CN104062385A - Method for detecting content of nicotine in smoke of electronic cigarette - Google Patents
Method for detecting content of nicotine in smoke of electronic cigarette Download PDFInfo
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- CN104062385A CN104062385A CN201410341580.0A CN201410341580A CN104062385A CN 104062385 A CN104062385 A CN 104062385A CN 201410341580 A CN201410341580 A CN 201410341580A CN 104062385 A CN104062385 A CN 104062385A
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Abstract
The invention discloses a method for detecting the content of nicotine in smoke of an electronic cigarette. The detection method comprises the following steps: (1) preparing an extracting agent; (2) preparing a standard series solution of the nicotine; (3) connecting a Cambridge filter and an absorption bottle with a smoking machine in series and capturing the smoke of the electronic cigarette; putting the Cambridge filter for capturing the smoke and absorption liquid into a tapered bottle and carrying out vibration extraction; (4) moving away an extracting liquid filtering membrane and analyzing filter liquid by using a gas chromatographic method; and (5) drawing a standard curve and calculating the content of the nicotine in the smoke of the electronic cigarette. The method disclosed by the invention has the advantages of high sensitivity, good selectivity, simplicity in operation and high repeatability, and can realize the accurate quantitative analysis of the nicotine in the electronic cigarette.
Description
Technical field
The present invention relates to the physical and chemical inspection technical field of electronic cigarette product flue gas, be specifically related to the method for nicotine content in a kind of detected electrons cigarette flue gas.
Background technology
Along with the sternness increasingly of global Tobacco Control environment and consumer are to healthy growing interest, break through traditional cigarette technology, researching and developing a kind of electronic cigarette that reduces all sidedly, significantly tobacco objectionable constituent burst size becomes the important means that countries in the world tobacco business solves tobacco business future development gradually.Electronic cigarette, has another name called electronics nicotine transfer system (electronic nicotine delivery systems, ENDS).To the official definition of electronics nicotine transfer system, (WHO technical report series 955 is P4-5): electronic cigarette nicotine transfer system (ENDS) is a kind of consumer products to transmit nicotine to lung in the World Health Organization (WHO).
People become to assign to meet physiology impression, psychological response demand by sucking nicotine in electronic cigarette, in flue gas, nicotine can be addicting and produce dependence, nicotine is sucked and can be produced many effects: as vessel retraction, palpitating speed, increased blood pressure, breathing accelerate, mental status changes (being emotionally stable or mental excitation as become), and promote platelet aggregation, for causing the main accomplice of the cardiovascular diseases such as cardiovascular obstruction, hypertension, apoplexy.
Bibliographical information mostly is the nicotine content in electronic cigarette tobacco tar at present, less to the research of nicotine content in electronic cigarette flue gas.Goniewicz, Maciej L etc. utilizes vapor-phase chromatography-thermionic detector to carry out analyzing (Nicotine & Tobacco Research to the nicotine composition in electronic cigarette tobacco tar and flue gas, 15,158-166. 2013.), but these researchs just provide measurement result with the form of laboratory report, method are not described in detail and are verified.
summary of the invention:
The Gas Chromatographic Method of nicotine content in a kind of electronic cigarette flue gas that the present invention provides based on the problems referred to above just.The detection method that this method provides, have simple to operate, quantitatively accurate, reproducible, highly sensitive and advantage that the recovery is good.
The present invention is achieved through the following technical solutions:
Described detection method comprises the following steps:
1) configuration of extractant: pipette a certain amount of n-heptadecane and dilute in aqueous isopropanol, shake up as extractant, the concentration range after n-heptadecane dilutes in aqueous isopropanol is 0.1mg/mL ~ 0.5mg/mL;
2) standard serial solution of configuration nicotine: nicotine (standard substance) is dissolved in aqueous isopropanol, prepares 6 series standard solution, the nicotinic density detecting in its concentration range overlay electronic cigarette sample, drawing standard curve;
3), after adopting cambridge filter and absorption bottle to connect with smoking machine, trapping electronic cigarette flue gas, puts into conical flask by cambridge filter and the absorption liquid of trapping flue gas, carries out oscillation extraction;
4) pipette extract filtering membrane, filtrate adopts vapor-phase chromatography to analyze it;
5) according to typical curve, calculate the content of nicotine in electronic cigarette flue gas.
Step 2) its concentration range of nicotinic density detecting in the electronic cigarette sample described in is 0.01 mg/mL ~ 3.0 mg/mL.
Step 2) the nicotine standard substance described in is nicotine or the nicotine salicylate salt of known purity, and preservation condition is 0 ℃ ~ 4 ℃.
The suction scheme of collecting the employing of electronic cigarette flue gas described in step 3) is determined by the power of electronic smoke atomizer and the parameters such as power of battery, provides the scope of some suction parameters below: suction capacity is 35 ~ 55 mL; The suction duration is 2 ± 0.05s; Suction frequency is 30 ± 0.5s, 60 ± 0.5s; Suction curve is triangular wave, square wave and bell; Puff number scope is 50 ~ 200 mouthfuls.
The smoking machine that traps the employing of electronic cigarette flue gas described in step 3) is linear pattern smoking machine, and cambridge filter diameter is 44mm, and smoking room is constant-temperature constant-humidity environment.For special-shaped and electronic cigarette, the trapping of flue gas need to connect and turns and bracket.Collected cambridge filter and the extract of flue gas and put into conical flask, the volume of extractant can make the appropriate adjustments according to the scope of typical curve nicotinic density.
Gas chromatograph described in step 4) is detecting device, registering instrument and the integraph of being furnished with flame ion, and the chromatographic column of employing is the gas chromatographic column of the methyl polysiloxane filler containing phenyl.
Instrument condition in vapor-phase chromatography described in step 4): post case temperature: 170 ℃; Injector temperature is 250 ℃; Detector temperature: 250 ℃; Carrier gas: helium or nitrogen, flow 30 mL/min; Sampling volume 2 μ L; Analysis time: 6 ~ 8 min.
The cubage of nicotine in the flue gas of electronic cigarette described in step 5), by the typical curve of making, calculate nicotinic density, the content of nicotine in nicotinic density calculating electronic cigarette flue gas, divided by the mouth number of suction, result represents with the milligram number of every mouthful of electronic cigarette, is accurate to 0.0001mg.
The method that the invention provides nicotine content in a kind of detected electrons cigarette flue gas, has following advantage:
1. the present invention provides gas chromatography-flame ionization ditector (GC-FID) assay method of nicotine content in a kind of electronic cigarette flue gas first, has realized the Fast Measurement of nicotine content in electronic cigarette flue gas.
2. in gas chromatographic analysis, employing be inner mark method ration, with respect to external standard method, can effectively eliminate operate miss, measure accurately the content of nicotine.N-heptadecane is noiseless to other components in electronic cigarette flue gas as interior mark.
3. adopt filter disc+absorption bottle by the nicotine trapping in electronic cigarette flue gas completely, to guarantee the accurate of measurement result.Compared filter disc, filter disc+absorption bottle, absorption bottle arresting efficiency, found that the efficiency of filter disc+absorption bottle trapping is more than 99%, in absorption bottle trapping, absorption liquid can not absorb flue gas well, causes measurement result incomplete.Therefore select the nicotine in filter disc trapping electronic cigarette flue gas.
4. adopt the isopropyl alcohol that contains n-heptadecane as extractant, can guarantee nicotine extraction completely.Compared methyl alcohol, isopropyl alcohol, ethyl acetate, normal hexane, methylene chloride and the sherwood oil effect of extracting to nicotine as extractant respectively, found that the extraction efficiency of isopropyl alcohol is the highest, therefore select the isopropyl alcohol that contains n-heptadecane as extractant.
5. method provided by the present invention, pre-treatment is simple, do not need purification enrichment, simple to operate, quick, detection limit (LOD) is 0.0064mg/ mouth, and the related coefficient of typical curve is greater than 0.9999, the average recovery rate of three mark-on levels is between 93.5 ~ 102.4%, relative standard deviation (RSD) is less than 5%, this show the sensitivity of method and the recovery high, repeatability is better.
Accompanying drawing explanation
Fig. 1 is the standard operation solution chromatogram of nicotine and interior mark n-heptadecane.
Embodiment
The present invention is further described by following specific embodiment, but is not limited to embodiment.
Embodiment 1:
Instrument, reagent and instrument condition of work:
1) instrument
Agilent 6890N gas chromatograph, joins flame ionization ditector; SM450 type 20 duct linear pattern smoking machines (Britain CERULEAN company); HY-8 type shaker (Changzhou Guohua Electric Appliance Co., Ltd.); ME414S electronic balance (sensibility reciprocal: 0.0001g, German Sartorius company)
2) reagent
N-heptadecane, nicotine is standard items, isopropyl alcohol (analyze pure, western Gansu Province chemical industry)
3) condition
Chromatographic column: Agilent HP-5(30m * 0.32mm * 0.25 μ m) gas chromatographic column; Post case temperature: 170 ℃; Detector temperature: 250 ℃; Injector temperature: 250 ℃; Carrier gas: nitrogen (purity >=99.999%), constant temperature flow velocity: 2.0mL/min; Sample size: 2 μ L;
Described detection method comprises the following steps:
1) configuration of extractant: accurately pipette a certain amount of n-heptadecane and dilute in aqueous isopropanol, shake up as extractant, the aqueous isopropanol that the concentration after n-heptadecane dilutes in aqueous isopropanol is 0.2mg/mL.
2) standard serial solution of configuration nicotine: the nicotine that takes 0.5g is dissolved in the brown volumetric flask of 100mL, using isopropyl alcohol constant volume as storing solution, get respectively 0.02,0.1,0.2,0.5,1.0, the storing solution of 2.0mL is in the brown volumetric flask of 10mL, prepare 6 series standard solution (nicotinic density detecting in its concentration range overlay electronic cigarette sample, the nicotinic density scope detecting in electronic cigarette sample is 0.01 mg/mL ~ 3.0 mg/mL), interior mark n-heptadecane concentration is 0.2mg/mL, drawing standard curve; Described nicotine is nicotine or the nicotine salicylate salt of known purity, and preservation condition is 0 ℃ ~ 4 ℃.
3), after adopting cambridge filter and absorption bottle to connect with smoking machine, trapping electronic cigarette flue gas, puts into conical flask by cambridge filter and the absorption liquid of trapping flue gas, carries out oscillation extraction; The suction scheme that described collection electronic cigarette flue gas adopts is determined by the power of electronic smoke atomizer and the parameters such as power of battery, provides the scope of some suction parameters below: suction capacity is 35 ~ 55 mL; The suction duration is 2 ± 0.05s; Suction frequency is 30 ± 0.5s, 60 ± 0.5s; Suction curve is triangular wave, square wave and bell; Puff number scope is 50 ~ 200 mouthfuls.The smoking machine that described trapping electronic cigarette flue gas adopts is linear pattern smoking machine, and cambridge filter diameter is 44mm, and smoking room is constant-temperature constant-humidity environment.For special-shaped and electronic cigarette, the trapping of flue gas need to connect and turns and bracket.Collected cambridge filter and the extract of flue gas and put into conical flask, the volume of extractant can make the appropriate adjustments according to the scope of typical curve nicotinic density.
4) pipette extract filtering membrane, filtrate adopts vapor-phase chromatography to analyze it; Described gas chromatograph is detecting device, registering instrument and the integraph of being furnished with flame ion, and the chromatographic column of employing is the gas chromatographic column of the methyl polysiloxane filler containing phenyl.Instrument condition in described vapor-phase chromatography: post case temperature: 170 ℃; Injector temperature is 250 ℃; Detector temperature: 250 ℃; Carrier gas: helium or nitrogen, flow 30 mL/min; Sampling volume 2 μ L; Analysis time: 6 ~ 8 min.
5) according to typical curve, calculate the content of nicotine in electronic cigarette flue gas.Series standard solution is carried out to GC-FID mensuration, calculate nicotine and interior target peak area ratio in each standard solution, make typical curve or the regression line equation of concentration and peak area ratio, coefficient R is not less than 0.9999.
By electronic cigarette flue gas, according to suction capacity, be 55mL, suction frequency is 2s, suction interval 30s, and suction curve is sinusoidal curve, puff number is that 100 mouthfuls of suctions trap in cambridge filter.By the cambridge filter after suction and the extractant conical flask that is placed in 100mL, sonic oscillation 40min, standing, get organic membrane filtration that supernatant liquor is crossed 0.22 μ m, then sample introduction, calculates the often amount of sucking (mg/ mouth) in electronic cigarette flue gas.
In electronic cigarette flue gas, the content of nicotine is calculated by following formula:
In formula:
xthe content of nicotine in-sample, unit is every mouthful (mg/ mouth) of milligram;
c i -from standard working curve, obtaining nicotinic density, unit is every milliliter (mg/mL) of milligram;
c 0 nicotinic density in-blank test, unit is every milliliter (mg/mL) of milligram;
vthe volume of-extractant, unit is milliliter (mL);
n-puff number, unit is mouth;
Each sample replicate determination 2 times, the mean value of 2 replicate determinations of take is measurement result.
According to above-mentioned Gas Chromatographic Method, select a kind of electronic cigarette, the content that records nicotine in flue gas is 0.018mg/ mouth.
Claims (8)
1. a method for nicotine content in detected electrons cigarette flue gas, is characterized in that described detection method comprises the following steps:
1) configuration of extractant: pipette a certain amount of n-heptadecane and dilute in aqueous isopropanol, shake up as extractant, the concentration range after n-heptadecane dilutes in aqueous isopropanol is 0.1mg/mL ~ 0.5mg/mL;
2) standard serial solution of configuration nicotine: nicotine standard substance is dissolved in aqueous isopropanol, prepares 6 series standard solution, the nicotinic density detecting in its concentration range overlay electronic cigarette sample, drawing standard curve;
3), after adopting cambridge filter and absorption bottle to connect with smoking machine, trapping electronic cigarette flue gas, puts into conical flask by cambridge filter and the absorption liquid of trapping flue gas, carries out oscillation extraction;
4) pipette extract filtering membrane, filtrate adopts vapor-phase chromatography to analyze it;
5) according to typical curve, calculate the content of nicotine in electronic cigarette flue gas.
2. the method for nicotine content in detected electrons cigarette flue gas according to claim 1, is characterized in that described step 2) in nicotine standard substance be nicotine or the nicotine salicylate salt of known purity, preservation condition is 0 ℃ ~ 4 ℃.
3. the method for nicotine content in detected electrons cigarette flue gas according to claim 1, is characterized in that collecting described in step 3) the scope of electronic cigarette flue gas suction parameter: suction capacity is 35 ~ 55 mL; The suction duration is 2 ± 0.05s; Suction frequency is 30 ± 0.5s, 60 ± 0.5s; Suction curve is triangular wave, square wave and bell; Puff number scope is 50 ~ 200 mouthfuls.
4. the method for nicotine content in detected electrons cigarette flue gas according to claim 1, it is characterized in that trapping described in step 3) the smoking machine that electronic cigarette flue gas adopts is linear pattern smoking machine, cambridge filter diameter is 44mm, and smoking room is constant-temperature constant-humidity environment.
5. the method for nicotine content in detected electrons cigarette flue gas according to claim 1, it is characterized in that the gas chromatograph described in step 4) is detecting device, registering instrument and the integraph of being furnished with flame ion, the chromatographic column of employing is the gas chromatographic column of the methyl polysiloxane filler containing phenyl.
6. the method for nicotine content in detected electrons cigarette flue gas according to claim 1, is characterized in that the instrument condition in the vapor-phase chromatography described in step 4): post case temperature: 170 ℃; Injector temperature is 250 ℃; Detector temperature: 250 ℃; Carrier gas: helium or nitrogen, flow 30 mL/min; Sampling volume 2 μ L; Analysis time: 6 ~ 8 min.
7. the method for nicotine content in detected electrons cigarette flue gas according to claim 1, it is characterized in that the cubage of nicotine in the flue gas of electronic cigarette described in step 5), by the typical curve of making, calculate nicotinic density, the content of nicotine in nicotinic density calculating electronic cigarette flue gas, divided by the mouth number of suction, result represents with the milligram number of every mouthful of electronic cigarette.
8. the assay method of nicotine in electronic cigarette flue gas according to claim 1, is characterized in that step 2) described in electronic cigarette sample in its concentration range of nicotinic density of detecting be 0.01 mg/mL ~ 3.0 mg/mL.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104614465A (en) * | 2015-02-16 | 2015-05-13 | 国家烟草质量监督检验中心 | Method for simultaneously measuring content of nicotine, 1,2-propylene glycol and glycerol in electronic smoke sol |
| CN104698117A (en) * | 2015-03-20 | 2015-06-10 | 中国烟草总公司郑州烟草研究院 | Simultaneous determination method for nicotine, 1,2-propylene glycol and glycerol in electronic cigarette smoke |
| CN105067716A (en) * | 2015-07-03 | 2015-11-18 | 江苏中烟工业有限责任公司 | Method for determining puff-by-puff nicotine and tar in cigarette mainstream smoke |
| CN105699519A (en) * | 2016-01-29 | 2016-06-22 | 云南同创检测技术股份有限公司 | Analysis method of transferring rate of nicotine in smoke in electronic cigarette smoking process |
| CN106153767A (en) * | 2016-06-25 | 2016-11-23 | 昌宁德康生物科技有限公司 | A kind of method that nicotine purity in tobacco tar product is detected by the GC of utilization FID |
| CN106442501A (en) * | 2016-09-29 | 2017-02-22 | 福建中烟工业有限责任公司 | Detection method of nicotine content of cigarette liquid of electronic cigarette |
| CN106483216A (en) * | 2016-09-30 | 2017-03-08 | 云南中烟工业有限责任公司 | A kind of mouthful of assay method with nicotine in type smoke-free tobacco product |
| CN108254233A (en) * | 2017-12-29 | 2018-07-06 | 国家烟草质量监督检验中心 | A kind of nicotine solution standard substance and its preparation method and application |
| CN108956848A (en) * | 2018-05-29 | 2018-12-07 | 云南中烟工业有限责任公司 | A kind of method of infrared mirror-reflection furnace-continuous flow method measurement tobacco leaf smoking nicotine |
| CN111398494A (en) * | 2020-03-19 | 2020-07-10 | 云南中烟工业有限责任公司 | Nicotine optical isomer separation and determination method based on reversed-phase two-dimensional liquid chromatography |
| CN112505201A (en) * | 2020-11-11 | 2021-03-16 | 国家烟草质量监督检验中心 | Method for simultaneously measuring release amount of nicotine and inorganic elements in electronic smoke sol |
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| CN104698117A (en) * | 2015-03-20 | 2015-06-10 | 中国烟草总公司郑州烟草研究院 | Simultaneous determination method for nicotine, 1,2-propylene glycol and glycerol in electronic cigarette smoke |
| CN105067716A (en) * | 2015-07-03 | 2015-11-18 | 江苏中烟工业有限责任公司 | Method for determining puff-by-puff nicotine and tar in cigarette mainstream smoke |
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| CN106153767A (en) * | 2016-06-25 | 2016-11-23 | 昌宁德康生物科技有限公司 | A kind of method that nicotine purity in tobacco tar product is detected by the GC of utilization FID |
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| CN108956848A (en) * | 2018-05-29 | 2018-12-07 | 云南中烟工业有限责任公司 | A kind of method of infrared mirror-reflection furnace-continuous flow method measurement tobacco leaf smoking nicotine |
| CN111398494A (en) * | 2020-03-19 | 2020-07-10 | 云南中烟工业有限责任公司 | Nicotine optical isomer separation and determination method based on reversed-phase two-dimensional liquid chromatography |
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