CN104614465B - Nicotine, 1,2-propylene glycol and the method for glycerol content in a kind of electronic cigarette aerosol of mensuration simultaneously - Google Patents

Nicotine, 1,2-propylene glycol and the method for glycerol content in a kind of electronic cigarette aerosol of mensuration simultaneously Download PDF

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CN104614465B
CN104614465B CN201510086968.5A CN201510086968A CN104614465B CN 104614465 B CN104614465 B CN 104614465B CN 201510086968 A CN201510086968 A CN 201510086968A CN 104614465 B CN104614465 B CN 104614465B
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nicotine
glycerol
propylene glycol
electronic cigarette
aerosol
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CN104614465A (en
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韩书磊
陈欢
刘彤
田永峰
姜兴益
庞永强
侯宏卫
胡清源
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National Tobacco Quality Supervision and Inspection Center
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Abstract

One measure simultaneously nicotine in electronic cigarette aerosol, 1,2 propylene glycol and the method for glycerol content, comprise the following steps: first with a smoking machine being provided with conversion attachment means, electronic cigarette is aspirated, use cambridge filter trapping aerosol in nicotine, 1,2 propylene glycol and glycerol, use added with interior target aqueous isopropanol as extractant, the method using oscillation extraction extracts the nicotine on filter disc, utilize gas chromatograph to join flame ionization ditector to be analyzed, inner mark method ration.It is an advantage of the current invention that: used assay method efficiency is high, conversion attachment means air-tightness is good, simple effective, nicotine, 1,2 propylene glycol and glycerol are good in respective range of linearity internal linear relation, and detection is limited to 0.40 ~ 2.16 μ g/mL, the average recovery rate of 3 mark-on levels is between 96.0% ~ 102.0%, relative standard deviation is less than 3.60%, and this shows that the method is highly sensitive, and repeatability and the response rate are good.

Description

Nicotine, 1,2-propylene glycol and the method for glycerol content in a kind of electronic cigarette aerosol of mensuration simultaneously
Technical field
The present invention relates to electronic cigarette product physical and chemical inspection technical field, be specifically related to nicotine, 1,2-PD and the gas chromatography of glycerol content in a kind of electronic cigarette aerosol of mensuration simultaneously.
Background technology
Electronic cigarette (electrical cigarette, e-cigarette) has another name called electronics nicotine transmission system (electronic nicotine Delivery systems, ENDS), be a kind of appearance be similar to Medicated cigarette novel nicotine take in mode.For many years, electronic cigarette is with " health care ", and " smoking cessation ", " lung heat clearing " etc. is slogan, and with network for approach of mainly marketing, in CHINESE REGION, sales volume increases.But, the research for aspects such as electronic cigarette aerosol Major Components is the most little.
Nicotine, 1,2-propylene glycol and glycerol are the main chemical compositions in electronic cigarette cartridge and tobacco juice.1,2-PD and glycerol are the solvents of most tobacco juice for electronic smoke, and major part content is more than 85%, although toxicity is the least, but as the primary solvent of tobacco juice for electronic smoke, it is the most persistently sucked by consumer, and its safety is the most fully proved.Nicotine generally exists in tobacco juice for electronic smoke (cigarette bullet), and content, at 0 ~ 3 mg/mL, is also electronic cigarette manufacturer's sales publicity " replacement smoking " and the principle active component of " helping smoking cessation ".Thus, it is necessary to the nicotine in electronic cigarette aerosol, 1,2-PD and glycerol content are carried out Accurate Determining.
In traditional cigarette and buccal cigarette, 1,2-PD and glycerol add in tobacco shred mainly as humectant, with reach keep moisture in cut tobacco, increase its pliability, reduce make broken, reduce zest and improve the purposes such as jealous, and have relevant criterion and document report[1].There are some researches show, in tobacco juice for electronic smoke (cigarette bullet), main component is 1,2-PD and glycerol, but has no 1,2-PD and the report of glycerol content in mensuration electronic cigarette aerosol[2].Measure the report of nicotine content in Nicotiana tabacum L. and cigarette smoke more[3, 4]But there is a great difference at aspects such as weight, pattern, aerosol (flue gas) mechanism of production, suction mode, chemical composition, content difference between single port suction nicotine content and mouth and mouth in electronic cigarette and traditional cigarette, so, nicotine assay method be not properly suited for electronic cigarette in traditional cigarette main flume[5, 6].Measure the research of nicotine content in electronic cigarette aerosol relatively little, such as Goniewicz, M[7]And Michael, L[8]Etc. utilizing cold hydrazine trapping-gas chromatography to be analyzed tobacco juice for electronic smoke and aerocolloidal nicotine composition, but the operation of cold hydrazine method of trapping is the most loaded down with trivial details, and trapping solution usage amount bigger (100 ML), one is to cause waste of solvent, the trapping solution usage amount that two is bigger is bigger to the diluting effect of nicotine, the electronic cigarette sample that this is low for nicotine content and puff number is relatively low (such as less than 5 mouthfuls) possibly cannot detect, so, urgently develop nicotine, 1,2-PD and the method for glycerol content in a kind of high-throughout aerosol of mensuration simultaneously, with the satisfied requirement analyzing detection.
Summary of the invention
It is contemplated that overcome above technological deficiency, it is provided that nicotine, 1,2-PD and the method for glycerol content in a kind of electronic cigarette aerosol of mensuration simultaneously.It is high that the method has pre-treatment efficiency, the most effectively, it is easy to operation, reproducible, highly sensitive and advantage that the response rate is good.
It is an object of the invention to be achieved through the following technical solutions:
1, the preparation of extract
Concentration range according to target compound, the concentration selecting nicotine internal standard heptadecane is 0.1 ~ 0.5 mg/mL, 1,2-propylene glycol and glycerol internal standard 1, the concentration of 3-butanediol is 0.5 ~ 2 mg/mL: accurately pipette 0.2 g heptadecane and 1 g1,3-butanediol is in 1 L volumetric flask, with isopropanol constant volume.
2, the preparation of standard working solution
Concentration range according to target compound prepares standard working solution, and method is:
1) preparation of nicotine standard working solution: accurately weigh 100 mg nicotine in 100 mL brown volumetric flasks, constant volume is dissolved with isopropanol, prepare nicotine standard stock solution, more accurately measure 0.02,0.05,0.1,0.2,0.5,1.0,2.0 mL Standard Stock solutions are in 10 mL brown volumetric flasks, more accurately add 100 μ L internal standard stock solutions (20 Mg/mL heptadecane is in isopropanol), with isopropanol constant volume, obtain the nicotine standard working solution of 7 grades of Concentraton gradient.
2) 1,2-PD, the preparation of glycerol hybrid standard working solution: the most accurately weigh 500 mg1,2-propylene glycol and 500 mg glycerol, in 100 mL volumetric flasks, dissolve constant volume with isopropanol, prepare 1,2-propylene glycol and glycerol Standard Stock solutions, more accurately measure 0.02,0.05,0.1,0.2,0.5,1.0,2.0 mL hybrid standard stock solutions are in 10 mL brown volumetric flasks, more accurately add 100 μ L internal standard stock solutions (100 Mg/mL1,3-butanediol is in isopropanol), with isopropanol constant volume, obtain the 1,2-PD of 7 grades of Concentraton gradient, glycerol standard working solution.
3, electronic cigarette suction and sample pre-treatments
1) selection of clamper and design:
First with the smoking machine being provided with conversion attachment means, electronic cigarette is aspirated, use ISO:3308, electronic cigarette is aspirated by Canada Health Intense or other suction modes, and with cambridge filter trapping electronic cigarette aerosol in nicotine, 1,2-propylene glycol and glycerol, use extract extracts, and obtains sample solution.
Described conversion attachment means includes an electronic-cigarette holder grafting sealing mechanism and a tobacco rod supporting mechanism, described cigarette holder grafting sealing mechanism is made up of the different two-part transfer tube of caliber and a gum cover, wherein one end pipe external diameter of two-part transfer tube is that 8mm plugs with smoking machine cigarette clamper, other end pipe external diameter is 8 ± n(n=1-10) mm and gum cover grafting, the other end of gum cover is electronic-cigarette holder inserted terminal;Described tobacco rod supporting mechanism is suitable to the collar being sleeved in cigarette clamper and the cantilevered bracing frame being fixed on collar external annulus by one, and is provided with the tobacco rod supporting bracket that can translate, tobacco rod supporting bracket height adjustable along bracing frame cross bar at bracing frame.
Comparing with traditional cigarette, first, electronic cigarette weight is relatively large, and as traditional cigarette weight is usually no more than 1 g, and electronic cigarette weight is typically not less than 10 g, the second filial generation electronic cigarette product weight of topping up can be even up to 50 more than g;Secondly, electronic cigarette nozzle type shape is different, existing traditional column type, also has Duckbill type etc. abnormally-structured, and thickness is different, utilizes traditional cigarette clamper can not meet requirement.So, the above-mentioned conversion attachment means being suitable to be connected with smoking machine should be used could to solve existing methodical deficiency, utilize this conversion attachment means can realize tradition smoking machine to dock with the intact of electronic cigarette, ensure that air-tightness when electronic cigarette aspirates and clamping stability, and then realize the trapping of electronic cigarette aerocolloidal No leakage.
This conversion attachment means has applied for utility model patent the most on the same day.
2) aerosol collection
Use Canada Health Intense suction mode that 6 kinds of electronic cigarette samples are aspirated 50 mouthfuls, be respectively adopted cambridge filter and 2 grades series connection absorption bottle trapping aerosoies in nicotine, 1,2-propylene glycol and glycerol: extract the determinand in cambridge filter with extract, filter disc is followed by 2 grades of series connection absorption bottles, and it is separately added into 20 mL trapping solutions (i.e. extract) trapping determinand, directly utilize chromatographic after suction and measure.Found that: 1. cambridge filter is about 100% to the arresting efficiency of nicotine, and 2 grades of series connection absorption bottles the most do not trap nicotine, as shown in table 1;2. cambridge filter is to the arresting efficiency of 1,2-PD more than 98.5%, and the 1st grade of absorption bottle traps very small amount 1,2-PD, and the 2nd grade of absorption bottle does not trap 1,2-PD, as shown in table 2;3. cambridge filter is about 100% to the arresting efficiency of glycerol, and 2 grades of series connection absorption bottles the most do not trap glycerol, as shown in table 3.
Table 1 cambridge filter and 2 grades of absorption bottles are to nicotine arresting efficiency
Note: N.D. means and does not detects.
Table 2 cambridge filter and 2 grades of absorption bottles are to 1,2-propylene glycol arresting efficiency
Note: N.D. means and does not detects.
Table 3 cambridge filter and 2 grades of absorption bottles are to glycerol arresting efficiency
Note: N.D. means and does not detects.
For the trapping of three kinds of compounds above-mentioned in electronic cigarette aerosol, owing to ISO:3308 or other suction modes simply exist difference, without there is essential distinction in arresting efficiency relative to Canada Health Intense in amount of collected.So, the arresting efficiency higher to nicotine, 1,2-PD and glycerol in electronic cigarette aerosol only just can be reached with cambridge filter.
3) nicotine, 1,2-propylene glycol and the extraction of glycerol in cambridge filter
With cambridge filter trapping electronic cigarette aerosol in nicotine, 1,2-propylene glycol and glycerol, filter disc is taken out, adds 20 mL extracts, use mechanical shaking extraction mode, and investigate the extraction time impact on extracted amount, as shown in Figures 2 and 3, as seen from the figure, nicotine after 30 minutes, 1,2-propylene glycol and glycerol can extract completely, so the selective extraction time is 30 minutes.
4, gas chromatographic analysis
1) GC conditions that nicotine measures is: chromatographic column is HP-50+ type capillary chromatographic column (30 Mm × 0.25, m × 0.32 μm);Detector temperature: 250 DEG C;Injector temperature: 250 DEG C;Carrier gas: nitrogen (purity >=99.999%), constant current flow velocity: 2.0 mL/min;Sample size: 1 μ L, Splitless injecting samples;Hydrogen flowing quantity: 30 mL/min;Air mass flow: 300 mL/min;Make-up gas flow: 29 mL/min;Heating schedule: initial temperature 80 DEG C, keeps 1 min, with the speed of 15 DEG C/min to 260 DEG C, keeps 6 min.
2) GC conditions that 1,2-propylene glycol and glycerol measure is: chromatographic column is Polyethylene Glycol elastic capillary pipe chromatographic column (30 mmid × 0.25, m × 0.25 μm df);Injector temperature: 250 DEG C;Carrier gas: nitrogen (purity >=99.999%), constant current flow velocity: 1.0 mL/min;Sample size: 1 μ L, Splitless injecting samples;Hydrogen flowing quantity: 30 mL/min;Air mass flow: 300 mL/min;Make-up gas flow: 29 mL/min;Heating schedule: initial temperature 90 DEG C, keeps 1 min, with the speed of 15 DEG C/min to 180 DEG C, keeps 5 min, then rises to 240 DEG C with the speed of 25 DEG C/min, keeps 5 min。
5, Specification Curve of Increasing and result calculate
The invention provides and a kind of measure nicotine in electronic cigarette aerosol, 1,2-PD and the gas chromatography of glycerol content simultaneously, there is techniques below advantage:
1. the invention provides nicotine, 1,2-PD and the gas chromatography of glycerol content in a kind of high-throughout electronic cigarette aerosol of mensuration simultaneously, it is achieved that electronic cigarette aerosol quickly measures while above-mentioned three kinds of compounds, has filled up prior art blank.
The most provided by the present invention a kind of using nicotine, 1,2-PD and the method for glycerol content in cambridge filter trapping-gas chromatography determination electronic cigarette aerosol, pre-treatment is simple, and efficiency is high, it is easy to operation.
Method the most provided by the present invention, detection limit (LOD) is 0.40 ~ 2.16 μ g/mL, and the average recovery rate of 3 mark-on levels is between 96.0% ~ 102.0%, and relative standard deviation (RSD) is less than 3.60%, this shows that the method is highly sensitive, and repeatability and the response rate are good.
Table 4 nicotine, 1,2-PD and the standard curve of glycerol, detection limit and the response rate
Accompanying drawing explanation
Fig. 1 is method flow diagram
Fig. 2 is that extraction time is on the impact of nicotine extraction efficiency in cambridge filter
Fig. 3 is that extraction time is on 1,2-propylene glycol in cambridge filter and the impact of glycerol extraction efficiency
Fig. 4 is typical sample chromatogram (nicotine)
Fig. 5 is typical sample chromatogram (1,2-propylene glycol and glycerol)
Fig. 6 is the schematic diagram being applicable on smoking machine aspirate the conversion attachment means of electronic cigarette,
In figure: 1. smoking machine;2. cigarette clamper;3. the collar;4. two-part transfer tube;5. gum cover;6. electronic cigarette;7. tobacco rod supporting bracket, 8. cantilevered bracing frame.
Detailed description of the invention
The present invention is further described by specific examples below, but is not intended to the present invention.
1. instrument, reagent and instrument working condition
1) instrument
SCION 456-GC gas chromatograph, joins flame ionization ditector (GC-FID, Bruker Daltonic company of the U.S.);AE163 electronic balance (sensibility reciprocal: 0.0001 g, Mettler company of Switzerland);Linear type smoking machine (Cerulin company of Britain), HY-8 velocity-modulated oscillator (Changzhou Guohua Electric Appliance Co., Ltd.).
2) reagent
Heptadecane, nicotine, 1,3 butylene glycol, 1,2-PD, glycerol, it is standard substance;Isopropanol (chromatographically pure, TEDIA company of the U.S.).
3) instrument working condition.
1. nicotine measure GC conditions be: chromatographic column be HP-50+ type capillary chromatographic column (30 m × 0.32 mm × 0.25 μm);Detector temperature: 250 DEG C;Injector temperature: 250 DEG C;Carrier gas: nitrogen (purity >=99.999%), constant current flow velocity: 2.0 mL/min;Sample size: 1 μ L, Splitless injecting samples;Hydrogen flowing quantity: 30 mL/min;Air mass flow: 300 mL/min;Make-up gas flow: 29 mL/min;Heating schedule: initial temperature 80 DEG C, keeps 1 min, with the speed of 15 DEG C/min to 260 DEG C, keeps 6 min.
2. the GC conditions that 1,2-propylene glycol and glycerol measure is: chromatographic column is Polyethylene Glycol elastic capillary pipe chromatographic column (30 mmid × 0.25, m × 0.25 μm df);Injector temperature: 250 DEG C;Carrier gas: nitrogen (purity >=99.999%), constant current flow velocity: 1.0 mL/min;Sample size: 1 μ L, Splitless injecting samples;Hydrogen flowing quantity: 30 mL/min;Air mass flow: 300 mL/min;Make-up gas flow: 29 mL/min;Heating schedule: initial temperature 90 DEG C, keeps 1 min, with the speed of 15 DEG C/min to 180 DEG C, keeps 5 min, then rises to 240 DEG C with the speed of 25 DEG C/min, keeps 5 min。
2. the preparation of standard working solution
1) preparation of nicotine standard working solution: accurately weigh 100 mg nicotine in 100 mL brown volumetric flasks, constant volume is dissolved with isopropanol, prepare nicotine standard stock solution, more accurately measure 0.02,0.05,0.1,0.2,0.5,1.0,2.0 mL Standard Stock solutions are in 10 mL brown volumetric flasks, more accurately add 100 μ L internal standard stock solutions (20 Mg/mL heptadecane is in isopropanol), with isopropanol constant volume, obtain the nicotine standard working solution of 7 grades of Concentraton gradient.
2) 1,2-PD and the preparation of glycerol hybrid standard working solution: the most accurately weigh 500 mg1,2-propylene glycol and 500 mg glycerol in 100 mL volumetric flasks, dissolve constant volume with isopropanol, prepare 1,2-PD and glycerol Standard Stock solutions, the most accurately measure 0.02,0.05,0.1,0.2,0.5,1.0,2.0 mL hybrid standard stock solutions are in 10 mL brown volumetric flasks, more accurately add 100 μ L internal standard stock solutions (100 Mg/mL1,3-butanediol is in isopropanol), with isopropanol constant volume, obtain the 1,2-PD of 7 grades of Concentraton gradient, glycerol standard working solution.
3. the determination of standard working curve
Standard working solution is carried out GC-FID mensuration, calculate nicotine in each standard solution, 1,2-propylene glycol and glycerol (are designated as n-heptadecane with internal standard in nicotine, 1,2-PD, is designated as 1 in glycerol, 3-butanediol) peak area ratio, making the standard curve of concentration and peak area ratio or calculate regression equation, standard curve should be linear relationship, coefficient R2Should be not less than 0.995.
4. sample pre-treatments and the determination of testing result
1) sample pre-treatments.Utilization is provided with the smoking machine of conversion attachment means (its structure is as shown in Figure 6) and aspirates electronic cigarette, uses ISO:3308, Canada Health Intense or other suction mode electronic cigarettes aspirate, and trap nicotine, 1,2-PD and the glycerol in electronic cigarette aerosol with cambridge filter, filter disc is taken out, add 20 mL extracts, oscillation extraction 30 min, directly carry out gas chromatographic analysis.
2) sample, each sample replication 2 times are measured according to instrument test condition.After often carrying out 20 sample determinations, the Working Standard Solution of an intermediate concentration should be added, if the value measured and initial value differ by more than 5%, then should re-start the making of whole standard curve.
3) in sample object content with shown in equation below:
Xi = (Ci-C0) ×V
In formula:
XiTarget compound quality in electronic cigarette aerosol, unit is milligram (mg);
CiTarget compound concentration in extract, unit is milligram every milliliter (mg/mL);
C0Target compound concentration in blank experiment extract, unit is milligram every milliliter (mg/mL);
V extract volume, unit is milliliter (mL);
It is final measurement result with the meansigma methods of 2 parallel assays, is accurate to 0.001 mg.
Embodiment 1
According to above-mentioned one measure simultaneously nicotine in electronic cigarette aerosol, 1,2-propylene glycol and the method for glycerol content, select a kind of electronic cigarette product, 50 mouthfuls are aspirated under ISO:3308 suction mode, record nicotine in aerosol, 1,2-propylene glycol and glycerol content are respectively 0.199 mg, 13.682 mg and 5.412 mg.
Embodiment 2
According to nicotine, 1,2-PD and the method for glycerol content in above-mentioned a kind of electronic cigarette aerosol of mensuration simultaneously, select a kind of electronic cigarette product, at Canada Health Aspirate 50 mouthfuls under Intense suction mode, record nicotine in aerosol, 1,2-PD and glycerol content and be respectively 0.305 mg, 19.596 mg and 7.264 mg。
List of references:
[1] Han Shulei;Li Zhonghao;Chen Huan, etc. dispersive solid-phase extraction-GC-MS measures 3 kinds of humectants [J] in cigarette shreds simultaneously. Nicotiana tabacum L. science and technology, 2014, (1): 49-52.
[2] Analysis of components from Gamucci electronic cigarette cartridges, tobacco flavor regular smoking liquid, 2009.
[3] The mensuration gas chromatography [S] of nicotine in GB/T 23,355 2009 Cigarette grain phase.
[4] The mensuration gas chromatography [S] of YC/T 246 2008 Nicotiana tabacum L. and tobacco product nicotine.
[5] Goniewicz, M L; Knysak, J; Gawron, M, et al. Levels of selected carcinogens and toxicants in vapour from electronic cigarettes[J]. Tobacco control, 2013, 0: 1-7.
[6] Cheng, T. Chemical evaluation of electronic cigarettes[J]. Tobacco control, 2014, 23(suppl 2): ii11-ii17.
[7] Goniewicz, M L; Kuma, T; Gawron, M, et al. Nicotine levels in electronic cigarettes[J]. Nicotine & Tobacco Research, 2013, 15(1): 158-166.
[8] Trehy, M L; Ye, W; Hadwiger, M E, et al. Analysis of electronic cigarette cartridges, refill solutions, and smoke for nicotine and nicotine related impurities[J]. Journal of Liquid Chromatography & Related Technologies, 2011, 34(14): 1442-1458。

Claims (4)

1. one kind measures nicotine, 1,2-PD, the method for glycerol content in electronic cigarette aerosol simultaneously, it is characterised in that: the method comprises the following steps:
1) preparation of extract
Preparation is containing internal standard heptadecane and the extract of 1,3 butylene glycol: accurately weighing 0.2 g heptadecane and 1 g1,3-butanediol is in 1 L volumetric flask, with isopropanol constant volume;
2) preparation of standard working solution
Prepare respectively and there is the nicotine of 7 grades of Concentraton gradient, 1,2-PD and glycerol standard working solution, nicotinic density scope: 0.002-0.2 mg/mL;1,2-propylene glycol and glycerol concentration scope: 0.01-1 mg/mL;
3) electronic cigarette suction and sample pre-treatments
Utilize the smoking machine being provided with conversion attachment means that electronic cigarette is aspirated, and with cambridge filter trapping electronic cigarette aerosol in nicotine, 1,2-propylene glycol and glycerol, use extract extracts, obtaining sample solution, the processing method trapping the cambridge filter having determinand is: taken out by filter disc, adds 15 ~ 30 mL extracts, oscillation extraction 30min, directly carries out gas chromatographic analysis;
Described conversion attachment means includes an electronic-cigarette holder grafting sealing mechanism and a tobacco rod supporting mechanism, described cigarette holder grafting sealing mechanism is made up of the different two-part transfer tube of caliber and a gum cover, wherein one end pipe external diameter of two-part transfer tube is that 8mm plugs with smoking machine cigarette clamper, the other end and gum cover grafting, the other end of gum cover is electronic-cigarette holder inserted terminal;Described tobacco rod supporting mechanism is suitable to the collar being sleeved in cigarette clamper and the cantilevered bracing frame being fixed on collar external annulus by one, and is provided with the tobacco rod supporting bracket that can translate, tobacco rod supporting bracket height adjustable along bracing frame cross bar at bracing frame;
4) gas chromatographic analysis
Utilize gas chromatograph to be equipped with flame ionization ditector (FID) made testing sample solution and standard working solution are analyzed, obtain related color spectrogram;
5) Specification Curve of Increasing and result calculate.
Nicotine, 1,2-PD, the method for glycerol content in the electronic cigarette aerosol of mensuration simultaneously the most according to claim 1, it is characterised in that: the preparation method of standard working solution is:
1) preparation of nicotine standard working solution: accurately weigh 100 mg nicotine in 100 mL brown volumetric flasks, dissolves constant volume with isopropanol, prepares nicotine standard stock solution, the most accurately measure 0.02,0.05,0.1,0.2,0.5,1.0,2.0 mL Standard Stock solutions are in 10 mL brown volumetric flasks, more accurately add 100 μ L internal standard stock solutions, with isopropanol constant volume, obtain the nicotine standard working solution of 7 grades of Concentraton gradient;
2) 1, 2-propylene glycol, the preparation of glycerol hybrid standard working solution: the most accurately weigh 500 mg1, 2-propylene glycol and 500 mg glycerol are in 100 mL volumetric flasks, constant volume is dissolved with isopropanol, prepare 1, 2-propylene glycol and glycerol hybrid standard stock solution, the most accurately measure 0.02, 0.05, 0.1, 0.2, 0.5, 1.0, 2.0 mL hybrid standard stock solutions are in 10 mL brown volumetric flasks, the most accurately add 100 μ L internal standard stock solutions again, with isopropanol constant volume, obtain the 1 of 7 grades of Concentraton gradient, 2-propylene glycol, glycerol hybrid standard working solution.
The most according to claim 1 measure simultaneously nicotine in electronic cigarette aerosol, 1,2-propylene glycol, the method for glycerol content, it is characterized in that: the GC conditions that nicotine measures is: chromatographic column is HP-50+ type capillary chromatographic column, mm × 0.25, specification 30 m × 0.32 μm;Detector temperature: 250 DEG C;Injector temperature: 250 DEG C;Carrier gas: nitrogen, purity >=99.999%, constant current flow velocity: 2.0 mL/min;Sample size: 1 μ L, Splitless injecting samples;Hydrogen flowing quantity: 30 mL/min;Air mass flow: 300 mL/min;Make-up gas flow: 29 mL/min;Heating schedule: initial temperature 80 DEG C, keeps 1 min, with the speed of 15 DEG C/min to 260 DEG C, keeps 6 min.
The most according to claim 1 measure simultaneously nicotine in electronic cigarette aerosol, 1,2-propylene glycol, the method for glycerol content, it is characterized in that: 1, the GC conditions that 2-propylene glycol and glycerol measure is: chromatographic column is Polyethylene Glycol elastic capillary pipe chromatographic column, mmid × 0.25, specification 30 m × 0.25 μm df;Injector temperature: 250 DEG C;Carrier gas: nitrogen, purity >=99.999%, constant current flow velocity: 1.0 mL/min;Sample size: 1 μ L, Splitless injecting samples;Hydrogen flowing quantity: 30 mL/min;Air mass flow: 300 mL/min;Make-up gas flow: 29 mL/min;Heating schedule: initial temperature 90 DEG C, keeps 1 min, with the speed of 15 DEG C/min to 180 DEG C, keeps 5 min, then rises to 240 DEG C with the speed of 25 DEG C/min, keep 5 min.
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CN112578069A (en) * 2020-12-29 2021-03-30 广西中烟工业有限责任公司 Analysis method for simultaneously measuring 11 components in electronic smoke sol
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
CN113720934B (en) * 2021-08-20 2023-06-30 中国烟草总公司郑州烟草研究院 Method for detecting aroma components in main stream smoke of cigarettes
CN113720822A (en) * 2021-09-18 2021-11-30 广西中烟工业有限责任公司 Method for detecting nicotine in electronic cigarette by combining magnetic solid phase extraction with carbon dot fluorescent probe

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103698431B (en) * 2013-12-27 2015-09-09 云南烟草科学研究院 The assay method of glycerine, 1,2-PD in a kind of cigarette, electronic cigarette and low temperature cigarette
CN103995066B (en) * 2014-06-06 2016-01-13 山东中烟工业有限责任公司 The method of nicotine burst size in vapor-phase chromatography detected electrons smog
CN104062385B (en) * 2014-07-18 2015-12-02 云南中烟工业有限责任公司 A kind of method of nicotine content in detected electrons cigarette flue gas

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