CN107389811B - Method for measuring diisopropyl naphthalene in cigarette tipping paper - Google Patents
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Abstract
The invention discloses a method for measuring diisopropyl naphthalene in tipping paper for cigarettes, which comprises the steps of taking dichloromethane as an extraction liquid, carrying out oscillation extraction on a tipping paper sample for cigarettes, then transferring the extraction liquid, purifying by a solid phase extraction column, centrifuging a purified liquid, filtering by an organic membrane, and measuring the diisopropyl naphthalene in the tipping paper for cigarettes by adopting a gas chromatography-tandem mass spectrometry combined method. The dilution internal standard method quantitatively avoids the difficulty of quantitative separation and purification of a complex mixture system and also overcomes the influence of matrix effect; the gas chromatography-tandem mass spectrometer is adopted to effectively realize the complete baseline separation of seven isomers of the target object, so that the quantitative accuracy is improved, and the determination result can accurately reflect the content of the target object in the sample; the method adopts direct sample injection, can quickly and accurately detect the content of the diisopropyl naphthalene in the tipping paper for cigarettes, has good repeatability and recovery rate, and is suitable for analysis of large batches of samples.
Description
Technical Field
The invention belongs to the technical field of physicochemical inspection, and particularly relates to a method for measuring diisopropyl naphthalene in tipping paper for cigarettes.
Background
Diisopropyl naphthalene has the outstanding advantages of strong dye dissolving capacity and the like, is an important compound used as a dye solvent for carbonless copy paper, and is widely applied to the aspects of paper, food contact packaging materials and the like. Since the substance enters the human body by ingestion of fat-containing food and is enriched in the human body, it poses a health risk to consumers. The cigarette tipping paper is taken as a paper material which is in direct contact with the human body, and the safety of the cigarette tipping paper is also worth paying attention.
At present, China lacks a relatively perfect inspection standard for such substances, and the related technologies mainly comprise the following two types: (1) the national inspection and quarantine industry standard SN/T2831-2011 & lt & ltExit food contact Material paper & cardboard Diisopropylnaphthalene (DIPN) determination gas chromatography-mass spectrometry & gt, because the method can only realize complete baseline separation on partial diisopropylnaphthalene isomers, but cannot realize complete baseline separation on isomers such as 2, 6-DIPN, 2, 7-DIPN, 1, 6-DIPN, 1, 4-DIPN and the like. Therefore, the error is easy to be larger during quantitative calculation; (2) both a method for detecting the residual amount of 2, 6-diisopropylnaphthalene in food (publication No. CN 106053694A) and a method for detecting the residual amount of 2, 6-diisopropylnaphthalene in food (publication No. CN 105301133A) only detect the residual amount of 2, 6-diisopropylnaphthalene in food, and the detection results cannot represent the content of other isomers of diisopropylnaphthalene in food. Therefore, the result is large one-sidedness, and the sample treatment cycle is long, resulting in low detection efficiency.
Disclosure of Invention
The purpose of the invention is: the method for measuring the diisopropyl naphthalene in the cigarette tipping paper is provided, the content of the diisopropyl naphthalene in the cigarette tipping paper is accurately measured, the quality of the cigarette tipping paper is better controlled, and the product quality risk is reduced.
The technical scheme of the invention is that the method for measuring the diisopropyl naphthalene in the tipping paper for the cigarette comprises the following steps:
(1) preparing an internal standard working solution: preparing an internal standard stock solution with the concentration of 50 mug/mL by using anthracene-d 10 as an internal standard substance and using dichloromethane as an extracting agent; accurately transferring 2mL of internal standard stock solution into a 10mL volumetric flask, diluting with dichloromethane and fixing the volume to obtain internal standard working solution with the concentration of 10 mug/mL;
(2) preparing a standard stock solution: using diisopropylnaphthalene as a standard substance and dichloromethane as a solvent to prepare a standard stock solution with the concentration of 1000 mug/mL;
(3) preparing a standard solution: transferring 1mL of standard stock solution into a 100mL volumetric flask, diluting with dichloromethane and fixing the volume to obtain 10 mu g/mL of standard solution;
(4) sample pretreatment and analysis: accurately weighing a certain sample of the tipping paper for the cigarette, adding a certain amount of dichloromethane extractant and accurately adding a certain amount of internal standard working solution, and performing oscillation extraction; extracting part of the extract, purifying by a solid phase extraction column, centrifuging the purified solution, filtering by an organic membrane, and determining the filtrate by GC-MS;
(5) drawing a standard working curve: accurately transferring the standard solution of the step (3) of 50 muL, 100 muL, 200 muL, 300 muL and 500 muL into a 10mL volumetric flask, respectively adding 0.1 muL internal standard working solution, diluting with dichloromethane, and performing constant volume to 10mL, and performing sample injection analysis; after GC-MS analysis, taking the peak area ratio of the sum of seven isomers of the diisopropylnaphthalene to the peak area of an internal standard substance as a horizontal coordinate, and taking the concentration of the seven diisopropylnaphthalenes in each standard solution as a vertical coordinate to carry out linear regression analysis to obtain a standard curve equation;
(6) data processing and detection: and (4) carrying out internal standard method quantification by the ratio of the component peak area to the internal standard peak area.
Further, in the step (4), the tipping paper for cigarettes is cut into pieces of 0.5cm × 0.5cm, and the sample amount is 1.0 g.
Further, in the step (4), the adding amounts of the internal standard working solution and the extraction liquid are 100 μ L and 20 mL respectively.
Further, in the step (4), the time of shaking extraction is 40 min, and the rotating speed is 220 r/min.
Further, in the step (4), the extraction column was 150mg of anhydrous magnesium sulfate and 25mg of N-propylethylenediamine bonded stationary phase adsorbent (i.e., PSA), and the organic filtration membrane was a 0.45 μm polytetrafluoroethylene filtration membrane.
Further, in steps (4) and (5), the analysis conditions of the gas chromatography are: the chromatographic column is a DB-17 fused silica elastic capillary column, and the column parameters are 30 m multiplied by 0.25 mm multiplied by 0.25 mu m; the carrier gas is helium; the constant flow rate is 1 mL/min; the sample injection amount is 1.0 mu L; the split ratio is 30: 1; the temperature of a sample inlet is 280 ℃; transmission line temperature 280 ℃; the temperature rise program is an initial temperature of 150 ℃, the temperature rises to 210 ℃ at the rate of 5 ℃/min and is kept for 1min, and then the temperature rises to 280 ℃ at the rate of 20 ℃/min and is kept for 15 min.
Further, in steps (4) and (5), the mass spectrometry conditions are: the ionization mode is an EI source; ionization energy: 70 eV; mass number range: 35-350 amu; ion source temperature: 280 ℃; quadrupole temperature: 150 ℃; solvent retardation: 2 min; the detection mode is as follows: ion Monitoring (SIM); the quantitative ions and retention time of each component are respectively as follows:
the invention has the beneficial effects that:
1. the used instruments and equipment are conventional laboratory analysis equipment, the method is easy to popularize, and the detection cost is low;
2. the dilution internal standard method is adopted for quantification, so that the difficulty of quantitative separation and purification of a complex mixture system is avoided, and the influence of matrix effect is overcome;
3. the seven isomers of the target can be effectively and completely separated by adopting a gas chromatography-tandem mass spectrometer, the quantitative accuracy is improved, and the content of the target in the sample can be accurately reflected by the determination result;
4. the invention firstly provides an analysis method for measuring the diisopropyl naphthalene in the tipping paper for cigarettes by adopting a gas chromatography-tandem mass spectrometer, has high analysis speed and high repeatability and recovery rate, and is suitable for analyzing mass samples.
Drawings
FIG. 1 is a graph of extracted ion flow of diisopropylnaphthalene and internal standard in a standard solution;
FIG. 2 is an extracted ion flow graph of diisopropylnaphthalene and internal standard in a sample.
Detailed Description
In order to facilitate better understanding of the technical solutions of the present invention, the following examples are further described, but the technical solutions are not to be construed as being limited thereto.
Example (b): the determination of diisopropyl naphthalene in the tipping paper for cigarette is carried out according to the following steps
(1) Instruments and reagents, materials: agilent 6890A-5975 gas chromatography-tandem mass spectrometry (GC-MS) USA; agilent DB-17 column (30 m.times.0.25 mm. times.0.25 μm); 0.45 μm microporous filter membrane, mechanical oscillator; dichloromethane (chromatographically pure, carbofuran chemicals), diisopropylnaphthalene standard (dr. ehrenstorfer GmbH, germany), extraction column: 150mg of anhydrous magnesium sulfate and 25mg of N-propylethylenediamine bonded stationary phase adsorbent (i.e., PSA) (Shanghai' an Spectrum scientific instruments, Inc.);
(2) preparing an internal standard working solution: preparing an internal standard stock solution with the concentration of 50 mug/mL by using anthracene-d 10 as an internal standard substance and using dichloromethane as an extracting agent; accurately transferring 2mL of internal standard stock solution into a 10mL volumetric flask, diluting with dichloromethane and fixing the volume to obtain internal standard working solution with the concentration of 10 mug/mL;
(3) preparing a standard solution: transferring 1mL of standard stock solution into a 100mL volumetric flask, diluting with dichloromethane and fixing the volume to obtain 10 mu g/mL of standard solution;
(4) sample pretreatment: accurately weighing 1.0 g (accurate to 0.0001 g) of a cigarette tipping paper sample (0.5 cm multiplied by 0.5cm in size) in a 50mL triangular flask, sequentially adding 100 muL of internal standard solution and 20 mL of dichloromethane extractant, performing oscillation (rotating speed of 220 r/min) extraction for 40 min, taking 2mL of supernatant, centrifuging for 10min (rotating speed of 5000 r/min) in a centrifuge tube containing 150mg of anhydrous magnesium sulfate and 25mg of N-propyl ethylenediamine bonded stationary phase adsorbent (namely PSA), filtering by a 0.45 mu m polytetrafluoroethylene filter membrane, and determining the filtrate by GC-MS; the analysis conditions of the gas chromatograph were: the chromatographic column is a DB-17 fused quartz elastic capillary column, and the column parameters are 30 m multiplied by 0.25 mm multiplied by 0.25 mu m; the carrier gas is helium; the constant flow rate is 1 mL/min; the sample injection amount is 1.0 mu L; the split ratio is 30: 1; the temperature of a sample inlet is 280 ℃; transmission line temperature 280 ℃; the temperature rise program is that the initial temperature is 150 ℃, the temperature is raised to 210 ℃ at the speed of 5 ℃/min and is kept for 1min, and then the temperature is raised to 280 ℃ at the speed of 20 ℃/min and is kept for 15 min; the mass spectrometry conditions were: the ionization mode is an EI source; ionization energy: 70 eV; mass number range: 35-350 amu; ion source temperature: 280 ℃; quadrupole temperature: 150 ℃; solvent retardation: 2 min; the detection mode is as follows: selective Ion Monitoring (SIM); the quantitative ions and retention time of each component are respectively as follows:
TABLE 1 quantitation of diisopropyl naphthalene isomers and internal standards and retention time
(5) Drawing a standard working curve: accurately transferring the standard solutions of 50 muL, 100 muL, 200 muL, 300 muL and 500 muL into a 10mL volumetric flask, respectively adding 0.1 muL internal standard working solution, diluting with dichloromethane, and performing constant volume to 10mL, and performing sample injection analysis; after GC-MS analysis, taking the peak area ratio of the sum of seven isomers of the diisopropylnaphthalene to the peak area of an internal standard substance as a horizontal coordinate, and taking the concentration of the seven diisopropylnaphthalenes in each standard solution as a vertical coordinate to carry out linear regression analysis to obtain a standard curve equation; the linear regression equation, correlation coefficient, detection limit and quantification limit of diisopropylnaphthalene are shown in table 2;
TABLE 2 Linear regression equation, correlation coefficient, detection limit, and quantitation limit for diisopropylnaphthalene
(6) Determination of the actual sample: the content of the diisopropyl naphthalene in 10 cigarette tipping paper samples is determined by the method established by the invention, and the result shows that the diisopropyl naphthalene is not detected in 10 samples, which is shown in table 3.
TABLE 3 detection results (μ g/g) of diisopropylnaphthalene in tipping paper samples for cigarettes
Note: "n.d." means not detected.
Precision: in order to investigate the precision of the method, a certain tipping paper sample for cigarettes is subjected to repeated experiments within 5 days, and the measurement result shows that the variation coefficient of the measurement result in the day of the diisopropylnaphthalene is 1.14 percent, which shows that the precision of the method in the day is good; meanwhile, repeated experiments are carried out on the sample for 5 days, the measurement result shows that the variation coefficient of the measurement result of the diisopropyl naphthalene in the daytime is 2.37%, and the result shows that the repeatability of the method in the daytime is good.
And (3) recovery rate: the sample labeling method is adopted to measure the recovery rate of a certain cigarette tipping paper sample on the high, medium and low content levels, and the result shows that the average recovery rate result of the diisopropylnaphthalene is 96.26-105.30%, the recovery rate is high, and the analysis requirement is met.
Claims (1)
1. The method for measuring diisopropyl naphthalene in the tipping paper for cigarettes comprises the following steps:
(1) preparing an internal standard working solution: preparing an internal standard stock solution with the concentration of 50 mug/mL by using anthracene-d 10 as an internal standard substance and using dichloromethane as an extracting agent; accurately transferring 2mL of internal standard stock solution into a 10mL volumetric flask, diluting with dichloromethane and fixing the volume to obtain internal standard working solution with the concentration of 10 mug/mL;
(2) preparing a standard stock solution: using diisopropylnaphthalene as a standard substance and dichloromethane as a solvent to prepare a standard stock solution with the concentration of 1000 mug/mL;
(3) preparing a standard solution: transferring 1mL of standard stock solution into a 100mL volumetric flask, diluting with dichloromethane and fixing the volume to obtain 10 mu g/mL of standard solution;
(4) sample pretreatment and analysis: accurately weighing a certain sample of the tipping paper for the cigarette, adding a certain amount of dichloromethane extractant and accurately adding a certain amount of internal standard working solution, and performing oscillation extraction; extracting part of the extract, purifying by a solid phase extraction column, centrifuging the purified solution, filtering by an organic membrane, and determining the filtrate by GC-MS;
(5) drawing a standard working curve: accurately transferring the standard solution of the step (3) of 50 muL, 100 muL, 200 muL, 300 muL and 500 muL into a 10mL volumetric flask, respectively adding 0.1 muL internal standard working solution, diluting with dichloromethane, and performing constant volume to 10mL, and performing sample injection analysis; after GC-MS analysis, taking the peak area ratio of the sum of seven isomers of the diisopropylnaphthalene to the peak area of an internal standard substance as a horizontal coordinate, and taking the concentration of the seven diisopropylnaphthalenes in each standard solution as a vertical coordinate to carry out linear regression analysis to obtain a standard curve equation;
(6) data processing and detection: carrying out internal standard method quantification by the ratio of the component peak area to the internal standard peak area;
the method is characterized in that:
in step (4): cutting the cigarette tipping paper into pieces of 0.5cm multiplied by 0.5cm, wherein the sample amount is 1.0 g; adding amounts of the internal standard working solution and the extraction liquid are respectively 100 muL and 20 mL; the oscillating extraction time is 40 min, and the rotating speed is 220 r/min; the extraction column is 150mg of anhydrous magnesium sulfate and 25mg of N-propyl ethylenediamine bonded stationary phase adsorbent (namely PSA), and the organic filter membrane is a 0.45 mu m polytetrafluoroethylene filter membrane;
in steps (4) and (5), the analysis conditions of the gas chromatography are: the chromatographic column is a DB-17 fused silica elastic capillary column, and the column parameters are 30 m multiplied by 0.25 mm multiplied by 0.25 mu m; the carrier gas is helium; the constant flow rate is 1 mL/min; the sample injection amount is 1.0 mu L; the split ratio is 30: 1; the temperature of a sample inlet is 280 ℃; transmission line temperature 280 ℃; the temperature rise program is that the initial temperature is 150 ℃, the temperature is raised to 210 ℃ at the speed of 5 ℃/min and is kept for 1min, and then the temperature is raised to 280 ℃ at the speed of 20 ℃/min and is kept for 15 min;
in steps (4) and (5), the mass spectrometry conditions are: the ionization mode is an EI source; ionization energy: 70 eV; mass number range: 35-350 amu; ion source temperature: 280 ℃; quadrupole temperature: 150 ℃; solvent retardation: 2 min; the detection mode is as follows: ion Monitoring (SIM); the quantitative ions and retention time of each component are respectively as follows:
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| 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 |
| 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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| CN101130481B (en) * | 2006-08-25 | 2013-01-30 | 北京石油化工学院 | Process for the separation of 2, 6- isopropyl naphthalene and 2, 7- isopropyl naphthalene |
| CN102998381A (en) * | 2012-10-17 | 2013-03-27 | 国家烟草质量监督检验中心 | Method for measuring content of phthalic acid ester in tipping paper for cigarettes |
| CN105301133B (en) * | 2015-11-12 | 2017-08-25 | 中华人民共和国张家口出入境检验检疫局 | The detection method of 2,6 diisopropyl naphthalene residual quantities in food |
| CN106053694A (en) * | 2016-06-23 | 2016-10-26 | 福清出入境检验检疫局综合技术服务中心 | Method for detecting residual amount of 2,6-diisopropylnaphthalene in food |
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