CN113219090B - GC-TCD combined detection method for main components of electronic cigarette liquid - Google Patents
GC-TCD combined detection method for main components of electronic cigarette liquid Download PDFInfo
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- 239000003571 electronic cigarette Substances 0.000 title claims abstract description 42
- 238000001514 detection method Methods 0.000 title claims abstract description 20
- 238000001165 gas chromatography-thermal conductivity detection Methods 0.000 title claims abstract 6
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 107
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims abstract description 66
- 229960004063 propylene glycol Drugs 0.000 claims abstract description 36
- SNICXCGAKADSCV-JTQLQIEISA-N (-)-Nicotine Chemical compound CN1CCC[C@H]1C1=CC=CN=C1 SNICXCGAKADSCV-JTQLQIEISA-N 0.000 claims abstract description 35
- 229960002715 nicotine Drugs 0.000 claims abstract description 35
- SNICXCGAKADSCV-UHFFFAOYSA-N nicotine Natural products CN1CCCC1C1=CC=CN=C1 SNICXCGAKADSCV-UHFFFAOYSA-N 0.000 claims abstract description 35
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 31
- NOOLISFMXDJSKH-UTLUCORTSA-N (+)-Neomenthol Chemical compound CC(C)[C@@H]1CC[C@@H](C)C[C@@H]1O NOOLISFMXDJSKH-UTLUCORTSA-N 0.000 claims abstract description 29
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- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 29
- 229940041616 menthol Drugs 0.000 claims abstract description 29
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims abstract description 26
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- 238000000034 method Methods 0.000 claims abstract description 21
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- 229910052734 helium Inorganic materials 0.000 claims description 6
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 6
- 238000002347 injection Methods 0.000 claims description 6
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- 239000011550 stock solution Substances 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
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- 238000012360 testing method Methods 0.000 abstract description 6
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- 235000011187 glycerol Nutrition 0.000 description 29
- 238000004817 gas chromatography Methods 0.000 description 8
- 235000019504 cigarettes Nutrition 0.000 description 7
- PUPZLCDOIYMWBV-UHFFFAOYSA-N (+/-)-1,3-Butanediol Chemical compound CC(O)CCO PUPZLCDOIYMWBV-UHFFFAOYSA-N 0.000 description 6
- 241000208125 Nicotiana Species 0.000 description 6
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 5
- DNIAPMSPPWPWGF-GSVOUGTGSA-N (R)-(-)-Propylene glycol Chemical compound C[C@@H](O)CO DNIAPMSPPWPWGF-GSVOUGTGSA-N 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000000796 flavoring agent Substances 0.000 description 4
- 235000019634 flavors Nutrition 0.000 description 4
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- URAYPUMNDPQOKB-UHFFFAOYSA-N triacetin Chemical compound CC(=O)OCC(OC(C)=O)COC(C)=O URAYPUMNDPQOKB-UHFFFAOYSA-N 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 235000013773 glyceryl triacetate Nutrition 0.000 description 2
- 239000001087 glyceryl triacetate Substances 0.000 description 2
- 238000010813 internal standard method Methods 0.000 description 2
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- 239000000463 material Substances 0.000 description 2
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- 238000000889 atomisation Methods 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 239000013065 commercial product Substances 0.000 description 1
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- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- MILWSGRFEGYSGM-UHFFFAOYSA-N propane-1,2-diol;propane-1,2,3-triol Chemical compound CC(O)CO.OCC(O)CO MILWSGRFEGYSGM-UHFFFAOYSA-N 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 230000000391 smoking effect Effects 0.000 description 1
- 238000012421 spiking Methods 0.000 description 1
- 239000013076 target substance Substances 0.000 description 1
- 235000019640 taste Nutrition 0.000 description 1
- 235000019505 tobacco product Nutrition 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
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/10—Chemical features of tobacco products or tobacco substitutes
- A24B15/16—Chemical features of tobacco products or tobacco substitutes of tobacco substitutes
- A24B15/167—Chemical features of tobacco products or tobacco substitutes of tobacco substitutes in liquid or vaporisable form, e.g. liquid compositions for electronic cigarettes
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24F—SMOKERS' REQUISITES; MATCH BOXES; SIMULATED SMOKING DEVICES
- A24F40/00—Electrically operated smoking devices; Component parts thereof; Manufacture thereof; Maintenance or testing thereof; Charging means specially adapted therefor
- A24F40/50—Control or monitoring
- A24F40/53—Monitoring, e.g. fault detection
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/64—Electrical detectors
- G01N30/66—Thermal conductivity detectors
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N2030/042—Standards
- G01N2030/045—Standards internal
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- General Physics & Mathematics (AREA)
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Abstract
The invention discloses a method for detecting main components of an electronic cigarette liquid based on GC-TCD combination, which comprises the steps of weighing 0.15g of the electronic cigarette liquid, adding 10mL of isopropanol solution containing an internal standard substance N-butanol and N, N-dimethylformamide, oscillating for 5min to obtain an extract, and preparing a standard working solution for GC-TCD analysis. The method can be used for simply, conveniently and rapidly analyzing the water, the 1, 2-propylene glycol, the glycerol, the menthol and the nicotine in the electronic cigarette liquid at the same time, measuring the water, the nicotine, the menthol and the 1, 2-propylene glycol and the glycerol with high mass fractions in the electronic cigarette liquid, has accurate and reliable quantitative results and good reproducibility, improves the analysis and test flux, can save the batch analysis time, and is suitable for rapid quantitative detection of the main components of the electronic cigarette liquid.
Description
Technical Field
The invention belongs to the technical field of detection of main components of electronic cigarette liquid, and particularly relates to a GC-TCD (gas chromatography-thermal conductivity detector) combined detection method of the main components of the electronic cigarette liquid.
Background
The electronic cigarette is a novel tobacco product, utilizes electronic equipment to simulate the smoke of a traditional cigarette, atomizes a nicotine-containing solution and provides a smoker with a satisfaction similar to the smoking of the traditional cigarette. The electronic cigarette liquid mainly comprises a fuming solvent, essence liquid, nicotine (or tobacco extract), water and other raw materials. Wherein, the fuming solvent (also called atomizing agent) accounts for about 90 percent of the electronic cigarette liquid, and 1, 2-propylene glycol and glycerol are generally adopted; the essence liquid content is low, and the component difference is huge according to different tastes; the nicotine content is generally between 0 and 3%. Moisture is one of the key components of the smoke of the electronic cigarette, and because glycerin and 1, 2-propylene glycol have strong hygroscopicity, the moisture content has an important influence on the quality of the smoke liquid of the electronic cigarette. In order to meet the requirements of formulation development and quality monitoring of electronic cigarette liquid, the atomization agent in the electronic cigarette liquid needs to be simply, conveniently, quickly and accurately measured.
At present, the most widely used technology for analyzing the content of nicotine, 1, 2-propylene glycol and glycerol in the cigarette liquid of the electronic cigarette is Gas Chromatography (GC), and the method has the advantages of simple sample treatment, accurate and sensitive quantification, short analysis time, low instrument maintenance cost, environment-friendly use and the like. However, because the content difference between nicotine and 1, 2-propylene glycol and glycerol in the cigarette liquid of the electronic cigarette is large, the existing analysis method generally detects moisture, nicotine and polyol solvents in a classified manner, which is relatively time-consuming and labor-consuming and has high detection cost.
In order to solve the problems of the existing detection technology, the literature 'GC-TCD method for simultaneously detecting the moisture of aerosol of a non-combustible heated cigarette and the release amount of nicotine, glycerol, 1, 2-propylene glycol, glyceryl triacetate and menthol' (Wangkang et al, tobacco science and technology, 2019.03, 63-68) discloses an analysis method combining a gas chromatography with a thermal conductivity detector, aiming at the aerosol of the non-combustible heated cigarette, isopropanol containing an internal standard is used as an extracting agent, n-butyl alcohol is used as an internal standard to carry out quantitative determination on the moisture, and 1, 3-butanediol is used as an internal standard to carry out simultaneous determination on the nicotine, the glycerol, the 1, 2-propylene glycol, the glyceryl triacetate and the menthol. However, the test object of the technique disclosed in this document is the heating of a non-combustible cigarette aerosol, and this technique cannot be directly used for testing relevant components in e-liquid.
For example, in the document "GC-TCD method for simultaneously detecting the content of solvent and moisture in tobacco flavor (kekunye leaf, etc., flavor and fragrance cosmetics 2020.10, 16-18, 23), an analytical method combining gas chromatography and a thermal conductivity detector is also disclosed, and the content of ethanol, water, 1, 2-propanediol and glycerol in tobacco flavor can be simultaneously detected by using methanol as an extraction agent and n-butanol as an internal standard. However, the test object of the technology disclosed in this document is a tobacco flavor and cannot be directly used for testing relevant components in electronic cigarette liquid.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method capable of simultaneously detecting moisture, nicotine, glycerol, 1, 2-propylene glycol and menthol in electronic cigarette liquid, and aims to provide technical support for the rapid determination of main components in the electronic cigarette liquid. Specifically, the following technique is used.
A method for detecting main components of electronic cigarette liquid based on GC-TCD combination comprises the following steps:
s1, preprocessing a sample; weighing electronic cigarette liquid and isopropanol solution containing internal standard substance with weight volume ratio of 15mg/ml, and oscillating for 5min to obtain extract;
the internal standard substance is N-butyl alcohol and N, N-dimethylformamide, and the concentrations of the internal standard substance in the isopropanol solution are 1mg/ml and 0.2mg/ml respectively;
s2, preparing a standard working solution for GC-TCD analysis.
Compared with the prior art which adopts N-butanol and 1, 3-butanediol as internal standard substances, the method has the advantages that the peak shape symmetry of the detection result is better, no obvious tailing phenomenon exists on chromatographic peaks of 1, 2-propanediol and glycerol, and the detection sensitivity on nicotine and menthol is higher.
Preferably, in step S2, the preparation method of the standard working solution is: weighing water, 1, 2-propylene glycol, glycerol, menthol and nicotine, adding the water, the 1, 2-propylene glycol, the glycerol, the menthol and the nicotine into isopropanol to prepare corresponding standard stock solutions, wherein the concentrations of the 1, 2-propylene glycol and the glycerol are both 60mg/mL, the concentration of the water is 30mg/mL, and the concentrations of the menthol and the nicotine are both 3mg/mL; and then 0.05ml, 0.1ml, 0.2ml, 0.5ml, 1ml and 2ml of the standard stock solution are respectively taken and added with 10ml of isopropanol solution containing the internal standard to prepare 6-grade standard working solution.
And quantifying by adopting an internal standard method when the 6 series of standard working solutions are subjected to GC analysis, and making a standard working curve. Performing linear regression analysis on the ratio of the peak areas of the 5 target compounds to the peak areas of the corresponding internal standards and the ratio of the concentrations of the 5 target compounds to the internal standards to obtain 5 standard working curves and correlation coefficients of the target compounds; and (3) injecting the standard solution with the minimum concentration for 8 times, calculating the standard deviation of the measurement result, and determining the detection limit and the quantification limit by respectively using 3 times and 10 times of the standard deviation. The results show that the working curves of the 5 targets are good in linearity, and the correlation coefficients are all higher than 0.999; the quantitative limit of each target object is lower than the content of the target object in the extraction liquid, and the method is suitable for quantitative analysis.
Preferably, in step S2, during GC-TCD analysis, the temperature rise procedure of GC is: maintaining the initial temperature at 100 deg.C for 2.5min; heating to 250 deg.C and maintaining for 3min; the temperature of a sample inlet is 260 ℃; the temperature of the TCD detector is 260 ℃, the carrier gas is helium, the flow rate of the carrier gas is 1.5ml/min, and the constant-current mode is adopted; tail gas blowing helium gas 30ml/min; the injection volume is 1 mul, the split injection is carried out, and the split ratio is 10-100.
Preferably, in step S2, the temperature increase rate of the GC is 20 ℃/min.
More preferably, the split ratio is 20. In order to ensure that the sample injection detection amount of the high-concentration component is not overloaded and simultaneously can meet the detection sensitivity requirement of the low-concentration component, the split ratio of the chromatographic column is investigated. When the split ratio is less than 10:1, the chromatographic peaks of 1, 2-propylene glycol and glycerol have trailing phenomena; when the split ratio is more than 100: at 1, the sensitivity of nicotine and menthol is low. When the shunt ratio is 20.
Preferably, in step S2, the column used for GC-TCD analysis is a capillary column of type DB-1701, with dimensions 30m × 0.32mm, 1.0. Mu.m. The separation effect of four chromatographic columns with different polarities DB-1, DB-5, DB-1701 and DB-INNOWAX on the target object is studied. In DB-1, 2-propylene glycol and glycerol cannot be effectively separated; in DB-5, although the tested substances can be separated, the 1, 2-propylene glycol and glycerol have serious peak tailing; in DB-INNOWAX, nicotine and 1, 2-propanediol peak at a later time, which is not suitable for rapid detection of samples. In contrast, 5 targets were separated relatively well using a DB-1701 column.
Compared with the prior art, the invention has the advantages that: according to the method, N-butanol and N, N-dimethylformamide are used as internal standard substances for GC-TCD combined detection of the main components of the electronic cigarette liquid, the peak shape symmetry of the detection result is better, no obvious tailing phenomenon exists on chromatographic peaks of 1, 2-propylene glycol and glycerol, and the detection sensitivity on nicotine and menthol is higher.
Drawings
FIG. 1 is a chromatogram of an isolated standard of example 1;
in the figure, 1 is the chromatographic peak of water; 2 is the chromatographic peak of n-butanol; 3 is the chromatographic peak of 1, 3-butanediol; 4 is the chromatographic peak of N, N-dimethylformamide; 5 is the chromatographic peak of glycerol; 6 is the chromatographic peak of menthol; 7 is the chromatographic peak for nicotine:
Detailed Description
The technical solutions of the present invention will be described clearly and completely below, and it should be apparent that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
Examples
The method for detecting the main components of the electronic cigarette liquid based on GC-TCD combination provided by the embodiment is as follows.
1. Instruments, reagents and materials
(1) The instrument comprises the following steps: an Agilent 7890A gas chromatograph (Agilent, usa) equipped with a thermal conductivity detector; HY-5A rotary oscillator (Toyoxinri instruments, toyodong, gold Tan, city); 10ml, 1000. Mu.l, 200. Mu.l pipettes (Gilson Corp., USA); an AL204 electronic balance (sensory: 0.0001g, mettler Toledo, switzerland); elastic quartz capillary chromatography columns DB-1701 (30 m.times.0.32mm, 1.0 μm), DB-5 (30 m.times.0.32mm, 1.0 μm), DB-1 (30 m.times.0.32mm, 1.0 μm), DB-INNOWAX (30 m.times.0.32mm, 1.0 μm).
(2) Reagent: nicotine-isopropyl alcohol solution (about 10mg/ml, provided by national tobacco quality supervision and inspection center); 1, 2-propylene glycol, glycerol, N-dimethylformamide, N-butanol and menthol (purity more than or equal to 99%, chemical reagent of national medicine group, ltd.); isopropanol (chromatographically pure, CNW, germany).
(3) Materials: the electronic cigarette liquid is a commercial product.
2. Sample pretreatment
Weighing 0.15g of electronic cigarette liquid, adding 10ml of isopropanol solution containing an internal standard (the concentration of N-butyl alcohol of the internal standard in the solution is 1mg/ml, and the concentration of N, N-dimethylformamide is 0.2 mg/ml), and oscillating for 5min to obtain an extract.
3. Preparation of Standard working solutions for GC-TCD analysis and discussion of results
The preparation method of the standard working solution comprises the following steps: weighing water, 1, 2-propylene glycol, glycerol, menthol and nicotine, adding the water, the 1, 2-propylene glycol, the glycerol, the menthol and the nicotine into isopropanol to prepare corresponding standard stock solutions, wherein the concentrations of the 1, 2-propylene glycol and the glycerol are both 60mg/ml, the concentration of the water is 30mg/ml, and the concentrations of the menthol and the nicotine are both 3mg/ml; and then 0.05ml, 0.1ml, 0.2ml, 0.5ml, 1ml and 2ml of the standard stock solution are respectively taken and added with 10ml of isopropanol solution containing the internal standard to prepare 6-grade standard working solution.
The specific method of GC-TCD analysis is as follows: and (3) carrying out GC analysis on the 6-grade standard working solution, quantifying by adopting an internal standard method, and making a standard working curve. The adopted chromatographic columns are DB-1, DB-5, DB-1701 and DB-INNOWAX chromatographic columns with different polarities; maintaining the initial temperature at 100 deg.C for 2.5min; heating to 250 deg.C and maintaining for 3min; the temperature of a sample inlet is 260 ℃; the temperature of the TCD detector is 260 ℃, the carrier gas is helium, the flow rate of the carrier gas is 1.5mL/min, and the constant-current mode is adopted; tail gas blowing helium gas 30mL/min; the sample injection volume is 1 mu L, and the sample is divided and injected, wherein the flow dividing ratio is 200;
performing linear regression analysis by using the ratio of the peak area of each target to the peak area of the corresponding internal standard and the ratio of the concentration of each target to the concentration of the internal standard to obtain a standard working curve and a correlation coefficient of each target compound; and (2) sampling the standard solution with the minimum concentration for 8 times, calculating the standard deviation of the measurement result, and determining the detection limit and the quantification limit by respectively using 3 times and 10 times of the standard deviation, wherein the calculation result is shown in the following table 1, the working curves of 6 targets have good linearity, the correlation coefficients are all higher than 0.999, and the quantification limit of each target is lower than the content of the target in the extraction liquid, so that the method is suitable for quantitative analysis.
Standard working curves for the Compounds of Table 1
For 4 electronic cigarette liquid samples, 5 target objects are subjected to GC-TCD measurement by using a chromatographic column DB-1701, the chromatogram of the separated standard sample is shown in figure 1, and the analysis results of the 5 target objects in the 4 electronic cigarette liquid samples are shown in the following table 2.
TABLE 2 four electronic cigarette liquid sample analysis results (mg/g)
| Number of | Moisture content | 1, 2-propanediol | Glycerol | Menthol | Nicotine |
| 1 | 174.3 | 415.1 | 502.1 | 6.4 | 8.3 |
| 2 | 159.0 | 403.7 | 519.5 | 8.1 | 8.2 |
| 3 | 79.2 | 387.3 | 528.5 | — | 9.5 |
| 4 | 89.1 | 322.4 | 469.5 | 4.6 | 6.3 |
The results shown in table 2 above show that 1, 2-propylene glycol and glycerol were detected in all samples, and the total content of the two components was 791.9-923.1mg/g, which is the main component of the electronic cigarette liquid.
The content of 1, 2-propylene glycol and glycerol in the electronic cigarette liquid is greatly different from the content of water, nicotine and menthol, in this embodiment, N-butanol is used as an internal standard to perform quantitative determination on 1, 2-propylene glycol and glycerol, and N, N-dimethylformamide is used to perform quantitative determination on water, nicotine and menthol. The retention time of the N-butanol and the N, N-dimethylformamide are respectively 3.0min and 5.8min, no overlapping with other components of the sample is generated, and the peak shape symmetry is good, so that the N-butanol and the N, N-dimethylformamide are very suitable to be used as internal standard substances for measuring the 5 target substances in the electronic cigarette liquid.
Taking 3 parts of electronic cigarette liquid samples with known content, adding water, 1, 2-propylene glycol, glycerol, menthol and nicotine standard solution according to low, medium and high levels respectively, and repeatedly measuring each adding level for 6 times. The samples were pretreated and chromatographed as described above and the recovery and Relative Standard Deviation (RSD) calculated from the original content, amount added and amount detected by spiking. The results in Table 3 below show that the normalized recoveries of water, 1, 2-propanediol, glycerol, menthol and nicotine were 97.1-102.5%, 97.9-101.2%, 103.2-107.5%, 96.9-106.1% and 94.2-98.1%, respectively, with a Relative Standard Deviation (RSD) of 0.59-7.78%. Therefore, the method has the advantages of high precision and high recovery rate, and is suitable for quantitative analysis of water, 1, 2-propylene glycol, glycerol, menthol and nicotine in the electronic cigarette extract.
TABLE 3 recovery of the analytical method with addition of standard
In conclusion, the method for detecting 5 main components in the electronic cigarette liquid provided by the invention can be used for simply, conveniently and quickly analyzing the water, the 1, 2-propylene glycol, the glycerol, the menthol and the nicotine in the electronic cigarette liquid at the same time, measuring the water, the nicotine, the menthol and the 1, 2-propylene glycol and the glycerol with high mass fractions in the electronic cigarette liquid, and has the advantages of accurate and reliable quantitative result, good reproducibility, improved analysis and test flux, batch analysis time saving and suitability for quick quantitative detection of the main components in the electronic cigarette liquid.
Claims (3)
1. A method for detecting main components of electronic cigarette liquid based on GC-TCD combination is characterized by comprising the following steps:
s1, preprocessing a sample; weighing electronic cigarette liquid and isopropanol solution containing an internal standard substance, wherein the weight volume ratio is 15mg/mL, and oscillating to obtain extract liquor;
the internal standard substance is N-butyl alcohol and N, N-dimethylformamide, and the concentrations of the internal standard substance in the isopropanol solution are 1mg/mL and 0.2mg/mL respectively;
s2, preparing a standard working solution for carrying out GC-TCD analysis on main components of the electronic cigarette liquid, wherein the main components comprise water, 1, 2-propylene glycol, glycerol, menthol and nicotine; the method comprises the following steps of (1) carrying out quantitative determination on water, nicotine and menthol by using N, N-dimethylformamide as an internal standard, and carrying out quantitative determination on 1, 2-propylene glycol and glycerol by using N-butyl alcohol as an internal standard;
when in GC-TCD analysis, the used chromatographic column is a DB-1701 type capillary column, the size is 30m multiplied by 0.32mm, and the diameter is 1.0 mu m; the temperature program of the GC is: maintaining the initial temperature at 100 deg.C for 2.5min; heating to 250 deg.C for 3min, and heating at 20 deg.C/min by GC; the temperature of a sample inlet is 260 ℃; the temperature of the TCD detector is 260 ℃, the carrier gas is helium, the flow rate of the carrier gas is 1.5mL/min, and the constant-current mode is adopted; tail gas blowing helium gas 30mL/min; the sample injection volume is 1 mu L, and the split injection is performed, wherein the split ratio is 10-100.
2. The detection method according to claim 1, wherein in step S2, the standard working solution is prepared by: weighing water, 1, 2-propylene glycol, glycerol, menthol and nicotine, adding the water, the 1, 2-propylene glycol, the glycerol, the menthol and the nicotine into isopropanol to prepare corresponding standard stock solutions, wherein the concentrations of the 1, 2-propylene glycol and the glycerol are both 60mg/mL, the concentration of the water is 30mg/mL, and the concentrations of the menthol and the nicotine are both 3mg/mL; and then 0.05mL, 0.1mL, 0.2mL, 0.5mL, 1mL and 2mL of the standard stock solution are respectively taken and added with 10mL of isopropanol solution containing the internal standard to prepare 6-grade standard working solution.
3. The detection method according to claim 1, wherein in step S2, the split ratio is 20.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103645262A (en) * | 2013-12-18 | 2014-03-19 | 中国烟草总公司湖北省公司 | Method for measuring benzene volatile organic compounds in cigarette filters by using headspace gas chromatograph |
| CN103808831A (en) * | 2014-03-16 | 2014-05-21 | 国家烟草质量监督检验中心 | Method for simultaneously determining content of 1,2-propylene glycol, menthol, diethylene glycol, glycerin and triethylene glycol in electronic cigarette juice |
| CN111272938A (en) * | 2020-03-19 | 2020-06-12 | 中国烟草总公司郑州烟草研究院 | Method for simultaneously measuring moisture, nicotine, propylene glycol and glycerol in electronic cigarette liquid |
| CN112505227A (en) * | 2020-12-29 | 2021-03-16 | 广西中烟工业有限责任公司 | Analysis method for simultaneously determining 11 components in electronic cigarette liquid |
Family Cites Families (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4145518A (en) * | 1976-12-06 | 1979-03-20 | Eastman Kodak Company | Fibers, filter rods and other nonwoven articles made from poly(1,2-propylene terephthalate)copolyesters of terephthalic acid, 1,2-propylene glycol and ethylene glycol |
| JPH1194812A (en) * | 1997-09-22 | 1999-04-09 | Asahi Breweries Ltd | Detection of diols in beverage |
| JP2005134274A (en) * | 2003-10-31 | 2005-05-26 | Jfe Steel Kk | Quantitative analytical method for aldehyde in solid sample |
| CN102128885B (en) * | 2010-12-08 | 2013-01-30 | 广东中烟工业有限责任公司 | Method for quickly and simultaneously detecting 16 inorganic anions and organic acids in tobacco |
| US9254001B2 (en) * | 2011-04-27 | 2016-02-09 | R.J. Reynolds Tobacco Company | Tobacco-derived components and materials |
| CN103969387B (en) * | 2014-05-08 | 2016-01-27 | 浙江中烟工业有限责任公司 | The method of the menthol content in Headspace Gas Chromatography Cigarette paper |
| CN103969389A (en) * | 2014-05-14 | 2014-08-06 | 合肥工业大学 | Gas chromatography detection method for trace N,N-dimethyl formamide in synthesized leather |
| CN104569197B (en) * | 2014-12-30 | 2016-10-26 | 广东中烟工业有限责任公司 | The silanization GC/MS detection method of sugar, 1,2-propylene glycol and the glycerol in mensuration Nicotiana tabacum L. simultaneously |
| CN109470781A (en) * | 2018-10-20 | 2019-03-15 | 南通烟滤嘴有限责任公司 | Measure double internal standard Chromatography test method methods of a variety of organic component contents in cellulose acetate filter rod |
-
2021
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103645262A (en) * | 2013-12-18 | 2014-03-19 | 中国烟草总公司湖北省公司 | Method for measuring benzene volatile organic compounds in cigarette filters by using headspace gas chromatograph |
| CN103808831A (en) * | 2014-03-16 | 2014-05-21 | 国家烟草质量监督检验中心 | Method for simultaneously determining content of 1,2-propylene glycol, menthol, diethylene glycol, glycerin and triethylene glycol in electronic cigarette juice |
| CN111272938A (en) * | 2020-03-19 | 2020-06-12 | 中国烟草总公司郑州烟草研究院 | Method for simultaneously measuring moisture, nicotine, propylene glycol and glycerol in electronic cigarette liquid |
| CN112505227A (en) * | 2020-12-29 | 2021-03-16 | 广西中烟工业有限责任公司 | Analysis method for simultaneously determining 11 components in electronic cigarette liquid |
Non-Patent Citations (1)
| Title |
|---|
| GC-TCD 法同时检测加热不燃烧卷烟气溶胶水分，及烟碱、丙三醇、1,2-丙二醇、三乙酸甘油酯和薄荷醇的释放量;王康 等;《烟草科技》;20190331;第52卷(第3期);第63-64页 * |
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