CN114062579A - Parallel detection device for gas chromatograph and cigarette total particulate matter determination method - Google Patents
Parallel detection device for gas chromatograph and cigarette total particulate matter determination method Download PDFInfo
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- 235000019504 cigarettes Nutrition 0.000 title claims abstract description 57
- 238000001514 detection method Methods 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title claims abstract description 33
- 239000013618 particulate matter Substances 0.000 title claims description 18
- URAYPUMNDPQOKB-UHFFFAOYSA-N triacetin Chemical compound CC(=O)OCC(OC(C)=O)COC(C)=O URAYPUMNDPQOKB-UHFFFAOYSA-N 0.000 claims abstract description 88
- SNICXCGAKADSCV-JTQLQIEISA-N (-)-Nicotine Chemical compound CN1CCC[C@H]1C1=CC=CN=C1 SNICXCGAKADSCV-JTQLQIEISA-N 0.000 claims abstract description 45
- 229960002715 nicotine Drugs 0.000 claims abstract description 45
- SNICXCGAKADSCV-UHFFFAOYSA-N nicotine Natural products CN1CCCC1C1=CC=CN=C1 SNICXCGAKADSCV-UHFFFAOYSA-N 0.000 claims abstract description 45
- 235000013773 glyceryl triacetate Nutrition 0.000 claims abstract description 27
- 229960002622 triacetin Drugs 0.000 claims abstract description 27
- 239000007789 gas Substances 0.000 claims abstract description 20
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000001257 hydrogen Substances 0.000 claims abstract description 18
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 18
- 230000010355 oscillation Effects 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000004817 gas chromatography Methods 0.000 claims abstract description 14
- 239000001087 glyceryl triacetate Substances 0.000 claims abstract description 12
- 238000000605 extraction Methods 0.000 claims description 26
- 230000000391 smoking effect Effects 0.000 claims description 19
- 239000012086 standard solution Substances 0.000 claims description 17
- 239000000779 smoke Substances 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 13
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 10
- NDJKXXJCMXVBJW-UHFFFAOYSA-N heptadecane Chemical compound CCCCCCCCCCCCCCCCC NDJKXXJCMXVBJW-UHFFFAOYSA-N 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 9
- 238000010813 internal standard method Methods 0.000 claims description 8
- 239000000243 solution Substances 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 5
- 239000012153 distilled water Substances 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 8
- 239000012159 carrier gas Substances 0.000 abstract description 6
- 239000001307 helium Substances 0.000 abstract description 5
- 229910052734 helium Inorganic materials 0.000 abstract description 5
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 abstract description 5
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 4
- 238000003965 capillary gas chromatography Methods 0.000 abstract description 3
- 239000000523 sample Substances 0.000 description 55
- 238000013461 design Methods 0.000 description 3
- 235000019441 ethanol Nutrition 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 238000007664 blowing Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- -1 Glycerol triacetate Nicotine Chemical compound 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- 230000014509 gene expression Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 239000012488 sample solution Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 125000006850 spacer group Chemical group 0.000 description 1
- 238000012421 spiking Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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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
- G01N30/62—Detectors specially adapted therefor
- G01N30/64—Electrical detectors
- G01N30/68—Flame ionisation detectors
-
- 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
- G01N30/64—Electrical detectors
- G01N30/66—Thermal conductivity detectors
-
- 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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- 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 discloses a parallel detection device for a gas chromatograph and a method for measuring total particulate matters of cigarettes, which are based on the concept of parallel capillary column gas chromatography, and are characterized in that peaks of triacetin, nicotine and moisture are separated by a single sample inlet and are quantitatively detected, helium or nitrogen is not needed, and only hydrogen can be used as carrier gas, so that the content of the triacetin, nicotine and moisture in the total particulate matters of the cigarettes can be measured simultaneously; specifically, a special device is constructed by a capillary column three-way connector, a sample inlet capillary column connector, a first capillary column, a second capillary column, a hydrogen flame ionization detector and a thermal conductivity cell detector, a sample to be detected is extracted by oscillation, a gas chromatography detection signal is obtained by using the device, and then the gas chromatography detection signal is fitted with a set standard working curve and regressed to obtain the contents of glyceryl triacetate, nicotine and water. The method is suitable for the characteristics of simplicity, high efficiency, high accuracy and good repeatability, and can also obviously reduce the detection cost.
Description
Technical Field
The invention relates to the field of cigarette detection, in particular to a parallel detection device for a gas chromatograph and a method for measuring triacetyl glycerine, nicotine and moisture in a cigarette total particulate matter.
Background
The determination of nicotine and moisture content in the total particulate matter of the cigarette is a routine detection item in the mainstream smoke of the cigarette, and the triacetyl glycerine plasticizer adopted by the filter tip rod can escape from the part of the cigarette bundle to enter the smoke along with the smoking of the cigarette.
At present, the method mainly adopts a packed column gas chromatography for measuring the nicotine in the smoke in the total particulate matter, and helium or nitrogen is used as carrier gas; the water content was determined by packed column gas chromatography with helium as carrier gas. Therefore, it is usually necessary to provide one inlet for each of nicotine and moisture; for detecting the glycerol triacetate in the smoke, a total particle phase substance needs to be separately obtained, and a chromatographic column, chromatographic conditions and an extraction method which are different from those of nicotine and moisture are adopted.
The existing measurement mode inevitably has the problems of more used equipment and more types of chemical reagents and carrier gas, and the problems that different chromatographic columns are required to be replaced, different extraction liquid is prepared and chromatographic conditions are required to be set for detecting the glycerol triacetate in the flue gas, so that the measurement work is complicated, the analysis time is long and the efficacy is low.
Disclosure of Invention
In view of the above, the present invention aims to provide a parallel detection device for a gas chromatograph and a method for measuring total particulate matters of cigarettes, so as to solve the aforementioned disadvantages of the prior art for measuring total particulate matters of a plurality of cigarettes.
The technical scheme adopted by the invention is as follows:
in a first aspect, a parallel detection apparatus for a gas chromatograph includes: the device comprises a capillary column three-way connector, a sample inlet capillary column connector, a first capillary column, a second capillary column, a hydrogen flame ionization detector and a thermal conductivity cell detector;
three channels of the capillary column three-way connector are respectively connected with an outlet of the sample inlet capillary column connector, one end of the first capillary column and one end of the second capillary column;
the inlet of the sample inlet capillary column connector is a unique gas chromatography sample inlet for detecting total particulate matters of the cigarettes;
the other end of the first capillary column is connected with the hydrogen flame ionization detector and is used for measuring the triacetyl glycerine and nicotine in the total particulate matters of the cigarettes;
the other end of the second capillary column is connected with the thermal conductivity cell detector and is used for measuring the moisture in the total particulate matters of the cigarettes.
In at least one possible implementation, a capillary connection is employed between the capillary column three-way connector and the outlet of the sample inlet capillary column connector.
In at least one possible implementation thereof, the capillary is a deactivated fused silica capillary.
In a second aspect, a method for determining total particulate matters of cigarettes comprises the following steps:
preparing an extraction solution based on heptadecane, ethanol and isopropanol solution;
performing standard smoking operation on the cigarette sample by using a smoking machine, and trapping total particulate matters in the mainstream smoke of the cigarette in the smoking process;
adding the extraction liquid into the collected total particulate matter, and performing oscillation extraction to obtain a sample to be detected;
after setting the parameters of the gas chromatograph, acquiring a detection signal of a sample to be detected by adopting any one of the parallel detection devices; wherein the gas chromatograph parameters comprise column oven temperature, hydrogen flame ionization detector and thermal conductivity cell detector parameters;
and synchronously measuring the contents of the triacetyl glycerine, the nicotine and the water in the sample to be measured based on the detection signal of the sample to be measured and the pre-configured standard sample.
In at least one possible implementation manner, the synchronously determining the content of triacetin, nicotine, and moisture in the sample to be tested based on the detection signal of the sample to be tested and the preconfigured standard sample includes:
respectively obtaining standard working curve regression equations by using an internal standard method based on the standard samples;
and combining a detection signal obtained by the sample to be detected through the parallel detection device with the regression equation of the standard working curve to obtain the contents of the triacetyl glycerine, the nicotine and the moisture in the mainstream smoke of the cigarette.
In at least one possible implementation manner, the obtaining the regression equation of the standard working curve by using an internal standard method based on the standard sample respectively includes: and quantifying the pre-configured first standard solution of which the internal standard substance comprises glycerol triacetate and nicotine and the second standard solution of which the internal standard substance comprises water by adopting a gas chromatography internal standard method, and fitting a regression equation.
In at least one possible implementation manner, the configuration manner of the standard sample includes:
quantitatively weighing glycerol triacetate and nicotine, and preparing a first standard solution by constant volume; quantitatively weighing distilled water to prepare a second standard solution by constant volume;
and adding the extraction liquid to the first standard solution and the second standard solution respectively to obtain a standard sample related to the triacetyl glycerine and the nicotine and a standard sample related to the moisture.
In at least one possible implementation manner, the standard working curve is a multi-level standard working curve obtained based on standard solutions with different capacities or qualities.
In at least one possible implementation manner, the capturing of total particulate matters in mainstream smoke of the cigarette comprises: after the cigarette sample is balanced in a preset environment, a rotary disc smoking machine is used for performing smoking operation, and a Cambridge filter disc is used for trapping total particulate matters in the mainstream smoke of the cigarette in the smoking process.
In at least one possible implementation manner, the determination method further comprises calibrating the oscillation extraction time according to the following manner:
respectively calibrating the influence degrees of different oscillation extraction time lengths on the glyceryl triacetate, the nicotine and the water in a preset time length range;
and comprehensively calibrating the obtained influence degree, and determining the target oscillation extraction time from the preset time range.
The main design concept of the invention is that based on the parallel capillary column gas chromatography concept, the single sample inlet separates the peaks of the triacetyl glycerine, the nicotine and the moisture by chromatography and carries out quantitative detection, helium or nitrogen is not needed, and only hydrogen can be used as carrier gas, so that the content of the triacetyl glycerine, the nicotine and the moisture in the total particulate matter of the cigarettes can be simultaneously measured; specifically, a special device is constructed by a capillary column three-way connector, a sample inlet capillary column connector, a first capillary column, a second capillary column, a hydrogen flame ionization detector and a thermal conductivity cell detector, a sample to be detected is extracted by oscillation, a gas chromatography detection signal is obtained by using the device, and then the gas chromatography detection signal is fitted with a set standard working curve and regressed to obtain the contents of glyceryl triacetate, nicotine and moisture. The method is suitable for detecting the mainstream smoke of the cigarettes, the content of the glycerol triacetate is also detected while the content of nicotine and moisture is detected, the maximum Relative Standard Deviation (RSD) is less than 2.5%, the recovery rate is 94-109%, and the method has the characteristics of simplicity, high efficiency, high accuracy and good repeatability, and can also obviously reduce the detection cost.
Drawings
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be further described with reference to the accompanying drawings, in which:
fig. 1 is a schematic diagram of a parallel detection apparatus for a gas chromatograph according to an embodiment of the present invention;
fig. 2 is a flow chart of a method for determining total particulate matters of cigarettes provided by the embodiment of the invention.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the drawings are illustrative only and should not be construed as limiting the invention.
The invention provides an embodiment of a parallel detection device for a gas chromatograph, specifically, as shown in fig. 1, the parallel detection device comprises: the device comprises a capillary column three-way connector 1, a sample inlet capillary column connector 2, a first capillary column 10, a second capillary column 20, a hydrogen flame ionization detector 11 and a thermal conductivity cell detector 21;
three channels of the capillary column three-way connector 1 are respectively connected with an outlet of the sample inlet capillary column connector 2, one end of the first capillary column 10 and one end of the second capillary column 20;
the inlet of the sample inlet capillary column connector 2 is a unique gas chromatography sample inlet for detecting total particulate matters of the cigarettes;
the other end of the first capillary column 10 is connected with the hydrogen flame ionization detector 11 and is used for measuring the triacetyl glycerine and nicotine in the total particulate matters of the cigarettes;
the other end of the second capillary column 20 is connected to the thermal conductivity cell detector 21 for measuring moisture in the total particulate matter of the cigarette.
Further, a capillary tube is adopted for connection between the capillary tube column three-way connector 1 and the outlet of the sample inlet capillary tube column connector 2. Preferably, the capillary is a deactivated fused silica capillary.
On the basis of the device, the invention also provides an embodiment of the method for determining the total particulate matter of the cigarettes, and the method is characterized in that a cigarette sample, isopropanol (AR grade, purity is more than or equal to 99.5), nicotine (AR grade, purity is more than or equal to 99.0), distilled water, heptadecane (GC grade, purity is more than or equal to 99.0), absolute ethyl alcohol (GC grade, purity is more than or equal to 99.9) and glycerol triacetate (purity is more than or equal to 99.5) can be prepared in advance before the determination method is implemented; and a turntable smoking machine, a gas chromatograph equipped with FID and TCD detectors (FID detector: hydrogen flame ionization detector; TCD detector: thermal conductivity cell detector), an analytical balance (inductance 0.1mg), and an oscillator.
In the foregoing, the method for measuring triacetyl glycerine, nicotine and moisture in the total particulate matter of cigarette can be shown in fig. 2, and includes:
step S1, preparing an extraction liquid based on heptadecane, ethanol and isopropanol solution; specifically, 0.5mL of heptadecane and 5mL of ethanol may be added, and an isopropanol solution may be added to the mixture to a volume of 1 liter, thereby preparing an extract.
Step S2, performing standard smoking operation on the cigarette sample by using a smoking machine, and trapping total particulate matters in the mainstream smoke of the cigarette in the smoking process; specifically, the cigarette sample can be balanced in a specified temperature and humidity environment for more than 48 hours, then 20 cigarettes are placed on a rotary disc smoking machine to perform smoking operation, and the cambridge filter disc is used for trapping total particulate matters in the mainstream smoke of the 20 cigarettes in the process.
Step S3, adding the extraction liquid into the collected total particulate matter, and performing oscillation extraction to obtain a sample to be detected; specifically, 50mL of the extract can be added to the Cambridge filter, and the mixture is placed in a shaking table to be shaken for 15 minutes, and the supernatant is taken as a sample to be detected. The oscillation extraction time can be calibrated in advance, for example, 50ml of extraction liquid is taken as an example, the preliminary test is carried out in the range of 10-50 minutes, and the extraction effect of the total particulate matter with different oscillation time lengths is inspected. The invention aims to measure the triacetyl glycerine, nicotine and water in the total grain phase, so that the influence of the oscillation extraction time on any target can be respectively examined, and the influence of the oscillation extraction time on the target can be integrated to determine the optimal oscillation extraction time, such as 15 minutes.
Step S4, after setting the parameters of the gas chromatograph, acquiring the detection signal of the sample to be detected by adopting a parallel detection device;
and step S5, synchronously measuring the contents of the triacetyl glycerine, the nicotine and the water in the sample to be measured based on the detection signal of the sample to be measured and the pre-configured standard sample.
The parameters of the gas chromatograph comprise the temperature of the column oven, other conditions are kept unchanged, and the preset standard sample and the sample to be detected are detected by adopting the parallel detection device, specifically, the peak emergence conditions of the standard sample and the sample to be detected are inspected; further, in order to keep good peak value separation effect and detection speed, the temperature of the column oven can be kept at 160 ℃ constantly, the time is kept for 9.1 minutes, and under the condition, a standard sample, a sample to be detected and even impurities can be completely separated, so that the analysis requirement can be well met.
Regarding the setting of the gas chromatograph, further reference may be made to: the sample introduction amount of the parallel type cigarette total particulate matter detection device is set to be 1uL, the temperature of a sample introduction port is 250 ℃, the pressure is constant at 10Psi, the split ratio is 20:1, and the spacer purging is carried out for 3 mL/min; the temperature of a hydrogen Flame Ionization (FID) detector is 250 ℃, the air flow is 320mL/min, the hydrogen flow is 30mL/min, the tail gas blowing is 15mL/min, and the specification of an Agilent chromatographic column CP-WAX52CB is 50m multiplied by 0.53mm multiplied by 1.00 mu m; the temperature of a thermal conductivity cell detector (TCD) is 250 ℃, the reference hydrogen flow is 10mL/min, the tail gas blowing is 5mL/min, and the specification of an Agilent chromatographic column HP-PLOT Q is 30m multiplied by 0.53mm multiplied by 40 mu m.
For the preparation of the standard sample, reference can then be made to the following: weighing 400mg of glycerol triacetate and 400mg of nicotine to 100mL of constant volume first standard solution, then respectively sucking 1mL, 2mL, 3mL, 4mL, 5mL and 6mL of first standard solution, and adding 50mL of the extract liquid one by one to prepare standard samples related to the glycerol triacetate and the nicotine, wherein six standard samples obtained in the example are used for obtaining a 6-grade standard working curve related to the glycerol triacetate and the nicotine, and other examples can be not limited to the above; in addition, distilled water was weighed as a second standard solution in six different masses, and 50mL of the aforementioned extract was added to prepare a standard sample concerning moisture in order to obtain a standard working curve of grade 6 concerning moisture.
As to the specific manner of detecting the predetermined standard sample and the sample to be detected, there may be, but not limited to: based on the standard samples, the regression equation of the standard curve is respectively obtained by using an internal standard method, that is, a plurality of standard sample solutions of which the internal standard substances are glycerol triacetate, nicotine and water are prepared in advance are quantified by using a gas chromatography internal standard method, and regression equation fitting is carried out, which can be specifically shown in the following table.
| Compound (I) | Retention time | Regression equation | Coefficient of correlation R |
| Glycerol triacetate | 8.845 | Y＝1.10034X | 0.99994 |
| Nicotine | 4.848 | Y＝2.65623X | 0.99997 |
| Moisture content | 1.665 | Y＝0.15846+0.50045 | 0.9998 |
And then combining a detection signal obtained by the sample to be detected through a parallel detection device with the regression equation of the standard curve to obtain the contents of the triacetyl glycerine, the nicotine and the water in the total particulate matter.
On the basis of the determination method, 0.4mg/cig, 0.8mg/cig and 1.2mg/cig of glycerol triacetate can be sequentially added into the total particulate matter of the same cigarette sample according to the low, medium and high content concentrations of 3; nicotine 0.3mg/cig, 0.6mg/cig, 0.9 mg/cig; the recovery rates for spiking and relative standard deviations (RSD/%) were obtained in six replicates after shaking extraction with water contents of 0.8mg/cig, 1.8mg/cig, and 2.8mg/cig, as shown in the following table.
On the basis of the above measurement method, six replicates of triacetin, nicotine and moisture in the same cigarette sample were also taken, and the standard deviation (STD), the relative deviation (RSD/%) were calculated to examine the reproducibility, as shown in the following table.
| Number of samples taken | Glycerol triacetate | | Moisture content | |
| 1 | 1.693 | 1.950 | 3.953 | |
| 2 | 1.693 | 1.953 | 3.968 | |
| 3 | 1.687 | 1.953 | 3.895 | |
| 4 | 1.705 | 1.952 | 3.884 | |
| 5 | 1.708 | 1.951 | 3.912 | |
| 6 | 1.711 | 1.951 | 3.939 | |
| Mean value of | 1.700 | 1.952 | 3.925 | |
| STD | 0.01 | 0.00 | 0.03 | |
| RSD/％ | 0.58 | 0.07 | 0.85 |
In conclusion, the main design concept of the invention is that based on the parallel capillary column gas chromatography concept, peaks are separated from triacetin, nicotine and moisture by a single sample inlet, and quantitative detection is carried out, helium or nitrogen is not needed, and only hydrogen can be used as carrier gas, so that the content of triacetin, nicotine and moisture in the total particulate matter of the cigarettes can be measured simultaneously; specifically, a special device is constructed by a capillary column three-way connector, a sample inlet capillary column connector, a first capillary column, a second capillary column, a hydrogen flame ionization detector and a thermal conductivity cell detector, a sample to be detected is extracted by oscillation, a gas chromatography detection signal is obtained by using the device, and then the gas chromatography detection signal is fitted with a set standard working curve and regressed to obtain the contents of glyceryl triacetate, nicotine and moisture. The method is suitable for detecting the mainstream smoke of the cigarettes, the content of the glycerol triacetate is also detected while the content of nicotine and moisture is detected, the maximum Relative Standard Deviation (RSD) is less than 2.5%, the recovery rate is 94-109%, and the method has the characteristics of simplicity, high efficiency, high accuracy and good repeatability, and can also obviously reduce the detection cost.
In the embodiments of the present invention, "at least one" means one or more, "a plurality" means two or more. "and/or" describes the association relationship of the associated objects, and means that there may be three relationships, for example, a and/or B, and may mean that a exists alone, a and B exist simultaneously, and B exists alone. Wherein A and B can be singular or plural. The character "/" generally indicates that the former and latter associated objects are in an "or" relationship. "at least one of the following" and similar expressions refer to any combination of these items, including any combination of singular or plural items. For example, at least one of a, b, and c may represent: a, b, c, a and b, a and c, b and c or a and b and c, wherein a, b and c can be single or multiple.
The structure, features and effects of the present invention have been described in detail with reference to the embodiments shown in the drawings, but the above embodiments are merely preferred embodiments of the present invention, and it should be understood that technical features related to the above embodiments and preferred modes thereof can be reasonably combined and configured into various equivalent schemes by those skilled in the art without departing from and changing the design idea and technical effects of the present invention; therefore, the invention is not limited to the embodiments shown in the drawings, and all the modifications and equivalent embodiments that can be made according to the idea of the invention are within the scope of the invention as long as they are not beyond the spirit of the description and the drawings.
Claims (10)
1. A parallel detection apparatus for a gas chromatograph, comprising: the device comprises a capillary column three-way connector, a sample inlet capillary column connector, a first capillary column, a second capillary column, a hydrogen flame ionization detector and a thermal conductivity cell detector;
three channels of the capillary column three-way connector are respectively connected with an outlet of the sample inlet capillary column connector, one end of the first capillary column and one end of the second capillary column;
the inlet of the sample inlet capillary column connector is a unique gas chromatography sample inlet for detecting total particulate matters of the cigarettes;
the other end of the first capillary column is connected with the hydrogen flame ionization detector and is used for measuring the triacetyl glycerine and nicotine in the total particulate matters of the cigarettes;
the other end of the second capillary column is connected with the thermal conductivity cell detector and is used for measuring the moisture in the total particulate matters of the cigarettes.
2. The parallel detection apparatus for gas chromatograph of claim 1, wherein a capillary connection is employed between the capillary column tee connector and the outlet of the sample inlet capillary column connector.
3. The parallel detection apparatus for gas chromatograph of claim 2, wherein the capillary is a deactivated fused silica capillary.
4. A method for measuring total particulate matters of cigarettes is characterized by comprising the following steps:
preparing an extraction solution based on heptadecane, ethanol and isopropanol solution;
performing standard smoking operation on the cigarette sample by using a smoking machine, and trapping total particulate matters in the mainstream smoke of the cigarette in the smoking process;
adding the extraction liquid into the collected total particulate matter, and performing oscillation extraction to obtain a sample to be detected;
after setting the parameters of the gas chromatograph, acquiring the detection signal of the sample to be detected by adopting the parallel detection device of any claim 1-3; wherein the gas chromatograph parameters comprise column oven temperature, hydrogen flame ionization detector and thermal conductivity cell detector parameters;
and synchronously measuring the contents of the triacetyl glycerine, the nicotine and the water in the sample to be measured based on the detection signal of the sample to be measured and the pre-configured standard sample.
5. The method for determining total particulate matters of cigarettes according to claim 4, wherein the step of synchronously determining the contents of triacetin, nicotine and moisture in the sample to be determined based on the detection signal of the sample to be determined and the preconfigured standard sample comprises:
respectively obtaining standard working curve regression equations by using an internal standard method based on the standard samples;
and combining a detection signal obtained by the sample to be detected through the parallel detection device with the regression equation of the standard working curve to obtain the contents of the triacetyl glycerine, the nicotine and the moisture in the mainstream smoke of the cigarette.
6. The method for determining total particulate matters of cigarettes according to claim 5, wherein the step of obtaining the regression equation of the standard working curve by using an internal standard method based on the standard samples comprises the following steps: and quantifying the pre-configured first standard solution of which the internal standard substance comprises glycerol triacetate and nicotine and the second standard solution of which the internal standard substance comprises water by adopting a gas chromatography internal standard method, and fitting a regression equation.
7. The method for determining total particulate matter of cigarettes according to claim 6, wherein the standard sample is disposed in a manner including:
quantitatively weighing glycerol triacetate and nicotine, and preparing a first standard solution by constant volume; quantitatively weighing distilled water to prepare a second standard solution by constant volume;
and adding the extraction liquid to the first standard solution and the second standard solution respectively to obtain a standard sample related to the triacetyl glycerine and the nicotine and a standard sample related to the moisture.
8. The method for determining the total particulate matters of the cigarettes according to any one of claims 5 to 7, wherein the standard working curve is a multi-level standard working curve obtained based on standard solutions with different capacities or qualities.
9. The method for determining total particulate matters of cigarettes according to any one of claims 4 to 7, wherein the step of collecting the total particulate matters in the mainstream smoke of the cigarettes comprises the following steps: after the cigarette sample is balanced in a preset environment, a rotary disc smoking machine is used for performing smoking operation, and a Cambridge filter disc is used for trapping total particulate matters in the mainstream smoke of the cigarette in the smoking process.
10. The method for determining total particulate matters of cigarettes according to any one of claims 4 to 7, wherein the method further comprises calibrating the oscillation extraction time as follows:
respectively calibrating the influence degrees of different oscillation extraction time lengths on the glyceryl triacetate, the nicotine and the water in a preset time length range;
and comprehensively calibrating the obtained influence degree, and determining the target oscillation extraction time from the preset time range.
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Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101169398A (en) * | 2007-11-20 | 2008-04-30 | 川渝中烟工业公司 | Method for determining glyceryl triacetate in cigarette main flue |
| CN102043027A (en) * | 2010-10-26 | 2011-05-04 | 上海烟草（集团）公司 | Method for evaluating absorbing performance of cigarette filter absorbing agent and testing system thereof |
| CN104280504A (en) * | 2014-10-29 | 2015-01-14 | 中国烟草总公司湖北省公司 | Capillary column gas chromatography method for simultaneously determining contents of water and nicotine in main stream smoke of cigarette |
| CN104458986A (en) * | 2014-10-29 | 2015-03-25 | 中国科学院广州地球化学研究所 | Gas chromatography multichannel sample introduction system and realized atmosphere detection method thereof |
| CN105067716A (en) * | 2015-07-03 | 2015-11-18 | 江苏中烟工业有限责任公司 | Method for determining puff-by-puff nicotine and tar in cigarette mainstream smoke |
| CN105954402A (en) * | 2016-04-27 | 2016-09-21 | 中国烟草总公司郑州烟草研究院 | Gas chromatography-flame ionization/tandem mass spectrometry detection method of alkaloids in cigarette main stream smoke |
| CN106093235A (en) * | 2016-06-06 | 2016-11-09 | 吉林烟草工业有限责任公司 | A kind of for measuring moisture and the extract of nicotine content and using method thereof in cigarette mainstream flue gas |
| CN108776184A (en) * | 2018-06-13 | 2018-11-09 | 湖北中烟工业有限责任公司 | A method of cigarette smoke component of not burning is heated in detection |
| CN111337603A (en) * | 2020-05-07 | 2020-06-26 | 贵州中烟工业有限责任公司 | Method for measuring nicotine content in tobacco product and method for simultaneously measuring water, 1, 2-propylene glycol, glycerol and nicotine content |
-
2021
- 2021-11-13 CN CN202111343752.4A patent/CN114062579A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101169398A (en) * | 2007-11-20 | 2008-04-30 | 川渝中烟工业公司 | Method for determining glyceryl triacetate in cigarette main flue |
| CN102043027A (en) * | 2010-10-26 | 2011-05-04 | 上海烟草（集团）公司 | Method for evaluating absorbing performance of cigarette filter absorbing agent and testing system thereof |
| CN104280504A (en) * | 2014-10-29 | 2015-01-14 | 中国烟草总公司湖北省公司 | Capillary column gas chromatography method for simultaneously determining contents of water and nicotine in main stream smoke of cigarette |
| CN104458986A (en) * | 2014-10-29 | 2015-03-25 | 中国科学院广州地球化学研究所 | Gas chromatography multichannel sample introduction system and realized atmosphere detection method thereof |
| CN105067716A (en) * | 2015-07-03 | 2015-11-18 | 江苏中烟工业有限责任公司 | Method for determining puff-by-puff nicotine and tar in cigarette mainstream smoke |
| CN105954402A (en) * | 2016-04-27 | 2016-09-21 | 中国烟草总公司郑州烟草研究院 | Gas chromatography-flame ionization/tandem mass spectrometry detection method of alkaloids in cigarette main stream smoke |
| CN106093235A (en) * | 2016-06-06 | 2016-11-09 | 吉林烟草工业有限责任公司 | A kind of for measuring moisture and the extract of nicotine content and using method thereof in cigarette mainstream flue gas |
| CN108776184A (en) * | 2018-06-13 | 2018-11-09 | 湖北中烟工业有限责任公司 | A method of cigarette smoke component of not burning is heated in detection |
| CN111337603A (en) * | 2020-05-07 | 2020-06-26 | 贵州中烟工业有限责任公司 | Method for measuring nicotine content in tobacco product and method for simultaneously measuring water, 1, 2-propylene glycol, glycerol and nicotine content |
Non-Patent Citations (5)
| Title |
|---|
| 何爱民: "气相色谱-质谱法测定卷烟烟气总粒相物中的三醋酸甘油酯", 化学工程师, no. 06, 30 June 2005 (2005-06-30) * |
| 周秋菊, 杨长顺, 范振霞, 张胜, 朱勇进: "气相色谱一次进样烟碱水分分析方法", 烟草科技, no. 08, 20 August 2000 (2000-08-20), pages 1 - 3 * |
| 张丽;王维维;张小涛;胡硕;姬厚伟;万强;陈永芳;刘剑;: "气相色谱法测定新型卷烟气溶胶中水、烟碱、1, 2-丙二醇和丙三醇的含量", 理化检验(化学分册), no. 10, 18 October 2018 (2018-10-18) * |
| 王维维;张丽;阮艺斌;姬厚伟;万强;黄新民;董睿;刘剑;: "气相色谱法同时测定烟草中水分及1, 2-丙二醇与丙三醇的含量", 贵州农业科学, no. 03, 15 March 2018 (2018-03-15) * |
| 黄晖, 黄海东, 李燕垣: "气相色谱法测定卷烟烟气总粒相物中的烟碱", 烟草科技, no. 05, 30 October 1997 (1997-10-30) * |
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