CN103808849B - Method for measuring content of menthol in electronic cigarette liquid - Google Patents

Method for measuring content of menthol in electronic cigarette liquid Download PDF

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Publication number
CN103808849B
CN103808849B CN201410094935.0A CN201410094935A CN103808849B CN 103808849 B CN103808849 B CN 103808849B CN 201410094935 A CN201410094935 A CN 201410094935A CN 103808849 B CN103808849 B CN 103808849B
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China
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menthol
solution
tobacco juice
standard
standard working
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CN201410094935.0A
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Chinese (zh)
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CN103808849A (en
Inventor
韩书磊
陈欢
刘彤
吴帅宾
侯宏卫
胡清源
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国家烟草质量监督检验中心
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Abstract

The invention relates to a method for measuring the content of menthol in electronic cigarette liquid. The method is characterized by comprising the steps of preparing a sample solution to be measured by an ultrasonic extracting method, configuring a standard working solution with six concentration gradients, performing analysis by a gas chromatograph matched with hydrogen flame ionized detector, and measuring the content of menthol by an internal standard method. The result shows that when the content of menthol is 0.001mg/mL to 0.1mg/mL, the linear relation is good, the limit of detection (LOD) is 0.0028 percent, the average recover rate of three scaled levels is 100.9 percent, and the average relative standard deviation (RSD) is 1.38 percent. The method is high in sensitivity and good in repeatability and recovery rate.

Description

The assay method of menthol content in a kind of tobacco juice for electronic smoke
Technical field
The present invention relates to electronic cigarette product physical and chemical inspection technical field, be specifically related to the assay method of menthol content in a kind of tobacco juice for electronic smoke.
Background technology
In recent years, smoking gets more and more people's extensive concerning with healthy topic always, and Smoking is harmful to your health has been subject to people and generally approves.2005, China's signature " Framework Convention on Tobacco Control ", made Tobacco Control have legal basis, 2012, and Chinese Government issues " Chinese tobacco controlling planning (2012-2015) ", proposed to create smokeless environment, implemented public place and banned on opium-smoking and the opium trade comprehensively.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 for the composition measurement of electronic cigarette product, the research of the aspects such as safety evaluation is also little.
Menthol is because of its special strong peppermint fragrance and nice and cool taste, be widely used in the industries such as personal-care supplies, food and medicine, have antipruritic, pain relieving and refrigerant effect, it is one of widely used fragrance type in the world, and be used widely in electronic cigarette product, the mouthfeel of electronic cigarette can be improved.But research shows, in traditional cigarette, menthol may strengthen the dependence of consumer to cigarette, and improve the incidence of disease of lung cancer, and have certain correlativity with relative risk, increase harm of smoking (Brooks, Daniel R, etc. Menthol cigarettes and risk of lung cancer. am J Epidemiol, 158, 609-616.2003; Clark, Pamela I, etc. Effect of menthol cigarettes on biochemical markers of smoke exposure among black and white smokers. cHEST Journal, 110, 1194-1198.1996.).But the contents level and safety evaluation etc. of menthol in tobacco juice for electronic smoke, still do not have pertinent literature to report.Therefore the assay method setting up the menthol content in tobacco juice for electronic smoke is necessary.
Summary of the invention
Object of the present invention provides the assay method of menthol content in a kind of tobacco juice for electronic smoke just based on above-mentioned prior art situation, the detection method that this method provides, has pre-treatment simply effective, quantitatively accurately, reproducible, highly sensitive and advantage that the recovery is good.
The object of the invention is to be achieved through the following technical solutions:
An assay method for menthol content in tobacco juice for electronic smoke, comprises the following steps:
1) preparation of testing sample solution: take 50 ~ 150 mg tobacco juice for electronic smoke in 5 mL volumetric flasks, accurately add mark in 100 μ L, add 0.5 ~ 4 mL methyl alcohol again, then be placed on ultrasonic cleaner with power ultrasonic 5 ~ 10 min of 80 W, after being cooled to room temperature, with methanol constant volume, (anhydrous magnesium sulfate will in muffle furnace after 600 DEG C of drying 5 h to add about 200 mg anhydrous magnesium sulfates absorption moisture again, be stored in exsiccator for subsequent use), vibrate after 0.5 min with hand, leave standstill, after clarification, get supernatant through 0.22 μm of organic phase membrane filtration, be testing sample solution,
2) preparation of standard working solution
Preparation has the methanol solution of the menthol of 6 grades of concentration gradients as standard working solution;
3) gas chromatographic analysis
Utilize gas chromatograph to be equipped with flame ionization ditector (FID) and with standard working solution, detection is separated to above-mentioned made testing sample solution, obtain related colour spectrogram;
4) Specification Curve of Increasing and result calculate.
Be designated as 1,3-BDO in described, dissolving with methyl alcohol is the inner mark solution that concentration is 0.05 mg/mL.
The menthol standard working solution of 6 grades of concentration gradients of preparation is specially: 0.001,0.002,0.005,0.02,0.05,0.1 mg/ mL.
The preparation method of standard working solution is:
First preparation standard stock solution: accurately take 100 mg menthols in 100 mL volumetric flasks, dissolves constant volume with methyl alcohol; Then accurately measure 0.01 respectively, 0.02,0.05,0.2,0.5,1.0 mL Standard Stock solutions in 10 mL volumetric flasks, more accurately add 100 μ L inner mark solutions, respectively with methanol constant volume.
GC conditions is: chromatographic column: 30 mmid × 0.25, m × 0.25 μm df polyglycol elastic capillary pipe chromatographic column; Injector temperature: 250 DEG C; Carrier gas: nitrogen, constant current flow velocity: 1.0 mL/min; Sample size: 1 μ L, Splitless injecting samples; Heating schedule: initial temperature 90 DEG C, keeps 1 min, with the speed to 180 DEG C of 15 DEG C/min, keeps 1 min, then rises to 240 DEG C with the speed of 50 DEG C/min, keeps 10 minutes.
The invention provides the assay method of menthol content in a kind of tobacco juice for electronic smoke, there is following technical advantage:
1. the present invention provides gas chromatography-flame ionization ditector (GC-FID) assay method of menthol content in a kind of tobacco juice for electronic smoke first, achieves the Fast Measurement of menthol content in tobacco juice for electronic smoke.
2. in gas chromatographic analysis, relative to external standard method, because the relative value of the peak area by measuring internal standard compound and tested component calculates, so, internal standard method effectively can eliminate the error that the operating conditionss such as sample size are brought, and the result of mensuration is more accurate, but, in internal standard method, suitable internal standard compound is selected to be crucial.Compare 1,3-BDO, 1, the effect of 4-butylene glycol and heptadecane three kinds of conventional internal standard compounds, found that, BDO and heptadecane have impurity to disturb in tobacco juice, not easily as internal standard compound, 1,3-BDO does not then disturb substantially, and good with other 5 kinds of compound separation, therefore selected 1,3-BDO is as internal standard compound.
3. menthol is hydroxyl polar compound, and selection polarity capillary column effect can be relatively good, and this patent selects the polyglycol elastic capillary pipe chromatographic column DB-WAX chromatographic column with strong polarity, and peak type is sharp-pointed, good separation.
4. method provided by the present invention, pre-treatment is simple, do not need purification, easy and simple to handle, fast, detection limit (LOD) is 0.0028%, typical curve related coefficient is greater than 0.9999, and the average recovery rate of 3 mark-on levels is 100.9%, and average relative standard's deviation (RSD) is 1.38%, this shows that the method is highly sensitive, repeatability and the recovery good.
Accompanying drawing explanation
Fig. 1 is standard working solution chromatogram.
Fig. 2 is typical sample chromatogram.
Embodiment
The present invention is further described by following specific embodiment, but does not limit the present invention.
Embodiment 1:
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); Ultrasonic generator (KQ-700DB type numerical control ultrasonic cleaner).
2) reagent
1,3-BDO (interior mark, CAS:107-88-0), menthol (CAS:89-78-1), is standard items; Methyl alcohol (chromatographically pure, TEDIA company of the U.S.).
3) GC conditions.Chromatographic column: 30 mmid × 0.25, m × 0.25 μm df polyglycol elastic capillary pipe chromatographic column (DB-WAX chromatographic column or other equivalent posts); 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; Heating schedule: initial temperature 90 DEG C, keeps 1 min, with the speed to 180 DEG C of 15 DEG C/min, keeps 1 min, then rises to 240 DEG C with the speed of 50 DEG C/min, keeps 10 minutes.
2. the preparation of standard working solution
1) preparation (5 mg/mL) of mark stock solution in.Accurately pipette about 0.5 g1,3-butylene glycol, in 100 mL volumetric flasks, dissolves constant volume with methyl alcohol, obtains the interior mark stock solution that concentration is 5 mg/mL.
2) preparation (0.001-0.1 mg/mL) of standard working solution.1) preparation (1.0 mg/mL) of Standard Stock solutions: accurately take 100 mg menthols in 100 mL volumetric flasks, dissolves constant volume with methyl alcohol; 2) preparation of standard working solution: accurately measure 0.01 respectively, 0.02,0.05,0.2,0.5,1.0 mL Standard Stock solutions in 10 mL volumetric flasks, more accurately add mark stock solution in 100 μ L, respectively with methanol constant volume.
3. the determination of standard working curve
Carry out GC-FID mensuration to standard working solution, calculate menthol and interior target peak area ratio in each standard solution, make the typical curve of concentration and peak area ratio or calculate regression equation, typical curve should be linear relationship, coefficient R 2should 0.999 be not less than.
4. the determination of sample pre-treatments and testing result
1) sample pre-treatments: accurately take about 100 mg tobacco juice for electronic smoke in 5 mL volumetric flasks, accurately add mark stock solution in 100 μ L, then add about 4 mL methyl alcohol, be then placed on ultrasonic cleaner with power ultrasonic 5 min of 80 W, after being cooled to room temperature, with methanol constant volume.Add about 200 mg anhydrous magnesium sulfates again and absorb moisture (in muffle furnace after 600 DEG C of drying 5 h, being stored in exsiccator for subsequent use), after hand vibration 0.5 min, leave standstill, after clarification, get supernatant through 0.22 μm of organic phase membrane filtration.
2) according to instrument test condition working sample, each sample replication 2 times.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 typical curve.
3) in sample object content with shown in following formula:
In formula:
X i---target compound concentration in tobacco juice for electronic smoke, unit is mass percent (%);
C i---target compound concentration in extract, unit is milligram every milliliter (mg/mL);
C 0---target compound concentration in blank assay, unit is milligram every milliliter (mg/mL);
V---extract constant volume, unit is milliliter (mL);
M---tobacco juice for electronic smoke quality, unit is milligram (mg).
Be final measurement result with the mean value of 2 replicate determinations, be accurate to 0.01%, its relative average debiation of horizontal survey result should be less than 10%.
According to said determination method, select a kind of tobacco juice for electronic smoke A, the content recording wherein menthol is 1.15%.
Embodiment 2
According to said determination method, select a kind of tobacco juice for electronic smoke B, the content recording wherein menthol is 0.11%.
Embodiment 3
According to said determination method, select a kind of tobacco juice for electronic smoke C, record wherein menthol and do not detect.
Embodiment 4
According to assay method, select a kind of tobacco juice for electronic smoke D, record wherein menthol and do not detect.

Claims (3)

1. the assay method of menthol content in tobacco juice for electronic smoke, it is characterized in that, the method comprises the following steps:
1) preparation of testing sample solution: take 50 ~ 150 mg tobacco juice for electronic smoke in 5 mL volumetric flasks, accurately add mark in 100 μ L, then add 0.5 ~ 4 mL methyl alcohol, be then placed on ultrasonic cleaner with power ultrasonic 5 ~ 10 min of 80 W, after being cooled to room temperature, with methanol constant volume, then add about 200 mg anhydrous magnesium sulfates absorption moisture, after hand vibration 0.5 min, leave standstill, after clarification, get supernatant through 0.22 μm of organic phase membrane filtration, be testing sample solution; Be designated as 1,3-BDO in described, dissolving with methyl alcohol is the inner mark solution that concentration is 0.075 mg/mL;
2) preparation of standard working solution
Preparation has the methanol solution of the menthol of 6 grades of concentration gradients as standard working solution;
3) gas chromatographic analysis
Utilize gas chromatograph to be equipped with flame ionization ditector (FID) and with standard working solution, detection is separated to above-mentioned made testing sample solution, obtain related colour spectrogram; GC conditions is: chromatographic column: 30 mmid × 0.25, m × 0.25 μm df polyglycol elastic capillary pipe chromatographic column; Injector temperature: 250 DEG C; Carrier gas: nitrogen, constant current flow velocity: 1.0 mL/min; Sample size: 1 μ L, Splitless injecting samples; Heating schedule: initial temperature 90 DEG C, keeps 1 min, with the speed to 180 DEG C of 15 DEG C/min, keeps 1 min, then rises to 240 DEG C with the speed of 50 DEG C/min, keeps 10 minutes;
4) Specification Curve of Increasing and result calculate.
2. the assay method of menthol content in tobacco juice for electronic smoke according to claim 1, it is characterized in that, the menthol standard working solution of 6 grades of concentration gradients of preparation is specially: 0.001,0.002,0.005,0.02,0.05,0.1 mg/ mL.
3. the assay method of menthol content in tobacco juice for electronic smoke according to claim 1, it is characterized in that, the preparation method of standard working solution is: first preparation standard stock solution: accurately take 100 mg menthols in 100 mL volumetric flasks, dissolves constant volume with methyl alcohol; Then accurately measure 0.01 respectively, 0.02,0.05,0.2,0.5,1.0 mL Standard Stock solutions in 10 mL volumetric flasks, more accurately add 100 μ L inner mark solutions, respectively with methanol constant volume.
?
CN201410094935.0A 2014-03-16 2014-03-16 Method for measuring content of menthol in electronic cigarette liquid CN103808849B (en)

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CN104068470A (en) * 2014-07-07 2014-10-01 嘉兴市得百科新材料科技有限公司 Electronic cigarette liquid solvent and preparation method for same
CN104122358B (en) * 2014-07-26 2015-10-28 云南中烟工业有限责任公司 A kind of assay method of electronic cigarette aroma volatile
CN104256885B (en) * 2014-08-05 2015-12-30 云南中烟工业有限责任公司 A kind of tobacco juice for electronic smoke solvent
CN104237428B (en) * 2014-08-26 2015-12-30 上海烟草集团有限责任公司 The assay method of menthol in a kind of smoke-free tobacco product
CN104489900A (en) * 2014-11-26 2015-04-08 浙江中烟工业有限责任公司 Mint-flavored nicotine liquid and electronic cigarette with same
CN104634914A (en) * 2015-02-16 2015-05-20 国家烟草质量监督检验中心 Method for determining content of 1,2-propanediol, propanetriol and triethylene glycol in suction aerosol of electronic cigarette

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CN101315353B (en) * 2008-07-11 2011-07-20 江苏中烟工业公司 Method for detecting perfuming homogeneity of cigarette production based on marker
CN102353736B (en) * 2011-07-14 2013-05-15 浙江中烟工业有限责任公司 Method for determining menthol in cigarette filter rod
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