetric flasks, dchloromethane and constant volume, are obtained
10 μ g/mL standard liquids；
（4）Sample pre-treatments：Accurately weigh 1.0 g（It is accurate to 0.0001g）Cigarette tipping paper sample（Size 0.5cm ×
0.5cm）In 50mL triangular flasks, 100 μ L inner mark solutions and 20 mL dichloromethane extractants are sequentially added, are vibrated（Rotating speed is
220 r/min）40 min are extracted, take 2mL supernatant liquors in containing 150mg anhydrous magnesium sulfates and 25mg N- propyl group ethylenediamine keys
Close stationary phase adsorbent（That is PSA）Centrifuge tube in carry out centrifugation 10min（Rotating speed is 5000 r/min）Afterwards, it is poly- through 0.45 μm
After tetrafluoroethene membrane filtration, filtrate determines for GC-MS；The analysis condition of gas-chromatography is：Chromatographic column is DB-17 vitreous silicas
Elastic capillary-column, column parameter are mm × 0.25 μm of 30 m × 0.25；Carrier gas is helium；Constant flow rate is 1mL/min；Sample introduction
Measure 1.0 μ L；Split ratio 30: 1；280 °C of injector temperature；280 °C of transmission line temperature；Heating schedule is 150 °C of initial temperature,
210 °C are increased to 5 °C/min speed and keeps 1min, then are increased to 280 °C with 20 °C/min speed and are kept
15min；Mass spectral analysis condition is：Ionization mode is EI sources；Ionizing energy：70 eV；Mass number scope：35~350amu；Ion
Source temperature：280°C；Level Four bar temperature：150°C；Solvent delay：2min；Detection mode：Salbutamol Selected Ion Monitoring（SIM）；Each component
Quota ion and retention time be respectively：
The diisopropyl naphthalene isomers of table 1 and interior target quota ion and retention time
（5）The drafting of standard working curve：Accurately pipette 50 μ L respectively, 100 μ L, 200 μ L, 300 μ L, 500 μ L above-mentioned standards are molten
Liquid is separately added into 0.1 μ L internal standard working solutions in 10mL volumetric flasks, and dchloromethane is simultaneously settled to 10mL, sample introduction point
Analysis；After GC-MS is analyzed, using the peak area ratio of seven kinds of isomers peak area sums of diisopropyl naphthalene and internal standard compound as horizontal seat
Mark, linear regression analysis is carried out by ordinate of the concentration of seven kinds of diisopropyl naphthalenes in each standard liquid, tries to achieve standard curve side
Journey；The equation of linear regression of diisopropyl naphthalene, coefficient correlation, detection limit and quantitative limit are as shown in table 2；
Equation of linear regression, coefficient correlation, detection limit and the quantitative limit of the diisopropyl naphthalene of table 2
（6）The measure of actual sample：The method established using the present invention determines diisopropyl naphthalene in 10 cigarette tipping paper samples
Content, the results showed that do not detect diisopropyl naphthalene in 10 samples, be shown in Table 3.
The testing result of diisopropyl naphthalene in the cigarette tipping paper sample of table 3（μg/g）
Note：" N.D. " represents not detect.
Precision：In order to investigate the precision of method, carry out 5 times with certain cigarette tipping paper sample and in a few days repeat to test, survey
Determine result show diisopropyl naphthalene in a few days measurement result the coefficient of variation be 1.14%, show that the withinday precision of method is good；Together
When, sample is carried out to repeat within 5 days to test in the daytime, measurement result shows that the coefficient of variation of diisopropyl naphthalene measurement result in the daytime is
Between 2.37%, the results showed that the repeatability in the daytime of this method is good.
The rate of recovery：Certain cigarette tipping paper sample is carried out on high, medium and low three contents levels using sample mark-on method
The measure of the rate of recovery, the results showed that the average recovery rate result of diisopropyl naphthalene between 96.26%-105.30%, the rate of recovery compared with
Height, meet that analysis requires.
Claims (7)
1. the assay method of diisopropyl naphthalene in cigarette tipping paper, it is characterised in that：This method comprises the following steps：
（1）Prepare internal standard working solution：Using anthracene-d10 as internal standard compound, make extractant with dichloromethane, preparation concentration is 50 μ g/mL
Internal standard storing solution；2mL internal standards storing solution accurately is pipetted in 10mL volumetric flasks, dchloromethane and constant volume, obtains the μ g/ of concentration 10
ML internal standard working solutions；
（2）Prepare Standard Stock solutions：Using diisopropyl naphthalene as standard items, make solvent with dichloromethane, preparation concentration is 1000 μ
G/mL Standard Stock solutions；
（3）Configuration standard solution：1mL Standard Stock solutions are pipetted into 100mL volumetric flasks, dchloromethane and constant volume, are obtained
10 μ g/mL standard liquids；
（4）Sample pre-treatments and analysis：The certain cigarette tipping paper sample of precise, add a certain amount of dichloromethane extraction
Agent simultaneously accurately adds quantitative internal standard working solution, oscillation extraction；Part extract is extracted, after SPE column purification, from
Heart scavenging solution, crosses organic membrane filter, and filtrate determines for GC-MS；
（5）The drafting of standard working curve：Accurately pipette 50 μ L respectively, 100 μ L, 200 μ L, 300 μ L, 500 μ L steps（3）Mark
Quasi- solution is separately added into 0.1 μ L internal standard working solutions in 10mL volumetric flasks, and dchloromethane is simultaneously settled to 10mL, entered
Sample is analyzed；After GC-MS is analyzed, using the peak area ratio of seven kinds of isomers peak area sums of diisopropyl naphthalene and internal standard compound as horizontal stroke
Coordinate, linear regression analysis is carried out by ordinate of the concentration of seven kinds of diisopropyl naphthalenes in each standard liquid, tries to achieve standard curve
Equation；
（6）Data processing and detection：Inner mark method ration is carried out by the ratio between component peak area and internal standard peak area.
2. the assay method of diisopropyl naphthalene in cigarette tipping paper according to claim 1, it is characterised in that：In step
（4）In, cigarette tipping paper shreds into 0.5cm × 0.5cm, and sample size is 1.0 g.
3. the assay method of diisopropyl naphthalene in cigarette tipping paper according to claim 1, it is characterised in that：In step
（4）In, the addition of internal standard working solution and extract is respectively 100 μ L and 20 mL.
4. the assay method of diisopropyl naphthalene in cigarette tipping paper according to claim 1, it is characterised in that：In step
（4）In, the time of oscillation extraction is 40 min, and rotating speed is 220 r/min.
5. the assay method of diisopropyl naphthalene in cigarette tipping paper according to claim 1, it is characterised in that：In step
（4）In, extraction column is 150mg anhydrous magnesium sulfates and 25mg N- propyl group ethylenediamine bonded stationary phase adsorbents（That is PSA）, it is organic
Filter membrane is 0.45 μm of teflon membrane filter.
6. the assay method of diisopropyl naphthalene in cigarette tipping paper according to claim 1, it is characterised in that：In step
（4）With（5）In, the analysis condition of gas-chromatography is：Chromatographic column is DB-17 vitreous silica elastic capillary-columns, column parameter 30
m×0.25 mm×0.25μm；Carrier gas is helium；Constant flow rate is 1mL/min；The μ L of sample size 1.0；Split ratio 30: 1；Sample introduction
280 °C of temperature of mouth；280 °C of transmission line temperature；Heating schedule is 150 °C of initial temperature, and 210 ° are increased to 5 °C/min speed
C simultaneously keeps 1min, then is increased to 280 °C with 20 °C/min speed and keeps 15min.
7. the assay method of diisopropyl naphthalene in cigarette tipping paper according to claim 1, it is characterised in that：In step
（4）With（5）In, mass spectral analysis condition is：Ionization mode is EI sources；Ionizing energy：70 eV；Mass number scope：35~
350amu；Ion source temperature：280°C；Level Four bar temperature：150°C；Solvent delay：2min；Detection mode：Ion monitoring
（SIM）；The quota ion and retention time of each component be respectively：
。
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108051521A (en) * | 2017-12-27 | 2018-05-18 | 浙江中烟工业有限责任公司 | A kind of test method of cigarette tipping paper quality stability |
| CN110376299A (en) * | 2019-06-24 | 2019-10-25 | 杭州市质量技术监督检测院 | The measuring method of diisopropyl naphthalene the amount of migration in silicone oil paper |
| CN111308003A (en) * | 2020-02-27 | 2020-06-19 | 福建中烟工业有限责任公司 | Method for simultaneously detecting diisopropylnaphthalenes, polychlorinated biphenyls, phthalate compounds and photoinitiator |
| CN114384163A (en) * | 2021-10-27 | 2022-04-22 | 江苏美思德化学股份有限公司 | Method for separating and detecting dipropylene glycol isomer |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108051521A (en) * | 2017-12-27 | 2018-05-18 | 浙江中烟工业有限责任公司 | A kind of test method of cigarette tipping paper quality stability |
| CN110376299A (en) * | 2019-06-24 | 2019-10-25 | 杭州市质量技术监督检测院 | The measuring method of diisopropyl naphthalene the amount of migration in silicone oil paper |
| CN111308003A (en) * | 2020-02-27 | 2020-06-19 | 福建中烟工业有限责任公司 | Method for simultaneously detecting diisopropylnaphthalenes, polychlorinated biphenyls, phthalate compounds and photoinitiator |
| CN111308003B (en) * | 2020-02-27 | 2022-11-08 | 福建中烟工业有限责任公司 | Method for simultaneously detecting diisopropylnaphthalenes, polychlorinated biphenyls, phthalate compounds and photoinitiator |
| CN114384163A (en) * | 2021-10-27 | 2022-04-22 | 江苏美思德化学股份有限公司 | Method for separating and detecting dipropylene glycol isomer |
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