CN104634914A - Method for determining content of 1,2-propanediol, propanetriol and triethylene glycol in suction aerosol of electronic cigarette - Google Patents
Method for determining content of 1,2-propanediol, propanetriol and triethylene glycol in suction aerosol of electronic cigarette Download PDFInfo
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- CN104634914A CN104634914A CN201510086967.0A CN201510086967A CN104634914A CN 104634914 A CN104634914 A CN 104634914A CN 201510086967 A CN201510086967 A CN 201510086967A CN 104634914 A CN104634914 A CN 104634914A
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- triethylene glycol
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Abstract
The invention provides a method for determining the content of 1,2-propanediol, propanetriol and triethylene glycol in suction aerosol of an electronic cigarette. The method is characterized by comprising the following steps: firstly, sucking the electronic cigarette by using a smoking machine provided with a conversion connection device; capturing 1,2-propanediol, propanetriol and triethylene glycol in the aerosol by using a Cambridge filter; taking an isopropanol solution added with an interior label as an extracting solvent; extracting an object to be detected by using a vibration extraction method; and analyzing by using a gas chromatograph and a hydrogen flame ionization detector; and quantifying with an internal standard method. An experiment result shows that the analysis method has high efficiency and is simple and effective; the linear relation of 1,2-propanediol, propanetriol and triethylene glycol in respective linear ranges is good, the detection limit is 1.01-2.16 micrograms/millimeter, the average recycling rate of three label adding levels is 96.0%-103.6%, and the relative standard deviation is less than 3.60%; and the method has high sensitivity and good repeatability and recovery rate.
Description
Technical field
The present invention relates to electronic cigarette product physical and chemical inspection technical field, being specifically related to a kind of method for measuring 1,2-PD, glycerine and triethylene glycol content in electronic cigarette suction gasoloid.
Background technology
Electronic cigarette (electrical cigarette, e-cigarette) has another name called electronics nicotine transfer system (electronic nicotine delivery systems, ENDS), is the novel nicotine absorption mode that a kind of appearance is similar to cigarette.For many years, electronic cigarette is with " health care ", and " smoking cessation ", " clearing lung-heat " etc. are slogan, and with network for approach of mainly marketing, in CHINESE REGION, sales volume increases.But, also little for the research of the aspects such as electronic cigarette gasoloid Major Components.
1,2-PD, glycerine are the main chemical compositions in electronic cigarette cartridge and tobacco juice.1,2-PD and glycerine are the solvents of most tobacco juice for electronic smoke, and most of content is more than 85%, although toxicity is very little, as the primary solvent of tobacco juice for electronic smoke, consumer continues to suck to it for a long time, and its security is not yet fully proved.Triethylene glycol is the polyvalent alcohol being similar to 1,2-PD and glycerine, is the restricted adjuvant in tobacco and tobacco product, may causes adverse effect, and can cause damage to kidney portion, nervous system etc. to its suction to human body
[1].So, be necessary to carry out Accurate Determining to the 1,2-PD in electronic cigarette gasoloid, glycerine and triethylene glycol content.
In traditional cigarette and buccal cigarette, 1,2-PD and glycerine add in pipe tobacco mainly as humectant, keep moisture in cut tobacco to reach, increase its pliability, reduce make broken, reduce pungency and improve the objects such as jealous, and have relevant criterion and bibliographical information
[2].There are some researches show, in tobacco juice for electronic smoke (cigarette bullet), principal ingredient is 1,2-PD and glycerine, and likely containing triethylene glycol, but have no the report measuring 1,2-PD, glycerine and triethylene glycol content in electronic cigarette gasoloid
[3,4].A great difference is there is in electronic cigarette and traditional cigarette in weight, pattern, gasoloid (flue gas) mechanism of production, suction mode, chemical composition, suction stability etc., so, urgently exploitation is a kind of to be used in electronic cigarette suction and gasoloid thereof 1, the method of 2-propylene glycol, glycerine and triethylene glycol assay, analyzes with satisfied the requirement detected.
Summary of the invention
The present invention is intended to overcome above technological deficiency, provides a kind of method for measuring 1,2-PD, glycerine and triethylene glycol content in electronic cigarette suction gasoloid.It is high that the method has pre-treatment efficiency, simply effectively, is easy to operation, reproducible, highly sensitive and advantage that the recovery is good.
The object of the invention is to be achieved through the following technical solutions:
For measuring a method for 1,2-PD, glycerine and triethylene glycol content in electronic cigarette suction gasoloid, comprise the following steps:
1) preparation of extract
Be interior mark with 1,3-BDO, accurately take in 1 g and be marked in 1 L volumetric flask, with isopropyl alcohol constant volume, make containing interior target extract;
2) preparation of standard working solution
Preparation has 1 of 7 grades of concentration gradients respectively, 2-propylene glycol, glycerine and triethylene glycol hybrid standard working solution, 1,2-PD and glycerol concentration scope: 0.01-1 mg/mL, triethylene glycol concentration range: 0.0025-0.25 mg/mL, its concrete preparation method is as follows:
Accurately take 500 mg1 respectively, 2-propylene glycol, glycerine and 200 mg triethylene glycols are in 100 mL volumetric flasks, constant volume is dissolved with isopropyl alcohol, obtained 1, 2-propylene glycol, glycerine and triethylene glycol Standard Stock solutions, accurately measure 0.02 respectively again, 0.05, 0.1, 0.2, 0.5, 1.0, 2.0 mL hybrid standard stock solutions are in the brown volumetric flask of 10 mL, accurately add mark stock solution in 100 μ L more respectively, with isopropyl alcohol constant volume, obtain 1 of 7 grades of concentration gradients, 2-propylene glycol, glycerine and triethylene glycol hybrid standard working solution, described interior mark stock solution is 100 mg/mL1, 3-butylene glycol is in isopropyl alcohol.
3) electronic cigarette suction and sample pre-treatments
A smoking machine being provided with conversion coupling arrangement is utilized to aspirate electronic cigarette, adopt ISO:3308, Canada Health Intense or other suction modes aspirate electronic cigarette, and with 1 in cambridge filter trap electrons smoke sol, 2-propylene glycol, glycerine and triethylene glycol, use extract extracts, and obtains sample solution.
Described conversion coupling arrangement comprises 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 8mm, plugs with smoking machine cigarette clamper, other end pipe external diameter is 8 ± n(n=1-10) mm, with gum cover grafting, the other end of gum cover is electronic-cigarette holder inserted terminal; The cantilevered bracing frame that described tobacco rod supporting mechanism is suitable for being sleeved on the collar in cigarette clamper by one and is fixed on collar external annulus, and be provided with at bracing frame can along the tobacco rod supporting bracket of bracing frame cross bar translation, tobacco rod supporting bracket height adjustable.
To the disposal route of cambridge filter be: filter disc is taken out, adds 15 ~ 30 mL extracts, oscillation extraction 30min, directly carry out gas chromatographic analysis.
4) gas chromatographic analysis
Utilize gas chromatograph to be equipped with flame ionization ditector (FID) to analyze made testing sample solution and standard working solution, obtain related colour spectrogram; GC conditions is: chromatographic column is polyglycol 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 to 180 DEG C of 15 DEG C/min, keeps 5 min, then rises to 240 DEG C with the speed of 25 DEG C/min, keep 5 min.
5) Specification Curve of Increasing and result calculate.
In electronic cigarette of the present invention suction and sample pre-treatments technique, being described as follows of the preparation of its testing sample solution:
1) clamper is selected
Compare with traditional cigarette, first, electronic cigarette weight is relatively large, be no more than 1 g, and electronic cigarette weight is generally not less than 10 g as traditional cigarette weight, the second generation electronic cigarette product weight of topping up can even reach 50 more than g; Secondly, electronic cigarette nozzle type shape is different, existing traditional column type, also have Duckbill type etc. abnormally-structured, and thickness is different, utilizes traditional cigarette clamper not meet the demands.So, the above-mentioned conversion coupling arrangement being suitable for being connected with smoking machine should be adopted could to solve existing methodical deficiency, utilize this conversion coupling arrangement can realize traditional smoking machine to dock with the intact of electronic cigarette, ensure that impermeability when electronic cigarette aspirates and clamping stability, and then realize the aerocolloidal No leakage trapping of electronic cigarette.
Utility model patent applied on the same day by this conversion coupling arrangement.
2) aerosol collection
Canada Health Intense suction mode is adopted to aspirate 50 mouthfuls to 6 kinds of electronic cigarette samples, adopt 1 in cambridge filter and 2 grades of series connection absorption bottle trapping gasoloids respectively, 2-propylene glycol, glycerine and triethylene glycol: extract the determinand in cambridge filter with extract, 2 grades of series connection absorption bottles are connect after filter disc, and add 20 mL trapping solutions (i.e. extract) respectively and trap determinand, directly utilize chromatographic to measure after suction.Found that: 1. the arresting efficiency of cambridge filter to 1,2-PD is greater than 98.5%, the 1st grade of absorption bottle traps minute quantity 1,2-PD, and the 2nd grade of absorption bottle does not trap 1,2-PD, as shown in table 1; 2. the arresting efficiency of cambridge filter to glycerine is about 100%, and 2 grades of series connection absorption bottles all do not trap glycerine, as shown in table 2; 3. the recall rate of electronic cigarette gasoloid to triethylene glycol is lower, detects in sample in an example, and the arresting efficiency of cambridge filter to triethylene glycol is about 100%, and 2 grades of series connection absorption bottles all do not trap triethylene glycol, as shown in table 3;
Table 1 cambridge filter and 2 grades of absorption bottles are to 1,2-PD arresting efficiency
Note: N.D. means and does not detect.
Table 2 cambridge filter and 2 grades of absorption bottles are to glycerine arresting efficiency
Note: N.D. means and does not detect.
Table 3 cambridge filter and 2 grades of absorption bottles are to triethylene glycol arresting efficiency
Note: N.D. means and does not detect.
For the trapping of three kinds of compounds above-mentioned in electronic cigarette gasoloid, because ISO:3308 or other suction modes just exist difference relative to Canada Health Intense in amount of collected, and essential distinction can not be there is in arresting efficiency.So, only just can reach the arresting efficiency higher to 1,2-PD, glycerine and triethylene glycol in electronic cigarette gasoloid with cambridge filter.
3) extraction of 1,2-PD, glycerine and triethylene glycol in cambridge filter
With 1 in cambridge filter trap electrons smoke sol, 2-propylene glycol, glycerine and triethylene glycol, filter disc is taken out, adds 20 mL extracts, adopt mechanical shaking extraction mode, and investigate the impact of extraction time on extracted amount, as shown in Figure 2, as seen from the figure, after 30 minutes 1,2-propylene glycol, glycerine and triethylene glycol can extract completely, so the selective extraction time is 30 minutes.
To the invention provides in a kind of gas chromatography determination electronic cigarette gasoloid 1, the method of 2-propylene glycol, glycerine and triethylene glycol content, achieve the Rapid Simultaneous Determination of above-mentioned three kinds of compounds in electronic cigarette gasoloid, fill up prior art blank, pre-treatment of the present invention is simple, efficiency is high, be easy to operation, detection limit (LOD) is 1.01 ~ 2.16 μ g/mL, the average recovery rate of 3 mark-on levels is between 96.0% ~ 103.6%, relative standard deviation (RSD) is less than 3.60%, and this shows that the method is highly sensitive, repeatability and the recovery good.
The typical curve of table 4 1,2-PD, glycerine and triethylene glycol, detectability and the recovery
Accompanying drawing explanation
fig. 1for method flow diagram.
fig. 2for extraction time is on the impact of 1,2-PD, glycerine and triethylene glycol extraction efficiency in cambridge filter.
fig. 3for typical sample chromatogram.
Fig. 4 is the schematic diagram of the conversion coupling arrangement being applicable to smoking machine aspirates 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.
Embodiment
The present invention is further described by following specific embodiment, but does not limit the present invention.
1. instrument, reagent and instrument condition of work
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 pattern smoking machine (Cerulin company of Britain), HY-8 velocity-modulated oscillator (Changzhou Guohua Electric Appliance Co., Ltd.).
2) reagent
Heptadecane, 1,3-BDO, 1,2-PD, glycerine, triethylene glycol, is standard items; Isopropyl alcohol (chromatographically pure, TEDIA company of the U.S.).
3) instrument condition of work.
Chromatographic column is polyglycol 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 to 180 DEG C of 15 DEG C/min, keeps 5 min, then rises to 240 DEG C with the speed of 25 DEG C/min, keep 5 min.
2. the preparation of standard working solution: prepare by method noted earlier.
3. the determination of standard working curve
GC-FID mensuration is carried out to standard working solution, to calculate in each standard solution 1,2-propylene glycol, glycerine and triethylene glycol and interior mark (1,3-butylene glycol) peak area ratio, make the typical curve of concentration and peak area ratio or calculate regression equation, typical curve should be linear relationship, coefficient R
2should 0.995 be not less than.
4. electronic cigarette suction, the determination of sample pre-treatments and testing result
1) electronic cigarette suction and sample pre-treatments.The smoking machine that utilization is provided with conversion coupling arrangement (its structure as shown in Figure 4) aspirates electronic cigarette, adopt ISO:3308, Canada Health Intense or other suction modes aspirate electronic cigarette, and with 1 in cambridge filter trap electrons smoke sol, 2-propylene glycol, glycerine and triethylene glycol, take out filter disc, add 20 mL extracts, oscillation extraction 30 min, directly carries out gas chromatographic analysis.
2) according to instrument test condition working sample, each sample replication 2 times.
3) in sample object content with shown in following formula:
X
i= (C
i－C
0) ×V
In formula:
X
i---target compound quality in electronic cigarette gasoloid, unit is milligram (mg);
C
i---target compound concentration in extract, unit is milligram every milliliter (mg/mL);
C
0---target compound concentration in blank assay extract, unit is milligram every milliliter (mg/mL);
V---extract volume, unit is milliliter (mL);
Be final measurement result with the mean value of 2 replicate determinations, be accurate to 0.001 mg.
Embodiment 1
According to the method described above, select a kind of electronic cigarette product, under ISO:3308 suction mode, aspirate 50 mouthfuls, record 1,2-PD in gasoloid, glycerine and triethylene glycol content and be respectively 13.682 mg, 5.412 mg and 0.512 mg.
Embodiment 2
According to the method described above, select a kind of electronic cigarette product, under Canada Health Intense suction mode, aspirate 50 mouthfuls, record 1,2-PD in gasoloid, glycerine and triethylene glycol content and be respectively 19.596 mg, 7.264 mg and 0.315 mg.
list of references:
[1] Material Safety Data Sheet Triethylene glycol MSDS http://www.sciencelab.com/msds.php?msdsId=9927307.
[2] Han Shulei; Li Zhonghao; Chen Huan, etc. 3 kinds of humectants [J] in dispersive solid-phase extraction-GC-MS(gas chromatography-mass spectrography) Simultaneously test cigarette shreds. tobacco science and technology, 2014, (1): 49-52.
[3] Analysis of components from Gamucci electronic cigarette cartridges, tobacco flavor regular smoking liquid, 2009.
[4] Etter, J F; Z?ther, E; Svensson, S. Analysis of refill liquids for electronic cigarettes[J]. Addiction, 2013, 108: 1671-1679.。
Claims (5)
1., for measuring a method for 1,2-PD, glycerine and triethylene glycol content in electronic cigarette suction gasoloid, it is characterized in that: the method comprises the following steps:
1) preparation of extract
Be interior mark with 1,3-BDO, accurately take in 1 g and be marked in 1 L volumetric flask, with isopropyl alcohol constant volume, make containing interior target extract;
2) preparation of standard working solution
Prepare 1,2-PD, glycerine and the triethylene glycol hybrid standard working solution with 7 grades of concentration gradients respectively, 1,2-PD and glycerol concentration scope: 0.01-1 mg/mL, triethylene glycol concentration range: 0.0025-0.25 mg/mL;
3) electronic cigarette suction and sample pre-treatments
A smoking machine being provided with conversion coupling arrangement is utilized to aspirate electronic cigarette, ISO:3308 or Canada Health Intense is adopted to aspirate electronic cigarette, and with 1 in cambridge filter trap electrons smoke sol, 2-propylene glycol, glycerine and triethylene glycol, use extract extracts, and obtains sample solution;
4) gas chromatographic analysis
Utilize gas chromatograph to be equipped with flame ionization ditector (FID) to analyze made testing sample solution and standard working solution, obtain related colour spectrogram;
5) Specification Curve of Increasing and result calculate.
2. the method for measuring 1,2-PD, glycerine and triethylene glycol content in electronic cigarette suction gasoloid according to claim 1, it is characterized in that: described 1,2-PD, the preparation method of glycerine and triethylene glycol hybrid standard working solution is:
Accurately take 500 mg1 respectively, 2-propylene glycol, glycerine and 200 mg triethylene glycols are in 100 mL volumetric flasks, constant volume is dissolved with isopropyl alcohol, obtained 1, 2-propylene glycol, glycerine and triethylene glycol Standard Stock solutions, accurately measure 0.02 respectively again, 0.05, 0.1, 0.2, 0.5, 1.0, 2.0 mL hybrid standard stock solutions are in the brown volumetric flask of 10 mL, accurately add mark stock solution in 100 μ L more respectively, with isopropyl alcohol constant volume, obtain 1 of 7 grades of concentration gradients, 2-propylene glycol, glycerine and triethylene glycol hybrid standard working solution, described interior mark stock solution is 100 mg/mL1, 3-butylene glycol is in isopropyl alcohol.
3. according to claim 1 for measure electronic cigarette suction gasoloid in 1, the method of 2-propylene glycol, glycerine and triethylene glycol content, it is characterized in that: to the disposal route of cambridge filter be: filter disc is taken out, add 15 ~ 30 mL extracts, oscillation extraction 30min, directly carries out gas chromatographic analysis.
4. according to claim 1 for measure electronic cigarette suction gasoloid in 1, the method of 2-propylene glycol, glycerine and triethylene glycol content, it is characterized in that: the GC conditions measured for 1,2-PD, glycerine and triethylene glycol is: chromatographic column is polyglycol 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 to 180 DEG C of 15 DEG C/min, keeps 5 min, then rises to 240 DEG C with the speed of 25 DEG C/min, keep 5 min.
5. according to claim 1 for measure electronic cigarette suction gasoloid in 1, 2-propylene glycol, the method of glycerine and triethylene glycol content, it is characterized in that: described conversion coupling arrangement comprises 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 8mm, plug with smoking machine cigarette clamper, other end pipe external diameter is 8 ± n(n=1-10) mm, with gum cover grafting, the other end of gum cover is electronic-cigarette holder inserted terminal, the cantilevered bracing frame that described tobacco rod supporting mechanism is suitable for being sleeved on the collar in cigarette clamper by one and is fixed on collar external annulus, and be provided with at bracing frame can along the tobacco rod supporting bracket of bracing frame cross bar translation, tobacco rod supporting bracket height adjustable.
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| CN108303477A (en) * | 2018-01-04 | 2018-07-20 | 国家烟草质量监督检验中心 | A kind of heating do not burn cigarette main flume in the compounds such as alcohols detection method |
| CN113655154A (en) * | 2020-05-12 | 2021-11-16 | 国家烟草质量监督检验中心 | In-situ extraction instrument suitable for measuring moisture in flue gas and test method |
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