CN112505227A - Analysis method for simultaneously determining 11 components in electronic cigarette liquid - Google Patents
Analysis method for simultaneously determining 11 components in electronic cigarette liquid Download PDFInfo
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- CN112505227A CN112505227A CN202011593990.6A CN202011593990A CN112505227A CN 112505227 A CN112505227 A CN 112505227A CN 202011593990 A CN202011593990 A CN 202011593990A CN 112505227 A CN112505227 A CN 112505227A
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- 238000004458 analytical method Methods 0.000 title claims abstract description 28
- 239000003571 electronic cigarette Substances 0.000 title claims abstract description 25
- 239000007788 liquid Substances 0.000 title claims abstract description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 54
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 54
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 51
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims abstract description 51
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 48
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims abstract description 32
- YPFDHNVEDLHUCE-UHFFFAOYSA-N propane-1,3-diol Chemical compound OCCCO YPFDHNVEDLHUCE-UHFFFAOYSA-N 0.000 claims abstract description 30
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 22
- SNICXCGAKADSCV-JTQLQIEISA-N (-)-Nicotine Chemical compound CN1CCC[C@H]1C1=CC=CN=C1 SNICXCGAKADSCV-JTQLQIEISA-N 0.000 claims abstract description 20
- 229960002715 nicotine Drugs 0.000 claims abstract description 20
- SNICXCGAKADSCV-UHFFFAOYSA-N nicotine Natural products CN1CCCC1C1=CC=CN=C1 SNICXCGAKADSCV-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000000243 solution Substances 0.000 claims abstract description 19
- 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 18
- NOOLISFMXDJSKH-UHFFFAOYSA-N DL-menthol Natural products CC(C)C1CCC(C)CC1O NOOLISFMXDJSKH-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229940041616 menthol Drugs 0.000 claims abstract description 18
- 229960004063 propylene glycol Drugs 0.000 claims abstract description 18
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000004587 chromatography analysis Methods 0.000 claims abstract description 15
- 238000004817 gas chromatography Methods 0.000 claims abstract description 14
- 239000011550 stock solution Substances 0.000 claims abstract description 12
- 239000006228 supernatant Substances 0.000 claims abstract description 12
- 238000005303 weighing Methods 0.000 claims abstract description 7
- PUPZLCDOIYMWBV-UHFFFAOYSA-N (+/-)-1,3-Butanediol Chemical compound CC(O)CCO PUPZLCDOIYMWBV-UHFFFAOYSA-N 0.000 claims description 26
- SMUQFGGVLNAIOZ-UHFFFAOYSA-N quinaldine Chemical compound C1=CC=CC2=NC(C)=CC=C21 SMUQFGGVLNAIOZ-UHFFFAOYSA-N 0.000 claims description 26
- 239000012159 carrier gas Substances 0.000 claims description 20
- 239000012224 working solution Substances 0.000 claims description 14
- 235000019437 butane-1,3-diol Nutrition 0.000 claims description 13
- 239000007789 gas Substances 0.000 claims description 12
- 150000001875 compounds Chemical class 0.000 claims description 11
- 238000007664 blowing Methods 0.000 claims description 10
- 239000001307 helium Substances 0.000 claims description 10
- 229910052734 helium Inorganic materials 0.000 claims description 10
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 10
- 239000000126 substance Substances 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000002347 injection Methods 0.000 claims description 7
- 239000007924 injection Substances 0.000 claims description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 6
- 238000001165 gas chromatography-thermal conductivity detection Methods 0.000 claims description 6
- 239000012491 analyte Substances 0.000 claims description 5
- 238000000769 gas chromatography-flame ionisation detection Methods 0.000 claims description 5
- 239000013076 target substance Substances 0.000 claims description 5
- 239000001257 hydrogen Substances 0.000 claims description 4
- 229910052739 hydrogen Inorganic materials 0.000 claims description 4
- 230000010355 oscillation Effects 0.000 claims description 4
- 238000012546 transfer Methods 0.000 claims description 4
- 239000012086 standard solution Substances 0.000 claims description 2
- 238000001514 detection method Methods 0.000 abstract description 6
- 235000019504 cigarettes Nutrition 0.000 abstract description 2
- 239000000523 sample Substances 0.000 description 32
- 229960005150 glycerol Drugs 0.000 description 14
- 238000011084 recovery Methods 0.000 description 6
- DNIAPMSPPWPWGF-GSVOUGTGSA-N (R)-(-)-Propylene glycol Chemical compound C[C@@H](O)CO DNIAPMSPPWPWGF-GSVOUGTGSA-N 0.000 description 4
- 241000208125 Nicotiana Species 0.000 description 4
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 4
- 235000013772 propylene glycol Nutrition 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 235000011389 fruit/vegetable juice Nutrition 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- DNIAPMSPPWPWGF-VKHMYHEASA-N (+)-propylene glycol Chemical compound C[C@H](O)CO DNIAPMSPPWPWGF-VKHMYHEASA-N 0.000 description 2
- 229940035437 1,3-propanediol Drugs 0.000 description 2
- 238000003556 assay Methods 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000007865 diluting Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229940093476 ethylene glycol Drugs 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 229920000166 polytrimethylene carbonate Polymers 0.000 description 2
- 239000012488 sample solution Substances 0.000 description 2
- 239000000779 smoke Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 229940058015 1,3-butylene glycol Drugs 0.000 description 1
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229960004756 ethanol Drugs 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 235000013355 food flavoring agent Nutrition 0.000 description 1
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000010813 internal standard method Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000001294 liquid chromatography-tandem mass spectrometry Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 230000001953 sensory effect Effects 0.000 description 1
- 230000000391 smoking effect Effects 0.000 description 1
- 238000012795 verification 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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
-
- 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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
-
- 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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
- G01N2030/884—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample organic compounds
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- 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 relates to an analysis method for simultaneously measuring 11 components in cigarette liquid of an electronic cigarette, which comprises the following steps: (1) weighing an electronic cigarette liquid sample, adding an internal standard stock solution and an isopropanol solution, uniformly oscillating, and transferring a supernatant into a chromatographic analysis bottle to be detected; (2) taking the supernatant obtained in the step (1) for Gas Chromatography (GC) analysis; (3) and calculating the content of the target object in the sample. The method realizes the simultaneous detection of the components in 11 such as methanol, ethanol, ethylene glycol, 1, 2-propylene glycol, 1, 3-propylene glycol, glycerol, diethylene glycol, menthol, triethylene glycol, nicotine, water and the like in the electronic cigarette liquid.
Description
Technical Field
The invention belongs to the technical field of tobacco chemical analysis, and particularly relates to an analysis method for simultaneously determining 11 components in electronic cigarette liquid.
Background
Electronic cigarette tobacco juice is electronic atomization liquid used in cooperation with an electronic cigarette, and the inherent quality of the electronic cigarette tobacco juice directly influences the smoking feeling of a consumer on the electronic cigarette, so that people pay attention to some key substances in the electronic cigarette tobacco juice. 1, 2-propylene glycol and glycerol are widely used solvents in electronic cigarette liquid, ethanol and water are widely used auxiliary solvents or additives, methanol, diethylene glycol, ethylene glycol, triethylene glycol and 1, 3-propylene glycol are possibly taken as impurities of the 1, 2-propylene glycol and the glycerol or other approaches to be brought into the cigarette liquid to bring adverse effects to human health and are widely concerned, and menthol is the most widely used flavoring agent in the electronic cigarette liquid. Currently, the main methods for measuring such substances are gas chromatography, gas chromatography-mass spectrometry, continuous flow method, raman spectroscopy, liquid chromatography-tandem mass spectrometry, etc., but these methods have low throughput and have little or no research on substances such as diethylene glycol, triethylene glycol, water, methanol, ethanol, menthol, etc.
The invention content is as follows:
the invention aims to establish an analysis method for simultaneously measuring 11 components in the electronic cigarette liquid (methanol, ethanol, ethylene glycol, 1, 2-propylene glycol, 1, 3-propylene glycol, glycerol, diethylene glycol, menthol, triethylene glycol, nicotine and water) based on the technical defects, and is suitable for general survey analysis of electronic cigarette liquid samples.
The purpose of the invention is realized by the following technical scheme:
an analysis method for simultaneously measuring 11 components in electronic cigarette liquid comprises the following steps:
(A) weighing an electronic cigarette liquid sample, placing the electronic cigarette liquid sample in a centrifugal tube with a plug scale, adding an internal standard stock solution and an isopropanol solution, oscillating and uniformly mixing, and taking supernatant to transfer to a chromatographic analysis bottle to be detected.
(B) Taking the supernatant obtained after uniformly mixing in the step (A) for Gas Chromatography (GC) analysis;
(C) and calculating the content of the target object in the sample.
Preferably, in step (A), the internal standard solution is an isopropanol solution of 1, 3-butanediol and 2-methylquinoline at concentrations of 100mg/mL and 10mg/mL, respectively.
Preferably, in step (a), 1, 3-butanediol is an internal standard for compounds other than nicotine and 2-methylquinoline is an internal standard for nicotine.
Preferably, in the step (A), the oscillation time is 10-30 min, preferably 10 min.
Preferably, in step (a), the speed of oscillation is 200 rpm.
Preferably, in step (B), the chromatographic conditions of the gas chromatographic analysis comprise:
methanol, ethanol, ethylene glycol, 1, 2-propanediol, 1, 3-propanediol, glycerol, diethylene glycol, menthol, triethylene glycol, nicotine were separated using a DB-ALC1 capillary column (30m × 0.32mm, 1.8 μm), and analyzed by GC-FID;
adopting a temperature programming mode: the initial temperature is 90 ℃, the temperature is kept for 1min, the temperature is increased to 120 ℃ at the speed of 15 ℃/min, the temperature is kept for 3min, the temperature is increased to 250 ℃ at the speed of 40 ℃/min, the temperature is kept for 3min, and the total running time is 12.25 min;
carrier gas: helium gas; the flow rate of the carrier gas is 1.8 mL/min;
tail blowing: 20 mL/min; air: 450 mL/min; hydrogen gas: 40 mL/min;
sample inlet temperature: 250 ℃; detector temperature: 275 ℃; sample introduction amount: 1 mu L of the solution; the split ratio is as follows: 20:1.
② the water was separated by using HP-PLOT/Q capillary chromatography column (30 m.times.0.53 mm, 40 μm) to
GC-TCD analysis;
adopting a temperature programming mode: the initial temperature is 100 ℃, the temperature is kept for 1min, the temperature is increased to 220 ℃ at the speed of 15 ℃/min, the temperature is kept for 6min, and the total operation time is 15 min;
carrier gas: helium gas; the flow rate of the carrier gas is 4.0 mL/min;
tail blowing: 8 mL/min; reference gas: 20 mL/min;
sample inlet temperature: 250 ℃; detector temperature: 250 ℃; sample introduction amount: 2 mu L of the solution; the split ratio is as follows: 5:1.
Preferably, in step (C), the content of the target in the sample is quantitatively calculated according to an internal standard curve method which is: preparing a series of standard working solutions containing a target substance, adding internal standards (1, 3-butanediol and 2-methylquinoline), and establishing a standard curve by taking the concentration (mg/mL) of each target compound as a horizontal coordinate and taking the peak area ratio of an analyte to the internal standard substance as a vertical coordinate; substituting the analysis result of the step (B) into a standard working curve to obtain the content of the target object in the solution to be detected, and further calculating to obtain the content of each target object in the sample.
Preferably, the concentration ranges of each target in the series of standard working solutions are as follows: 0.25-10 mg/mL of 1, 2-propylene glycol and glycerol, 0.025-1 mg/mL of methanol, ethanol, ethylene glycol, 1, 3-propylene glycol, diethylene glycol, menthol, triethylene glycol and nicotine, and 0-1 mg/mL of water.
In a specific embodiment, the method comprises the steps of:
(A) weighing 0.1g of sample, accurately measuring the sample to 0.1mg, placing the sample in a centrifuge tube with a plug scale, adding 100 mu L of internal standard stock solution (isopropanol solution of 1, 3-butanediol and 2-methylquinoline with the concentration of 10mg/mL and 1mg/mL respectively), metering the volume to 10mL by using isopropanol, oscillating the solution on an oscillator at the rotating speed of 200rpm for 10min, and taking the supernatant to transfer to a chromatographic analysis bottle for detection.
(B) Taking the supernatant obtained in the step (A) to perform Gas Chromatography (GC) analysis, wherein the analysis conditions are as follows:
methanol, ethanol, ethylene glycol, 1, 2-propylene glycol, 1, 3-propylene glycol, glycerol, diethylene glycol, menthol, triethylene glycol, nicotine were separated using DB-ALC1 capillary chromatography column (30m × 0.32mm, 1.8 μm), and analyzed by GC-FID; the programmed heating mode is that the initial temperature is 90 ℃, the temperature is kept for 1min, the temperature is increased to 120 ℃ at the speed of 15 ℃/min, the temperature is kept for 3min, the temperature is increased to 250 ℃ at the speed of 40 ℃/min, the temperature is kept for 3min, and the total running time is 12.25 min; the carrier gas is helium; the flow rate of the carrier gas is 1.8 mL/min; tail blowing 20 mL/min; air 450 mL/min; hydrogen is 40 mL/min; the temperature of a sample inlet is 250 ℃; the detector temperature was 275 ℃; the sample injection amount is 1 mu L; the split ratio was 20: 1.
The water was separated using an HP-PLOT/Q capillary chromatography column (30 m.times.0.53 mm, 40 μm), analyzed by GC-TCD; the programmed heating mode is that the initial temperature is 100 ℃, the temperature is kept for 1min, the temperature is increased to 220 ℃ at the speed of 15 ℃/min, the temperature is kept for 6min, and the total operation time is 15 min; the carrier gas is helium; the flow rate of the carrier gas is 4.0 mL/min; blowing 8mL/min at the tail; 20mL/min of reference gas; the temperature of a sample inlet is 250 ℃; the temperature of the detector is 250 ℃; the sample injection amount is 2 mu L; the split ratio was 5: 1.
(C) Quantitatively calculating the content of the target object in the sample by adopting an internal standard curve method; wherein, the internal standard curve method is as follows: preparing a series of standard working solutions containing a target substance, adding internal standards (1, 3-butanediol and 2-methylquinoline), and establishing a standard curve by taking the concentration (mg/mL) of each target compound as a horizontal coordinate and taking the peak area ratio of an analyte to the internal standard substance as a vertical coordinate; substituting the analysis result of the step (B) into the standard curve to obtain the content of the target object in the solution to be detected, and further calculating to obtain the content of each target object in the sample.
Compared with the prior art, the invention has at least the following beneficial technical effects:
the invention establishes an analysis method for simultaneously measuring 11 components in the electronic cigarette liquid based on GC technology, realizes the simultaneous analysis of methanol, ethanol, ethylene glycol, 1, 2-propylene glycol, 1, 3-propylene glycol, glycerol, diethylene glycol, menthol, triethylene glycol, nicotine and water, has the advantages of high flux, good sensitivity, repeatability and recovery rate and the like, and is suitable for the general investigation analysis of electronic cigarette liquid samples.
Drawings
FIG. 1 is a chromatogram of a target and an internal standard in a standard working solution (internal standard 1: 1, 3-butanediol; internal standard 2: 2-methylquinoline);
FIG. 2 is a chromatogram of a target and an internal standard in a typical sample solution (internal standard 1: 1, 3-butanediol; internal standard 2: 2-methylquinoline).
Detailed Description
The technical solution of the present invention will be further described below with reference to specific embodiments.
Example 1: analysis method for simultaneously determining 11 components in electronic cigarette liquid
(1) Instruments and reagents
The instrument comprises the following steps: the gas chromatograph is Bruker456GC, and is provided with a hydrogen flame detector (FID) and a Thermal Conductivity Detector (TCD), the sample inlet has a split-flow sample injection mode, and the sample inlet, the column box and the detector are respectively provided with an independently controllable heating unit; an oscillator (YY-5A, Riwa instruments manufacturing Co., Ltd.); analytical balance (AE163, Mettler, Switzerland, sensory: 0.1 mg).
Reagent consumables: methanol, ethanol from Merck (analytical grade); diethylene glycol, 1, 3-propylene glycol, glycerol, 1, 3-butylene glycol, menthol and ethylene glycol are purchased from AlfaAesar (the purity is more than or equal to 99 percent); 1, 2-propanediol from Sigma-Aldrich (purity ≥ 99.5%); triethylene glycol was purchased from TCI (purity > 99%), nicotine was purchased from TRC (purity > 99%); 2-methylquinoline from damas-beta (> 99% pure); the water is deionized water.
(2) Working conditions of the apparatus
Chromatographic conditions are as follows: methanol, ethanol, ethylene glycol, 1, 2-propylene glycol, 1, 3-propylene glycol, glycerol, diethylene glycol, menthol, triethylene glycol, nicotine were separated using DB-ALC1 capillary chromatography column (30m × 0.32mm, 1.8 μm), and analyzed by GC-FID; the programmed heating mode is that the initial temperature is 90 ℃, the temperature is kept for 1min, the temperature is increased to 120 ℃ at the speed of 15 ℃/min, the temperature is kept for 3min, the temperature is increased to 250 ℃ at the speed of 40 ℃/min, the temperature is kept for 3min, and the total running time is 12.25 min; the carrier gas is helium; the flow rate of the carrier gas is 1.8 mL/min; tail blowing 20 mL/min; air 450 mL/min; hydrogen is 40 mL/min; the temperature of a sample inlet is 250 ℃; the detector temperature was 275 ℃; the sample injection amount is 1 mu L; the split ratio was 20: 1.
The water was separated using an HP-PLOT/Q capillary chromatography column (30 m.times.0.53 mm, 40 μm), analyzed by GC-TCD; the programmed heating mode is that the initial temperature is 100 ℃, the temperature is kept for 1min, the temperature is increased to 220 ℃ at the speed of 15 ℃/min, the temperature is kept for 6min, and the total operation time is 15 min; the carrier gas is helium; the flow rate of the carrier gas is 4.0 mL/min; blowing 8mL/min at the tail; 20mL/min of reference gas; the temperature of a sample inlet is 250 ℃; the temperature of the detector is 250 ℃; the sample injection amount is 2 mu L; the split ratio was 5: 1.
(3) Sample pretreatment
Weighing 0.1g of sample, accurately measuring to 0.1mg, placing the sample in a centrifuge tube with a plug scale, adding 100 mu L of internal standard stock solution, metering to 10mL with isopropanol, oscillating on an oscillator at the rotating speed of 200rpm for 10min, and taking supernatant to transfer to a chromatographic analysis bottle to be measured.
(4) Standard working solution preparation
Preparation of internal standard stock solution: 10g of 1, 3-butanediol and 1g of 2-methylquinoline are accurately weighed into a 100mL brown volumetric flask (accurate to 0.1mg), isopropanol is added to dissolve and fix the volume to a scale, and then the internal standard stock solution is obtained.
Preparing standard stock solutions of methanol, ethanol, ethylene glycol, 1, 2-propylene glycol, 1, 3-propylene glycol, glycerol, diethylene glycol, menthol, triethylene glycol and nicotine: respectively and accurately weighing 1, 2-propylene glycol, glycerol and 0.5g of methanol, ethanol, ethylene glycol, 1, 3-propylene glycol, diethylene glycol, menthol, triethylene glycol and nicotine in a 50mL brown volumetric flask, and adding isopropanol to dissolve and fix the volume to a scale.
Preparing standard working solution of methanol, ethanol, ethylene glycol, 1, 2-propylene glycol, 1, 3-propylene glycol, glycerol, diethylene glycol, menthol, triethylene glycol and nicotine: and respectively transferring 25 mu L, 50 mu L, 100 mu L, 250 mu L, 500 mu L and 1000 mu L of standard stock solutions into a 10mL brown volumetric flask, respectively and accurately adding 100 mu L of internal standard stock solutions, and diluting with isopropanol to fix the volume to a scale, thus obtaining six standard working solutions.
Preparation of water standard working solution
And respectively transferring 0 mu L, 1 mu L, 2 mu L, 4 mu L, 7 mu L and 10 mu L of aqueous solution into a 10mL volumetric flask, respectively and accurately adding 100 mu L of internal standard stock solution, diluting with isopropanol, and fixing the volume to the scale to obtain six standard working solutions.
(5) Sample assay
Samples were tested according to the instrumental test conditions and the test was repeated twice for each sample. While a set of blanks was made for each sample batch.
And (3) respectively carrying out GC analysis on the standard working solution obtained in the step (4) and the sample solution obtained in the step (3), wherein chromatograms of the target substance in the standard working solution and the internal standard thereof are shown in figures 1 and 2. Quantifying by adopting an internal standard method, and establishing a standard curve by taking the concentration (mg/mL) of each target compound as a horizontal coordinate and taking the peak area ratio of an analyte to an internal standard substance as a vertical coordinate; and (4) substituting the analysis result of the step (3) into the standard curve to obtain the content of the target object in the solution to be detected, and further calculating to obtain the content of each target object in the sample.
(6) Method verification
Under the optimized condition, based on the concentration range of the target compound in the matrix, determining the linear range of the method, taking the corresponding concentration of the target compound with the signal-to-noise ratio of 3 as a detection Limit (LOD), calculating the quantitative Limit (LOQ) of the method according to the signal-to-noise ratio which is 10 times, calculating the standard addition recovery rate according to 3 addition levels of low, medium and high, adding 5 parallel samples at each level, and calculating the test precision according to the parallel test result. The recovery, detection limit and precision of the method are shown in table 1. As shown in the table, the recovery rate of the target compound is 98.5-102.3%, the detection limit is 0.03-1.13 mg/g, and the precision is 0.48-2.56%.
TABLE 1 recovery, detection limit and precision of 11 ingredients in E-cigarette smoke solution
| Serial number | Compound (I) | Recovery (%) | LOD(mg/g) | LOQ(mg/g) | Precision (%) |
| 1 | Methanol | 101.2 | 0.06 | 0.21 | 0.81 |
| 2 | Ethanol | 102.1 | 0.03 | 0.11 | 1.22 |
| 3 | Ethylene glycol | 100.8 | 0.37 | 1.24 | 1.35 |
| 4 | 1, 2-propanediol | 102.3 | 0.45 | 1.50 | 0.81 |
| 5 | 1, 3-propanediol | 98.6 | 0.48 | 1.60 | 1.13 |
| 6 | Glycerol | 99.5 | 1.13 | 3.75 | 1.21 |
| 7 | Diethylene glycol | 98.9 | 0.36 | 1.20 | 0.89 |
| 8 | Menthol | 99.6 | 0.03 | 0.10 | 0.92 |
| 9 | Triethylene glycol | 102.2 | 0.30 | 0.99 | 1.33 |
| 10 | Nicotine | 100.8 | 0.07 | 0.25 | 0.48 |
| 11 | Water (W) | 98.5 | 0.33 | 1.00 | 2.56 |
(7) Analysis of actual samples
The results of 20 representative e-cigarette smoke solutions tested according to the above assay are detailed in table 2. As can be seen from the table, in these samples, the water content was 2.30 to 51.18mg/g, the nicotine content was 1.49 to 5.80mg/g, the 1, 2-propanediol content was 204.71 to 499.00mg/g, the glycerol content was 407.90 to 682.64mg/g, the ethanol content was 1.30 to 8.56mg/g, the menthol content was 5.51 to 19.70mg/g, and none of the other components was detected.
TABLE 2 results of analysis of actual samples (unit: mg/g)
Note: "ND" means not detected
Claims (8)
1. An analysis method for simultaneously measuring 11 components in electronic cigarette liquid comprises the following steps:
(A) weighing an electronic cigarette liquid sample, placing the electronic cigarette liquid sample in a centrifugal tube with a plug scale, adding an internal standard stock solution and an isopropanol solution, uniformly oscillating, taking supernatant, and transferring the supernatant into a chromatographic analysis bottle to be detected;
(B) subjecting the supernatant obtained in step (a) to Gas Chromatography (GC) analysis;
(C) and calculating the content of the target object in the sample.
2. The method according to claim 1, wherein in step (a), the internal standard solution is an isopropanol solution of 1, 3-butanediol and 2-methylquinoline at concentrations of 100mg/mL and 10mg/mL, respectively.
3. The method according to claim 1, wherein in step (a), 1, 3-butanediol is an internal standard for compounds other than nicotine and 2-methylquinoline is an internal standard for nicotine.
4. The method according to claim 1, wherein in the step (A), the time of the oscillation is 10 to 30min and the speed of the oscillation is 200 rpm.
5. The method of any one of claims 1 to 4, wherein in step (B), the gas chromatography conditions comprise:
methanol, ethanol, ethylene glycol, 1, 2-propylene glycol, 1, 3-propylene glycol, glycerol, diethylene glycol, menthol, triethylene glycol, nicotine were separated using a DB-ALC1 capillary column, 30m × 0.32mm, 1.8 μm, and analyzed by GC-FID;
② the water was separated using HP-PLOT/Q capillary chromatography column, 30 m.times.0.53 mm, 40 μm, analyzed by GC-TCD.
6. The method of claim 5, wherein in step (B), the gas chromatographic conditions further comprise:
firstly, a GC-FID program heating mode is that the initial temperature is 90 ℃, the temperature is kept for 1min, the temperature is increased to 120 ℃ at the speed of 15 ℃/min, the temperature is kept for 3min, the temperature is increased to 250 ℃ at the speed of 40 ℃/min, and the temperature is kept for 3 min; the total running time is 12.25 min;
carrier gas: helium gas; the flow rate of the carrier gas is 1.8 mL/min;
tail blowing: 20 mL/min; air: 450 mL/min; hydrogen gas: 40 mL/min;
sample inlet temperature: 250 ℃; detector temperature: 275 ℃; sample introduction amount: 1 mu L of the solution; the split ratio is as follows: 20: 1;
secondly, the GC-TCD temperature programming mode is that the initial temperature is 100 ℃, the temperature is kept for 1min, the temperature is increased to 220 ℃ at the speed of 15 ℃/min, and the temperature is kept for 6 min; the total running time is 15 min;
carrier gas: helium gas; the flow rate of the carrier gas is 4.0 mL/min;
tail blowing: 8 mL/min; reference gas: 20 mL/min;
sample inlet temperature: 250 ℃; detector temperature: 250 ℃; sample introduction amount: 2 mu L of the solution; the split ratio is as follows: 5:1.
7. The method according to any one of claims 1 to 4, wherein in step (C), the content of the target in the sample is quantitatively calculated according to an internal standard curve method using: preparing a series of standard working solutions containing a target substance, adding internal standards of 1, 3-butanediol and 2-methylquinoline, and establishing a standard curve by taking the concentration mg/mL of each target compound as a horizontal coordinate and taking the peak area ratio of an analyte to the internal standard substance as a vertical coordinate; substituting the analysis result of the step (B) into a standard working curve to obtain the content of the target object in the solution to be detected, and further calculating to obtain the content of each target object in the sample;
in the series of standard working solutions, the concentration ranges of the targets are as follows: 0.25-10 mg/mL of 1, 2-propylene glycol and glycerol, 0.025-1 mg/mL of methanol, ethanol, ethylene glycol, 1, 3-propylene glycol, diethylene glycol, menthol, triethylene glycol and nicotine, and 0-1 mg/mL of water.
8. Method according to claim 1, characterized in that it comprises the following steps:
(A) weighing 0.1g of sample, accurately measuring the sample to 0.1mg, placing the sample in a centrifuge tube with a plug scale, adding 100 mu L of internal standard stock solution, metering the volume to 10mL by using isopropanol, oscillating the sample on an oscillator at the rotating speed of 200rpm for 10min, and taking supernatant to transfer to a chromatographic analysis bottle to be measured;
(B) taking the supernatant obtained in the step (A) to perform Gas Chromatography (GC) analysis, wherein the analysis conditions are as follows:
methanol, ethanol, ethylene glycol, 1, 2-propylene glycol, 1, 3-propylene glycol, glycerol, diethylene glycol, menthol, triethylene glycol, and nicotine were separated by using DB-ALC1 capillary chromatography column, 30m × 0.32mm, 1.8 μm, and analyzed by GC-FID; the programmed heating mode is that the initial temperature is 90 ℃, the temperature is kept for 1min, the temperature is increased to 120 ℃ at the speed of 15 ℃/min, the temperature is kept for 3min, the temperature is increased to 250 ℃ at the speed of 40 ℃/min, the temperature is kept for 3min, and the total running time is 12.25 min; the carrier gas is helium; the flow rate of the carrier gas is 1.8 mL/min; tail blowing 20 mL/min; air 450 mL/min; hydrogen is 40 mL/min; the temperature of a sample inlet is 250 ℃; the detector temperature was 275 ℃; the sample injection amount is 1 mu L; the split ratio is 20: 1;
the water was separated using an HP-PLOT/Q capillary chromatography column, 30 m.times.0.53 mm, 40 μm, analyzed by GC-TCD; the programmed heating mode is that the initial temperature is 100 ℃, the temperature is kept for 1min, the temperature is increased to 220 ℃ at the speed of 15 ℃/min, the temperature is kept for 6min, and the total operation time is 15 min; the carrier gas is helium; the flow rate of the carrier gas is 4.0 mL/min; blowing 8mL/min at the tail; 20mL/min of reference gas; the temperature of a sample inlet is 250 ℃; the temperature of the detector is 250 ℃; the sample injection amount is 2 mu L; the split ratio is 5: 1;
(C) quantitatively calculating the content of the target object in the sample by adopting an internal standard curve method; wherein, the internal standard curve method is as follows: preparing a series of standard working solutions containing a target substance, adding internal standards of 1, 3-butanediol and 2-methylquinoline, and establishing a standard curve by taking the concentration mg/mL of each target compound as a horizontal coordinate and taking the peak area ratio of an analyte to the internal standard substance as a vertical coordinate; substituting the analysis result of the step (B) into the standard curve to obtain the content of the target object in the solution to be detected, and further calculating to obtain the content of each target object in the sample.
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