CN115406983A - Method for measuring breaking time of blasting beads in cigarette filter - Google Patents
Method for measuring breaking time of blasting beads in cigarette filter Download PDFInfo
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- 239000011324 bead Substances 0.000 title claims abstract description 86
- 235000019504 cigarettes Nutrition 0.000 title claims abstract description 76
- 238000005422 blasting Methods 0.000 title claims abstract description 59
- 238000000034 method Methods 0.000 title claims abstract description 28
- 239000000523 sample Substances 0.000 claims abstract description 48
- 230000008859 change Effects 0.000 claims abstract description 24
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- 239000000463 material Substances 0.000 claims description 17
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- XHXUANMFYXWVNG-UHFFFAOYSA-N D-menthyl acetate Natural products CC(C)C1CCC(C)CC1OC(C)=O XHXUANMFYXWVNG-UHFFFAOYSA-N 0.000 claims description 14
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 14
- 238000012360 testing method Methods 0.000 claims description 14
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- 239000012074 organic phase Substances 0.000 claims description 8
- 125000005456 glyceride group Chemical group 0.000 claims description 7
- 239000012528 membrane Substances 0.000 claims description 7
- WWZKQHOCKIZLMA-UHFFFAOYSA-N octanoic acid Chemical compound CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 7
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- 238000001914 filtration Methods 0.000 claims description 6
- 238000004587 chromatography analysis Methods 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 4
- 230000005540 biological transmission Effects 0.000 claims description 3
- 239000012159 carrier gas 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
- 239000010453 quartz Substances 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 2
- 239000011148 porous material Substances 0.000 claims description 2
- PHALYIWLKRSLME-UHFFFAOYSA-N decanoic acid;2,3-dihydroxypropyl octanoate Chemical compound CCCCCCCCCC(O)=O.CCCCCCCC(=O)OCC(O)CO PHALYIWLKRSLME-UHFFFAOYSA-N 0.000 claims 1
- 229940061567 glyceryl caprylate-caprate Drugs 0.000 claims 1
- 238000003860 storage Methods 0.000 abstract description 17
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- 238000002546 full scan Methods 0.000 abstract description 3
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- NOOLISFMXDJSKH-UTLUCORTSA-N (+)-Neomenthol Chemical compound CC(C)[C@@H]1CC[C@@H](C)C[C@@H]1O NOOLISFMXDJSKH-UTLUCORTSA-N 0.000 description 1
- LKUNXBRZDFMZOK-GFCCVEGCSA-N Capric acid monoglyceride Natural products CCCCCCCCCC(=O)OC[C@H](O)CO LKUNXBRZDFMZOK-GFCCVEGCSA-N 0.000 description 1
- NOOLISFMXDJSKH-UHFFFAOYSA-N DL-menthol Natural products CC(C)C1CCC(C)CC1O NOOLISFMXDJSKH-UHFFFAOYSA-N 0.000 description 1
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- 238000004817 gas chromatography Methods 0.000 description 1
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- 238000011068 loading method Methods 0.000 description 1
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- LKUNXBRZDFMZOK-UHFFFAOYSA-N rac-1-monodecanoylglycerol Chemical compound CCCCCCCCCC(=O)OCC(O)CO LKUNXBRZDFMZOK-UHFFFAOYSA-N 0.000 description 1
- 230000000391 smoking effect Effects 0.000 description 1
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- 229940093609 tricaprylin Drugs 0.000 description 1
- VLPFTAMPNXLGLX-UHFFFAOYSA-N trioctanoin Chemical compound CCCCCCCC(=O)OCC(OC(=O)CCCCCCC)COC(=O)CCCCCCC VLPFTAMPNXLGLX-UHFFFAOYSA-N 0.000 description 1
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Classifications
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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
-
- 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
- G01N30/62—Detectors specially adapted therefor
- G01N30/72—Mass spectrometers
-
- 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
- G01N30/86—Signal analysis
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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
- G01N30/86—Signal analysis
- G01N30/8665—Signal analysis for calibrating the measuring apparatus
-
- 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
- G01N30/86—Signal analysis
- G01N30/8675—Evaluation, i.e. decoding of the signal into analytical information
-
- 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
- G01N30/86—Signal analysis
- G01N30/8675—Evaluation, i.e. decoding of the signal into analytical information
- G01N30/8686—Fingerprinting, e.g. without prior knowledge of the sample components
-
- 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
- G01N30/86—Signal analysis
- G01N30/8696—Details of Software
Abstract
The invention discloses a method for measuring the breaking time of blasting beads in a cigarette filter, which comprises the following steps: extracting a cigarette sample after the exploded beads are crushed to prepare a sample solution; analyzing and processing the sample solution by GC-MS to obtain an SIM (subscriber identity module) diagram of the sample solution; and (4) quantifying the ion peak area according to a calibration object in the SIM map to obtain a calibration value, and comparing the calibration value with a preset standard change curve to obtain the time for breaking the sample when the sample explodes the bead. Carrying out full-scan analysis on the contents of the blasting beads by using GC-MS (gas chromatography-mass spectrometry), and selecting a characteristic peak as a calibration substance; secondly, the cigarette sample after bead blasting is manually crushed, and the change curve of the content of the calibration object along with the storage time is inspected; by means of the curve, after the actual bead blasting and crushing cigarette sample is analyzed, the approximate time of bead blasting and crushing can be quickly judged, and therefore data support is provided for quality complaint analysis and product quality maintenance of the bead blasting cigarettes after delivery.
Description
Technical Field
The invention relates to a method for measuring the bead blasting crushing time in a cigarette filter, and belongs to the technical field of quality control of bead blasting cigarettes.
Background
The cigarette blasting bead is prepared by loading tobacco essence, perfume, additive, solvent, etc. into sealed blasting bead, and breaking the blasting bead to release the contained substances under the action of external force during smoking. The bead-blasting perfuming is an important way for perfuming cigarette, which not only can keep the stability of perfume materials, reduce volatilization and increase retention effect, but also can avoid the problems of flavor change and the like caused by high-temperature combustion of the cigarette.
Many researches on bead-blasting cigarettes are already carried out, and the researches mainly focus on the technical fields of stable quality of bead-blasting inclusion, online detection of bead-blasting capsules and the like. Quality and quality, and the like, by adopting a method of GC-MS analysis after n-hexane extraction, different batches of samples of different cigarette blasting beads are analyzed, a GC-MS fingerprint of contents of the blasting beads for cigarettes is established, and the quality stability of the contents of the blasting beads is evaluated by various statistical analysis means. Gong Shi Wen and the like design a capsule filter stick quality detection device based on a microwave resonant cavity perturbation method, and the rapid detection of three conditions such as bead blasting loss, position deviation and breakage is realized. Wangwei et al discloses an intelligent detection method for cigarette capsule damage defects based on Fisher discriminant analysis and Mahalanobis distance variation degree, which can accurately judge whether a cigarette capsule is damaged or not. However, most of the analyses are focused on the production of the exploded beads and the processing process of cigarettes, and the effective analysis on the crushing time of the exploded beads in the storage, transportation and use processes of the exploded bead cigarettes after leaving factories is not available.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide the method for measuring the breaking time of the exploded beads in the cigarette filter, which can quickly and accurately judge the breaking time of the exploded beads.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for measuring the breaking time of blasting beads in a cigarette filter comprises the following steps:
extracting a cigarette sample after the exploded beads are crushed to prepare a sample solution;
analyzing and processing the sample solution by GC-MS to obtain an SIM (subscriber identity module) diagram of the sample solution;
and (4) quantifying the ion peak area according to a calibration object in the SIM map to obtain a calibration value, and comparing the calibration value with a preset standard change curve to obtain the time for breaking the sample when the sample explodes the bead.
Further, the preparation method of the sample solution comprises the following steps:
taking a cigarette sample after the exploded beads are broken, tearing the sample, adding an extraction liquid for extraction, standing the sample, taking a supernatant, and filtering the supernatant through an organic phase filter membrane to obtain a sample solution.
Further, the extraction liquid is n-hexane.
Further, the pore diameter of the organic phase filtration membrane is 0.45 μm.
Further, the calibration object comprises a first volatile calibration object and a second nonvolatile calibration object in the cigarette blasting bead, and the calibration value is the quantitative ion peak area ratio of the first calibration object to the second calibration object in the SIM image.
Further, the first calibration material is menthyl acetate, and the second calibration material is caprylic/capric glyceride.
Further, the method for formulating the pre-formulated standard change curve comprises the following steps:
taking a plurality of test samples in the same batch with the sample to be tested, breaking the exploded beads of the test samples, storing at room temperature, calculating the calibration value of the test samples at a plurality of time nodes, and drawing a standard change curve of the calibration value-time.
Further, GC analysis was performed using a DB-5MS elastic quartz capillary chromatography column.
Further, the GC chromatographic analysis adopts a temperature programming method, and the temperature programming conditions are as follows: the initial temperature is 60 ℃, the temperature is kept for 1min, then the temperature is increased to 200 ℃ at 10 ℃/min, the temperature is kept for 2min, the temperature is increased to 300 ℃ at 5 ℃/min, and the temperature is kept for 5min; the flow splitting ratio is 5; carrier gas: helium gas with a purity of 99.999%; a constant flow mode, wherein the flow rate is 1.0mL/min; the total run time was 42min.
Further, the MS conditions are: ionization energy 70eV; filament current: 35 muA; ion source temperature: 230 ℃; quadrupole rod temperature: 150 ℃; transmission line temperature: 280. DEG C; delaying the solvent for 5min; the scanning mode is as follows: SIM selects ion scanning, the first calibration material menthyl acetate has the quantitative ion of 138, and the qualitative ions of 123, 95; the second calibration material, caprylic capric glyceride, had a quantitative ion of 355 and qualitative ions of 327, 127, 155.
Compared with the prior art, the invention has the following beneficial effects:
(1) Carrying out full-scan analysis on the contents of the blasting beads by using GC-MS (gas chromatography-mass spectrometry), and selecting a characteristic peak as a calibration substance; secondly, the cigarette sample after the bead blasting is manually broken is inspected for the change curve of the content of the calibration object along with the storage time; by means of the curve, after the actual bead blasting broken cigarette sample is analyzed, the approximate time of bead blasting breakage can be quickly judged, and therefore data support is provided for quality complaint analysis and product quality maintenance of ex-factory bead blasting cigarettes;
(2) Volatile menthyl acetate is selected as a first calibration material, a nonvolatile solvent of caprylic/capric glyceride is stable, the volatile solvent is used as a second calibration material, the peak area ratio of the quantitative ions of the menthyl acetate and the caprylic/capric glyceride is provided as a calibration value and is used as a vertical coordinate of a content change curve, the stability of a GC-MS instrument can be corrected, the step of adding an internal standard is omitted, a standard product and a reference sample are not needed, and the rapid judgment is really realized;
(3) The two conditions of sealed storage and open storage are inspected through the content change of the calibration substances after bead blasting and crushing, two actual states of non-unsealing of the cigarette carton and loose cigarette storage are simulated, and the correlation coefficient R of a standard change curve model under the two conditions 2 Are all larger than 0.95, and the test accuracy is high.
Drawings
FIG. 1 is a flow chart of the assay method of the present invention;
FIG. 2 is a full scan chromatogram of a sample of an explosive content;
FIG. 3 is a graph showing the standard change of the seal of the first embodiment;
FIG. 4 is a graph showing a standard change in open storage in the second embodiment.
Detailed Description
The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
For the purposes of the present specification and appended claims, unless otherwise indicated, all numbers expressing quantities, percentages or proportions, and other numerical values used in the specification and appended claims, are to be understood as being modified in all instances by the term "about". Moreover, all ranges disclosed herein are inclusive of the endpoints and independently combinable.
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below.
As shown in fig. 1, a method for measuring the breaking time of blasting beads in a cigarette filter specifically comprises the following steps:
extracting a cigarette sample after the exploded beads are crushed to prepare a sample solution;
analyzing and processing the sample solution by GC-MS to obtain an SIM (subscriber identity module) diagram of the sample solution;
and quantifying the ion peak area according to a calibration object in the SIM map to obtain a calibration value, and comparing the calibration value with a preset standard change curve to obtain the time for breaking the sample after blasting the beads.
The preparation method of the sample solution comprises the following steps:
tearing a cigarette sample after the blasting beads are broken, adding n-hexane for extraction, standing, taking supernate, filtering the supernate with a 0.45 mu m organic phase filter membrane to obtain a sample solution, and storing the sample solution in a chromatographic small bottle for later use.
The selection of the calibration object is based on specific components in the bead-exploded cigarette, at least two calibration objects are selected, the calibration objects comprise at least one volatile calibration object and at least one non-volatile calibration object in the bead-exploded cigarette, two calibration objects are adopted in the invention, the calibration objects comprise a first volatile calibration object and a second non-volatile calibration object, and the calibration value is the quantitative ion peak area ratio of the first calibration object and the second calibration object in an SIM (subscriber identity module) diagram.
In the invention, the method for making the pre-made standard change curve comprises the following steps:
taking a plurality of test samples in the same batch with the sample to be tested, breaking the exploded beads of the test samples, storing at room temperature, calculating the calibration value of the test samples at a plurality of time nodes, and drawing a standard change curve of the calibration value-time.
The first embodiment is as follows:
in this example, the employed bead-exploded cigarette is a brand a bead-exploded cigarette, and a bead-exploded cigarette sample #1 (which is stored in a sealed state for a certain period of time after bead-explosion) is from cigarette in zhejiang.
Instruments and reagents used: 7890B-5975C GC (Agilent, USA); an HY-8 adjustable-speed oscillator (Changzhou Guohua electric Co., ltd.); n-hexane (chromatographically pure, dikma corporation); 0.45 μm organic phase filter (Dikma).
1. Preparation of blasting bead inclusion solution and cigarette sample solution
Solution of contents of bead blasting: taking 0.1g of a sample of the bead blasting particles, manually crushing the sample, placing the crushed sample in a 50mL conical flask, adding 20mL of n-hexane, oscillating and extracting for 20min, standing the mixture to take supernatant, filtering the supernatant through a 0.45 mu m organic phase filter membrane, and storing the supernatant in a 2mL chromatographic vial for later use.
Cigarette sample solution: taking 1 cigarette sample after breaking the exploded bead, tearing the sample, placing the sample in a 50mL conical flask, adding 20mL n-hexane, oscillating and extracting for 20min, standing the sample, taking supernate, filtering the supernate with a 0.45 mu m organic phase filter membrane, and storing the supernate in a 2mL chromatographic vial for later use.
2. Determination of GC-MS conditions
The chromatographic conditions are-chromatographic column: DB-5MS elastic quartz capillary chromatographic column (30 m × 0.25mm × 0.25 μm); sample inlet temperature: 250 ℃; temperature programming: the initial temperature is 60 ℃, the temperature is kept for 1min, then the temperature is increased to 200 ℃ at the speed of 10 ℃/min, the temperature is kept for 2min, the temperature is increased to 300 ℃ at the speed of 5 ℃/min, and the temperature is kept for 5min; the flow splitting ratio is 5; carrier gas: helium (99.999% pure); a constant flow mode, wherein the flow rate is 1.0mL/min; the total run time was 42min.
The mass spectrum condition is-ionization energy 70eV; filament current: 35 muA; ion source temperature: 230 ℃; quadrupole rod temperature: 150 ℃; transmission line temperature: 280. DEG C; delaying the solvent for 5min; the scanning mode comprises the following steps: full Scan (Scan), scan range 40-500amu.
3. Determination of calibration object
On-machine test was performed on the solution of the contents of the popped beads to obtain a TIC spectrum obtained by scanning the contents of the popped beads, as shown in FIG. 2, the main flavor components contained in the popped beads are menthol (8.28 min) and menthyl acetate (9.84 min). Three peaks with later peak appearance and higher response are bead blasting solvent peaks, and are qualitatively confirmed to be tricaprylin, dicaprylin monocaprate and dicaprylin monocaprate (collectively called as caprylic/capric glyceride) through literature retrieval and a spectrum library, and the five detected characteristic peaks are subjected to GC-MS-SIM scanning method established by selecting menthyl acetate (9.84 min) and dicaprylin monocaprate (36.41 min) as calibration substances according to the principles of high response, good specificity and wide coverage. Wherein, the quantitative ion of the first calibration material menthyl acetate is 138, and the qualitative ion is 123, 95; the second calibrator glyceryl monocaprate had a quantitative ion of 355 and qualitative ions of 327, 127, 155.
4. Drawing a standard change curve
Selecting 15 groups of bead-exploded cigarette samples of the same kind as the bead-exploded cigarettes to be tested, kneading bead-exploded cigarettes in the bead-exploded cigarette samples, sealing and storing at room temperature, and analyzing the batch of samples respectively at 1 st, 2 nd, 3 th, 5 th, 7 th, 9 th, 12 th, 15 th, 20 th, 25 th, 30 th, 40 th, 50 th, 65 th and 85 th days after bead-exploded. The specific analysis steps are as follows: tearing off the broken cigarettes which are hermetically stored for a certain number of days and subjected to bead blasting, putting the broken cigarettes into a conical flask, performing sample processing according to the step 1-3 to obtain a cigarette sample solution, performing GC-MS-SIM scanning, and drawing a change curve of the calibration value along with the storage time by taking the calibration value as a vertical coordinate, wherein the calibration value is the ratio of the first calibration substance quantitative ion peak area to the second calibration substance quantitative ion peak area, and the specific figure is 3.
As can be seen from FIG. 3, under the sealed storage condition, the retention capacity of the menthyl acetate is good, the calibration value is linearly related to the storage days, the equation is y = -0.0012x +0.1205, and the correlation coefficient R is 2 Was 0.9872. And according to the deduction of a formula, the menthyl acetate volatilizes and migrates completely after the bead blasting, breaking and sealing storage is carried out for about 100 days, so that the sample with the bead blasting, breaking and within 100 days can be effectively judged under the sealing storage condition.
5. Actual testing
And (4) performing sample treatment and GC-MS-SIM scanning on the actual cigarette bead blasting crushing sample #1 according to the steps 1-3. And calculating a standard value of 0.07322 in the sample #1, and substituting the standard value into the content change curve to obtain the breaking time of the blasting beads, wherein the breaking time is 39.4 days. The time for breaking the beads of sample #1 was estimated to be 39 days, which was substantially equivalent to the actual breaking time of 37 days.
Example two:
different from the first embodiment, the sample is selected as a brand A bead-exploded cigarette, and a bead-exploded cigarette sample #2 (which is stored in an open state at room temperature for a period of time after bead-explosion) is obtained from Zhejiang cigarette.
Selecting 15 groups of the same kind of bead blasting cigarette samples as the bead blasting cigarettes to be tested, crushing the bead blasting in the bead blasting cigarette samples, storing the bead blasting samples in an open room temperature, and analyzing the batch of samples respectively at 1 st, 2 nd, 3 rd, 5 th, 7 th, 9 th, 12 th, 15 th, 20 th, 25 th, 30 th, 40 th, 50 th, 65 th and 85 th days after the bead blasting is crushed. The specific analysis steps are as follows: tearing off the broken cigarettes which are stored for a certain number of days after the exploded cigarettes are broken, putting the broken cigarettes into a conical flask, processing samples according to the steps 1-3 to obtain cigarette sample solution, carrying out GC-MS-SIM scanning, wherein the calibration value is the ratio of the peak area of the first calibration substance quantitative ion to the peak area of the second calibration substance quantitative ion, and drawing a change curve of the calibration value along with the storage time by taking the calibration value as a vertical coordinate, which is shown in figure 4.
As shown in FIG. 4, the retention of menthyl acetate was poor under open storage conditions, and the peak area ratio of the marker was exponentially related to the number of days of storage, and the equation was y =0.0742e -0.111x Coefficient of correlation R 2 It was 0.9517. According to experimental data, the menthyl acetate basically volatilizes and completely migrates after the exploded beads are broken and stored for about 40 days, so that the samples within 40 days after the exploded beads are broken can be effectively judged under the open storage condition.
In the actual test, the actual cigarette bead breaking sample # 2 is subjected to sample treatment and GC-MS-SIM scanning in reference to the steps 1-3. And calculating the nominal value of 0.04138 in the sample # 2, and substituting the nominal value into the content change curve to obtain the breaking time of the blasting beads, namely 5.3 days. The time to break the bead for sample # 2 was assumed to be 5 days, which was substantially identical to the actual break time of 5 days.
Test results of the two embodiments are integrated, the contents of the blasting beads are subjected to full-scan analysis by using GC-MS, and characteristic peaks are selected as calibration substances; secondly, observing the change curve of the content of the calibration object along with the storage time of the cigarette sample after the bead blasting is manually broken by using a GC-MS-SIM method; by means of the curve, after the actual bead blasting and crushing cigarette sample is analyzed, the approximate time of bead blasting and crushing can be quickly judged, and therefore data support is provided for quality complaint analysis and product quality maintenance of the bead blasting cigarettes after delivery. The quantitative ion peak area ratio of the menthyl acetate and the caprylic/capric glyceride is used as the ordinate of the content change curve for the first time, so that the stability of a GC-MS instrument can be corrected, the step of adding an internal standard is omitted, a standard substance and a reference sample are not needed, and the rapid judgment is really realized.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, it is possible to make various improvements and modifications without departing from the technical principle of the present invention, and those improvements and modifications should be considered as the protection scope of the present invention.
Claims (10)
1. A method for measuring the breaking time of the blasting beads in the cigarette filter is characterized by comprising the following steps:
extracting a cigarette sample after the blasting beads are crushed to prepare a sample solution;
analyzing and processing the sample solution by GC-MS to obtain an SIM (subscriber identity module) diagram of the sample solution;
and quantifying the ion peak area according to a calibration object in the SIM map to obtain a calibration value, and comparing the calibration value with a preset standard change curve to obtain the time for breaking the sample after blasting the beads.
2. The method for measuring the breaking time of the popping beads in the cigarette filter according to claim 1, wherein the preparation method of the sample solution comprises the following steps:
taking a cigarette sample after the exploded beads are broken, tearing the sample, adding an extraction liquid for extraction, standing the sample, taking a supernatant, and filtering the supernatant through an organic phase filter membrane to obtain a sample solution.
3. The method for measuring the bead blasting breakage time in a cigarette filter according to claim 2, wherein the extraction liquid is n-hexane.
4. The method for measuring the breaking time of the popping beads in the cigarette filter according to claim 2, wherein the pore size of the organic phase filter membrane is 0.45 μm.
5. The method for measuring the bead burst breakage time in the cigarette filter according to claim 1, wherein the calibration material includes a first volatile calibration material and a second non-volatile calibration material in the cigarette bead burst, and the calibration value is a quantitative ion peak area ratio of the first calibration material to the second calibration material in a SIM (subscriber identity module) diagram.
6. The method for measuring the breaking time of the popping beads in the cigarette filter according to claim 5, wherein the first calibration material is menthyl acetate, and the second calibration material is glyceryl caprylate caprate.
7. The method for measuring the bead breakage time in a cigarette filter according to claim 1, wherein the method for preparing the standard change curve prepared in advance comprises the following steps:
taking a plurality of test samples in the same batch with the sample to be tested, breaking the exploded beads of the test samples, storing the broken beads at room temperature, calculating the calibration value of the test samples at a plurality of time nodes, and drawing a standard variation curve of the calibration value-time.
8. The method for measuring the breaking time of the popping beads in the cigarette filter according to claim 1, wherein a DB-5MS elastic quartz capillary chromatographic column is adopted for GC chromatographic analysis.
9. The method for measuring the bead blasting breakage time in the cigarette filter according to claim 1, wherein the GC chromatographic analysis adopts a temperature programming method, and the temperature programming conditions are as follows: the initial temperature is 60 ℃, the temperature is kept for 1min, then the temperature is increased to 200 ℃ at the speed of 10 ℃/min, the temperature is kept for 2min, the temperature is increased to 300 ℃ at the speed of 5 ℃/min, and the temperature is kept for 5min; the flow splitting ratio is 5; carrier gas: helium gas with a purity of 99.999%; a constant flow mode, wherein the flow rate is 1.0mL/min; the total run time was 42min.
10. The method for measuring the bead-blasting breakage time in a cigarette filter according to claim 1, wherein the MS condition is: ionization energy 70eV; filament current: 35 muA; ion source temperature: 230 ℃; temperature of the quadrupole rods: 150 ℃; transmission line temperature: 280. DEG C; delaying the solvent for 5min; the scanning mode is as follows: SIM selects ion scanning, the first calibration material menthyl acetate has the quantitative ion of 138, and the qualitative ions of 123, 95; the second calibration material, caprylic capric glyceride, had a quantitative ion of 355 and qualitative ions of 327, 127, 155.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107884504A (en) * | 2017-11-07 | 2018-04-06 | 国家烟草质量监督检验中心 | Pungent, the assay method of glycerol decanoate in a kind of quick-fried pearl of cigarette |
| CN107941978A (en) * | 2017-11-23 | 2018-04-20 | 陕西中烟工业有限责任公司 | A kind of quick-fried pearl inherent quality method for estimating stability of cigarette |
| CN108285830A (en) * | 2018-01-24 | 2018-07-17 | 云南中烟工业有限责任公司 | A kind of cigarette quick-fried pearl herbal essential oil and quick-fried pearl preparation method |
| CN109580832A (en) * | 2018-12-29 | 2019-04-05 | 陕西中烟工业有限责任公司 | A kind of quick-fried pearl content flash distillation-GC/MS rapid detection method of cigarette |
| CN110333306A (en) * | 2019-07-15 | 2019-10-15 | 中国烟草总公司郑州烟草研究院 | A kind of method for quantitatively determining of cigarette Glycerin, mixed triester with caprylic acid capric acid in quick-fried pearl solvent |
| CN113049709A (en) * | 2021-03-23 | 2021-06-29 | 江苏中烟工业有限责任公司 | Method for screening characteristic markers in bead blasting for cigarettes and quality control method |
-
2022
- 2022-08-16 CN CN202210979249.6A patent/CN115406983A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107884504A (en) * | 2017-11-07 | 2018-04-06 | 国家烟草质量监督检验中心 | Pungent, the assay method of glycerol decanoate in a kind of quick-fried pearl of cigarette |
| CN107941978A (en) * | 2017-11-23 | 2018-04-20 | 陕西中烟工业有限责任公司 | A kind of quick-fried pearl inherent quality method for estimating stability of cigarette |
| CN108285830A (en) * | 2018-01-24 | 2018-07-17 | 云南中烟工业有限责任公司 | A kind of cigarette quick-fried pearl herbal essential oil and quick-fried pearl preparation method |
| CN109580832A (en) * | 2018-12-29 | 2019-04-05 | 陕西中烟工业有限责任公司 | A kind of quick-fried pearl content flash distillation-GC/MS rapid detection method of cigarette |
| CN110333306A (en) * | 2019-07-15 | 2019-10-15 | 中国烟草总公司郑州烟草研究院 | A kind of method for quantitatively determining of cigarette Glycerin, mixed triester with caprylic acid capric acid in quick-fried pearl solvent |
| CN113049709A (en) * | 2021-03-23 | 2021-06-29 | 江苏中烟工业有限责任公司 | Method for screening characteristic markers in bead blasting for cigarettes and quality control method |
Non-Patent Citations (7)
| Title |
|---|
| 何媛;彭军仓;吕娟;杨芳;樊亚玲;曹永艳;王瑶;李小斌;王永红;邓宝安;曹稳;雷东锋;黄仲波;: "GC/MS指纹图谱及系统聚类分析用于烟用爆珠内含物的测定", 烟草科技, no. 07, 26 July 2018 (2018-07-26) * |
| 夏启东;何邦华;侯英;申晓锋;蒋举兴;杨蕾;邱昌桂;: "气相色谱质谱法测定6种加香目标物质的含量及对烟丝加香均匀性的评价", 分析测试学报, no. 07, 25 July 2012 (2012-07-25) * |
| 席辉;柴国璧;张启东;刘俊辉;王丁众;孙世豪;吴晶晶;: "卷烟爆珠溶剂中链甘油三酯的分离与鉴定", 烟草科技, no. 07, 26 July 2018 (2018-07-26) * |
| 朱瑞芝;刘凌璇;刘志华;张凤梅;司晓喜;王庆华;白晓莉;谢静;詹建波;: "不同印刷食品包装纸溶剂残留量及与存放时间相关性研究", 分析化学, no. 05, 15 May 2015 (2015-05-15) * |
| 朱瑞芝;詹建波;蒋薇;李振杰;司晓喜;程量;张凤梅;尤俊衡;苏钟璧;刘志华;: "GC-MS/MS法分析爆珠关键成分在卷烟中的转移行为", 烟草科技, no. 06, 27 June 2018 (2018-06-27) * |
| 莫新良 等: "黄酒储存期间4-乙烯基愈疮木酚和香草醛的变化及影响因素", 黄酒储存期间4-乙烯基愈疮木酚和香草醛的变化及影响因素, vol. 42, no. 2, 28 February 2016 (2016-02-28), pages 29 - 34 * |
| 郭华诚;赵琪;吴艳艳;朱远洋;郜海民;李瑞丽;: "爆珠香味成分剖析及其在卷烟中转移率", 食品工业, no. 03, 20 March 2020 (2020-03-20) * |
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