CN114252512A - Method for measuring total nicotine in electronic cigarette liquid and aerosol containing nicotine salt - Google Patents
Method for measuring total nicotine in electronic cigarette liquid and aerosol containing nicotine salt Download PDFInfo
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- SNICXCGAKADSCV-JTQLQIEISA-N (-)-Nicotine Chemical compound CN1CCC[C@H]1C1=CC=CN=C1 SNICXCGAKADSCV-JTQLQIEISA-N 0.000 title claims abstract description 179
- SNICXCGAKADSCV-UHFFFAOYSA-N nicotine Natural products CN1CCCC1C1=CC=CN=C1 SNICXCGAKADSCV-UHFFFAOYSA-N 0.000 title claims abstract description 133
- 229960002715 nicotine Drugs 0.000 title claims abstract description 127
- 239000003571 electronic cigarette Substances 0.000 title claims abstract description 58
- 239000007788 liquid Substances 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 49
- 239000000443 aerosol Substances 0.000 title claims abstract description 34
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 32
- 238000002347 injection Methods 0.000 claims description 28
- 239000007924 injection Substances 0.000 claims description 28
- NDJKXXJCMXVBJW-UHFFFAOYSA-N heptadecane Chemical compound CCCCCCCCCCCCCCCCC NDJKXXJCMXVBJW-UHFFFAOYSA-N 0.000 claims description 26
- 239000000779 smoke Substances 0.000 claims description 21
- 239000003795 chemical substances by application Substances 0.000 claims description 13
- 239000000243 solution Substances 0.000 claims description 11
- 230000000391 smoking effect Effects 0.000 claims description 9
- 239000012086 standard solution Substances 0.000 claims description 5
- 238000007865 diluting Methods 0.000 claims description 4
- 239000003085 diluting agent Substances 0.000 claims description 3
- 238000010790 dilution Methods 0.000 claims description 3
- 239000012895 dilution Substances 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 239000013582 standard series solution Substances 0.000 claims description 3
- 238000003965 capillary gas chromatography Methods 0.000 claims description 2
- 238000005086 pumping Methods 0.000 claims description 2
- 101000777053 Homo sapiens Chromodomain-helicase-DNA-binding protein 1-like Proteins 0.000 claims 1
- 101000635895 Homo sapiens Myosin light chain 4 Proteins 0.000 claims 1
- 102100030739 Myosin light chain 4 Human genes 0.000 claims 1
- 238000004587 chromatography analysis Methods 0.000 claims 1
- 238000000769 gas chromatography-flame ionisation detection Methods 0.000 abstract description 9
- 239000002253 acid Substances 0.000 description 21
- 239000007789 gas Substances 0.000 description 10
- 229940049920 malate Drugs 0.000 description 7
- BJEPYKJPYRNKOW-UHFFFAOYSA-N malic acid Chemical compound OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 description 7
- XPGVXOLNUCRXLA-UHFFFAOYSA-N 3-(1-methylpyrrolidin-2-yl)pyridine;oxalic acid Chemical compound OC(=O)C(O)=O.CN1CCCC1C1=CC=CN=C1 XPGVXOLNUCRXLA-UHFFFAOYSA-N 0.000 description 6
- 238000001514 detection method Methods 0.000 description 6
- FRBGPVAIEYCFOW-UHFFFAOYSA-N 3-(1-methylpyrrolidin-2-yl)pyridine;phosphoric acid Chemical compound OP(O)(O)=O.CN1CCCC1C1=CC=CN=C1 FRBGPVAIEYCFOW-UHFFFAOYSA-N 0.000 description 4
- VAUQRLHPXWYZRZ-PPHPATTJSA-N benzoic acid 3-[(2S)-1-methylpyrrolidin-2-yl]pyridine Chemical compound OC(=O)c1ccccc1.CN1CCC[C@H]1c1cccnc1 VAUQRLHPXWYZRZ-PPHPATTJSA-N 0.000 description 4
- 235000019504 cigarettes Nutrition 0.000 description 4
- 238000004817 gas chromatography Methods 0.000 description 4
- 239000001307 helium Substances 0.000 description 4
- 229910052734 helium Inorganic materials 0.000 description 4
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 4
- QLDPCHZQQIASHX-UHFFFAOYSA-N 2,3-dihydroxybutanedioic acid;3-(1-methylpyrrolidin-2-yl)pyridine Chemical compound OC(=O)C(O)C(O)C(O)=O.CN1CCCC1C1=CC=CN=C1 QLDPCHZQQIASHX-UHFFFAOYSA-N 0.000 description 3
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 3
- 238000003556 assay Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 2
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 2
- 239000012159 carrier gas Substances 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 210000000214 mouth Anatomy 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 230000000638 stimulation Effects 0.000 description 2
- AIBWPBUAKCMKNS-PPHPATTJSA-N 2-hydroxybenzoic acid;3-[(2s)-1-methylpyrrolidin-2-yl]pyridine Chemical compound OC(=O)C1=CC=CC=C1O.CN1CCC[C@H]1C1=CC=CN=C1 AIBWPBUAKCMKNS-PPHPATTJSA-N 0.000 description 1
- SDVKWBNZJFWIMO-UHFFFAOYSA-N 2-hydroxypropane-1,2,3-tricarboxylic acid;3-(1-methylpyrrolidin-2-yl)pyridine Chemical compound CN1CCCC1C1=CC=CN=C1.OC(=O)CC(O)(C(O)=O)CC(O)=O SDVKWBNZJFWIMO-UHFFFAOYSA-N 0.000 description 1
- GFOQKERSYGGJCN-UHFFFAOYSA-N 3-(1-methylpyrrolidin-2-yl)pyridine;propanoic acid Chemical compound CCC(O)=O.CN1CCCC1C1=CC=CN=C1 GFOQKERSYGGJCN-UHFFFAOYSA-N 0.000 description 1
- 239000005711 Benzoic acid Substances 0.000 description 1
- 241000208125 Nicotiana Species 0.000 description 1
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- CPCNAMNNSLASDC-UHFFFAOYSA-N acetic acid;3-(1-methylpyrrolidin-2-yl)pyridine Chemical compound CC(O)=O.CN1CCCC1C1=CC=CN=C1 CPCNAMNNSLASDC-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000012491 analyte Substances 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 235000010233 benzoic acid Nutrition 0.000 description 1
- 238000013375 chromatographic separation Methods 0.000 description 1
- 230000009089 cytolysis Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- WYGGDMVSCZUUMV-UHFFFAOYSA-N formic acid;3-(1-methylpyrrolidin-2-yl)pyridine Chemical compound OC=O.CN1CCCC1C1=CC=CN=C1 WYGGDMVSCZUUMV-UHFFFAOYSA-N 0.000 description 1
- 235000011389 fruit/vegetable juice Nutrition 0.000 description 1
- 229960005150 glycerol Drugs 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000004811 liquid chromatography Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 229960004063 propylene glycol Drugs 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 210000002345 respiratory system Anatomy 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 230000001953 sensory effect Effects 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention discloses a method for accurately measuring total nicotine in electronic cigarette liquid and aerosol containing nicotine salt. The method comprises the steps of measuring the content of total nicotine in the electronic cigarette liquid containing the nicotine salt by using a gas phase method (GC-FID), and researching the influence of the temperature of a sample inlet, the flow split ratio and the nicotine concentration of the sample inlet on the content of the total nicotine in detail, wherein the gas phase sample inlet temperature is 250-300 ℃, the flow split ratio is 5-50: 1, and the content of the total nicotine in the electronic cigarette containing the nicotine salt is more accurate when the nicotine concentration of the sample inlet is less than or equal to 0.001 mg/mL.
Description
Technical Field
The invention belongs to the field of nicotine detection, and relates to a method for determining total nicotine in electronic cigarette liquid and aerosol containing nicotine salt.
Background
The electronic cigarette is a device which atomizes the tobacco juice to generate aerosol in an electric heating mode and is used for being sucked by consumers. Due to the low atomization temperature, the release amount of harmful ingredients is far lower than that of the traditional cigarette, and the cigarette is favored by consumers in recent years. In order to make consumers obtain satisfaction, a certain proportion of nicotine is usually added into electronic cigarette liquid, but two problems exist, namely firstly, the nicotine is mainly adhered to the oral cavity and the upper respiratory tract, so that strong stimulation and throat choking are generated during smoking; ② the nicotine is easy to be oxidized after long-time storage, which causes the satisfaction in suction to be reduced. Therefore, in 2015, Pax Labs company takes benzoic acid as an additive to react with nicotine to generate nicotine benzoate, so that consumers feel smooth in the process of smoking. The electronic cigarette liquid containing nicotine salt can overcome the defects of bad smell, stimulation, large miscellaneous gas and poor sensory experience caused by free nicotine in aerosol, and can also increase the nicotine stability in the process of placing the electronic cigarette liquid.
At present, methods for measuring the nicotine content in electronic cigarette liquid mainly comprise gas chromatography, liquid chromatography and the like. A method for measuring nicotine, 1, 2-propylene glycol and glycerol in electronic cigarette liquid is established by adopting gas chromatography, such as Chua Junlan and the like, and the method is simple and convenient to operate, is suitable for measuring a large number of samples, and cannot measure the content of nicotine salt. In the prior art, CN104062385A adopts a GC-FID method to determine the nicotine content in electronic smoke, but under the operating condition, the total nicotine content in smoke containing nicotine salt cannot be determined, and only free nicotine content can be measured. Also, in the previous research (CN11323490A) of determining the content of free nicotine and nicotine salt in the electronic cigarette liquid and the smoke aerosol by a gas phase method, the inventor of the present application found that the nicotine content in the nicotine salt could not be effectively determined at the temperature of the injection sample of 100-. Mainly because part of the nicotine salts are not completely cracked under the measuring conditions and cannot be completely detected.
However, most of nicotine in the existing electronic cigarette liquid containing nicotine exists in the form of nicotine salt, and if the content of nicotine is measured by the existing method, accurate nicotine content cannot be provided, which causes certain misleading to consumers, so a method for accurately measuring the content of nicotine in the electronic cigarette liquid containing nicotine salt is needed.
Disclosure of Invention
The invention takes the electronic cigarette liquid containing nicotine salt and the smoke aerosol as research objects, selects the proper range of the temperature of the sample inlet by a gas phase method by analyzing the release temperature range of several commonly used nicotine salts, ensures that the nicotine salts can be completely cracked, and researches the influence of the temperature of the sample inlet, the flow division ratio and the nicotine concentration of the sample inlet on the total nicotine measured value in detail, aiming at establishing a method for accurately measuring the total nicotine in the electronic cigarette liquid containing nicotine salt and the smoke aerosol by adopting GC-FID.
In order to achieve the purpose, the technical scheme provided by the invention is as follows:
a method for measuring total nicotine in electronic cigarette liquid and aerosol containing nicotine salt comprises the following steps:
s1, preparation of an extracting agent: transferring a certain amount of n-heptadecane to an isopropanol solution for dilution and shaking up to be used as an extracting agent, wherein the concentration range of the diluted n-heptadecane in the isopropanol solution is 0.01 mg/mL-0.1 mg/mL;
s2, preparing a standard series solution of nicotine: dissolving nicotine in isopropanol solution, preparing 5 series of standard solutions, covering the concentration range of nicotine detected in the electronic cigarette sample, and drawing a standard curve;
s3, diluting the electronic cigarette liquid containing nicotine salt or the Cambridge filter disc for collecting the electronic smoke aerosol containing nicotine salt with an extracting agent, and analyzing the diluent by adopting a GC-FID method;
s4, calculating the nicotine content according to the standard curve;
the electronic cigarette liquid containing nicotine salt or the Cambridge filter for collecting the electronic cigarette aerosol in the step S3 is diluted by an extracting agent until the concentration of nicotine is less than or equal to 0.001 mg/mL.
Preferably, the nicotine salt in step S3 includes one or more of nicotine tartrate, nicotine malate, nicotine phosphate, nicotine citrate, nicotine acetate, nicotine oxalate, nicotine benzoate, nicotine formate, nicotine propionate, and nicotine salicylate.
Preferably, the concentration of the standard solution in step S2 is 0.0002, 0.0004, 0.008, 0.0016, 0.0032 mg/mL.
Preferably, the nicotine salt-containing e-liquid described in step S3 or the cambridge filter for collecting e-smoke aerosol is diluted with an extractant to a nicotine concentration of 0.0005 mg/mL.
Preferably, the suction parameters of the suction scheme adopted by the cambridge filter for collecting the electronic smoke aerosol in step S3 are as follows: the suction capacity is 55mL, the suction time is 3s, the suction interval is 30s, and 30-port smoke aerosol is collected; the pumping curves are triangular, square and bell shaped.
Preferably, the smoking machine adopted by the cambridge filter for collecting the electronic smoke aerosol in the step S3 is a linear smoking machine, the diameter of the cambridge filter is 44mm, and the smoking room is in a constant temperature and humidity environment. For special-shaped and large electronic cigarettes, the collection of smoke needs a connecting bracket.
Preferably, the cambridge filter disc and the extraction liquid which collect the smoke are put into a conical flask, and the volume of the extraction agent can be properly adjusted according to the range of the nicotine concentration of a standard curve.
Preferably, the GC-FID described in step S3 uses a column of DB-ALC1(30m × 0.32mm × 0.118 μm) capillary gas chromatography.
Preferably, the instrument conditions in the GC-FID process described in step S3 are: temperature of the column box: 170 ℃; the temperature of a sample inlet is 280-300 ℃; the split ratio is 5-50: 1, the temperature of a detector is as follows: 275 ℃; carrier gas: helium (99.999%), constant flow mode flow rate: 1.0 mL/min; compressed air flow rate: 400.0 mL/min; hydrogen flow rate: 40.0 mL/min; tail-blow helium flow rate: 25.0 mL/min; sample introduction amount: 1 mu L, split-flow sample injection; temperature rising procedure: 90 deg.C (1min), 15 deg.C/min; 120 deg.C (0min), 40 deg.C/min; 240 deg.C (4 min).
Further preferably, the injection port temperature is 280-300 ℃.
Further preferably, the injection port temperature is 300 ℃.
The temperature is too low, the nicotine salt can not be completely cracked, and the test result of the content of the total nicotine is lower.
More preferably, the flow dividing ratio is 5-25: 1.
Further preferably, the split ratio is 25: 1.
The split ratio is high, namely, less gas enters the chromatographic column, and when the chromatographic peak cannot be separated or the tailing is serious, the split ratio is properly adjusted to improve the separation. If the split ratio is too large, the peaks of the components have good separation degree, but if the sensitivity of the detector is insufficient, the peaks obtained by the trace components are very small, even the trace components cannot be detected, so that the basis of qualitative and quantitative determination is lost. The split ratio is low, i.e. more gas enters the chromatographic column, when the content of the analyte is low, the separation degree of each chromatographic peak in the chromatogram is reduced, the retention value of each peak is shortened, and even each component peak can not be separated, i.e. chromatographic separation fails. It is therefore important to carefully determine the split ratio based on the composition of the sample.
The influence of the injection port temperature and the split ratio on the detection result is not independent, the two influence each other, and the nicotine salt can be completely cracked when the injection port temperature is 300 ℃ and the split ratio is 25:1, so that the test result is more accurate.
And step S4, calculating the nicotine content, calculating the nicotine concentration according to the prepared standard curve, and calculating the nicotine content in the electronic cigarette smoke aerosol and the electronic cigarette liquid according to the nicotine concentration to be accurate to 0.0001 mg.
The method has universality for measuring the content of nicotine salt with the decomposition temperature of 200-300 ℃, is simple and easy to operate, has simple treatment steps, and is a method for accurately analyzing the total nicotine content in the electronic cigarette liquid containing nicotine salt.
The invention is further explained below:
taking a certain amount of electronic cigarette liquid containing nicotine salt or a Cambridge filter disc sample for collecting electronic smoke aerosol containing nicotine salt, diluting the electronic cigarette liquid with extract liquid containing internal standard, performing ultrasonic treatment for 10-40 min at room temperature, and determining the total nicotine content in the electronic cigarette liquid containing nicotine salt by a gas phase method (GC-FID), wherein the gas phase injection port temperature is 280-300 ℃, the split ratio is 5-50: 1, and the determination of the total nicotine content in the electronic cigarette containing nicotine salt is more accurate when the nicotine concentration at the injection port is less than or equal to 0.001 mg/mL. The method has important theoretical significance and practical value in the process of selecting raw materials for blending the electronic cigarette oil and controlling the taste absorption quality of the electronic cigarette oil.
Drawings
FIG. 1 is a graph of the effect of mouth temperature on total nicotine assay results;
FIG. 2 Effect of split ratio on Total nicotine assay results
FIG. 3 Effect of inlet nicotine concentration on Total nicotine assay results
Detailed Description
Example 1
Instruments and instrument working conditions:
the chromatographic column is a DB-ALC1(30m × 0.32mm × 0.118 μm) capillary gas chromatographic column.
Preferably, the instrument conditions in the GC-FID process described in step S3 are: temperature of the column box: 170 ℃; detector temperature: 275 ℃; carrier gas: helium (99.999%), constant flow mode flow rate: 1.0 mL/min; compressed air flow rate: 400.0 mL/min; hydrogen flow rate: 40.0 mL/min; tail-blow helium flow rate: 25.0 mL/min; sample introduction amount: 1 mu L, split-flow sample injection; temperature rising procedure: 90 deg.C (1min), 15 deg.C/min; 120 deg.C (0min), 40 deg.C/min; 240 deg.C (4 min).
The detection comprises the following steps:
s1, preparation of an extracting agent: transferring a certain amount of n-heptadecane to an isopropanol solution for dilution and shaking up to be used as an extracting agent, wherein the concentration range of the diluted n-heptadecane in the isopropanol solution is 0.01 mg/mL-0.1 mg/mL;
s2, preparing a standard series solution of nicotine: dissolving nicotine in isopropanol solution, preparing 5 series of standard solutions, covering the concentration range of nicotine detected in the electronic cigarette sample, and drawing a standard curve;
s3, diluting the electronic cigarette liquid containing nicotine salt or the Cambridge filter disc for collecting the electronic smoke aerosol containing nicotine salt with an extracting agent, and analyzing the diluent by adopting a GC-FID method;
and S4, calculating the nicotine content according to the standard curve.
The method provided by the invention is applied to determine the total nicotine content in the electronic cigarette liquid containing nicotine salt, wherein the nicotine salt in the electronic cigarette liquid is as follows: nicotine tartrate (molar ratio of nicotine to acid 1:1), nicotine phosphate (molar ratio of nicotine to acid 1:1), nicotine benzoate (molar ratio of nicotine to acid 1:1), nicotine oxalate (molar ratio of nicotine to acid 2:1), nicotine malate (molar ratio of nicotine to acid 1:1), nicotine malate (molar ratio of nicotine to acid 2: 1). The extractant selects isopropanol, n-heptadecane is used as an internal standard, the temperature of a sample inlet is 250 ℃, 280 ℃, 300 ℃, the split ratio is 25:1, the nicotine concentration at the sample inlet is 0.001mg/mL, and the measurement result (figure 1) shows that the total nicotine content in the electronic cigarette liquid of the 7 nicotine salts is increased along with the increase of the temperature of the sample inlet, the ratio of the measured value to the actual value is also increased all the time, which indicates that the temperature of the sample inlet is increased, the pyrolysis of the nicotine salts is more complete, and the detection data is more accurate. Especially nicotine oxalate (molar ratio of nicotine to acid is 2:1), the injection inlet temperature is 250 ℃, the ratio of the measured value to the actual value is only 65%, the temperature is increased to 300 ℃, the ratio of the measured value to the actual value is increased to 95%, and the accurate value of the test is obviously improved.
Example 2
The method provided by the invention is applied to determine the total nicotine content in the electronic cigarette liquid containing nicotine salt, wherein the nicotine salt in the electronic cigarette liquid is as follows: nicotine tartrate (molar ratio of nicotine to acid 1:1), nicotine phosphate (molar ratio of nicotine to acid 1:1), nicotine oxalate (molar ratio of nicotine to acid 2:1), nicotine malate (molar ratio of nicotine to acid 1:1), nicotine malate (molar ratio of nicotine to acid 2: 1). Wherein the extractant selects isopropanol, n-heptadecane as an internal standard, the injection port temperature is 300 ℃, the split ratio is 5:1, 15:1 and 25:1, and the nicotine concentration at the injection port is 0.001 mg/mL. As shown in fig. 2, most of the nicotine-containing e-liquid exhibited more complete lysis and more accurate detection data as the split ratio increased. Especially nicotine oxalate (molar ratio of nicotine to acid is 1:1), the split ratio is 5:1, the ratio of the measured value to the actual value is only 94%, the split ratio is increased to 25:1, the ratio of the measured value to the actual value is increased to 100%, and the accurate value of the test is obviously improved.
Example 3
The method provided by the invention is applied to determine the total nicotine content in the electronic cigarette liquid containing nicotine salt, wherein the nicotine salt in the electronic cigarette liquid is as follows: nicotine tartrate (molar ratio of nicotine to acid 1:1), nicotine phosphate (molar ratio of nicotine to acid 1:1), nicotine benzoate (molar ratio of nicotine to acid 1:1), nicotine oxalate (molar ratio of nicotine to acid 2:1), nicotine malate (molar ratio of nicotine to acid 1:1), nicotine malate (molar ratio of nicotine to acid 2: 1). Wherein the extractant selects isopropanol, n-heptadecane as an internal standard, the injection port temperature is 300 ℃, the split ratio is 25:1, and the nicotine concentration at the injection port is 0.0005mg/mL, 0.001mg/mL, 0.002mg/mL and 0.008 mg/mL. As shown in fig. 3, it can be seen that most of the nicotine-containing e-liquid is more completely cracked as the nicotine concentration at the injection port decreases. For example, nicotine tartrate (nicotine to acid molar ratio of 1:1), the nicotine concentration at the injection port is 0.008mg/mL, the ratio of the measured value to the actual value is only 80%, while the nicotine concentration at the injection port is reduced to 0.001mg/mL, and the ratio of the measured value to the actual value is increased to 94%; and the nicotine concentration at the sample inlet is reduced to 0.0005mg/mL, the ratio of the measured value to the actual value is improved to 99 percent, and the accurate value of the test is obviously improved. The result shows that the amount of nicotine at the sample inlet has great influence on the total nicotine determination result. The invention finds that the proper range of the nicotine concentration at the gas phase injection port is less than or equal to 0.001mg/mL when the total nicotine content in the electronic cigarette liquid containing nicotine salt is measured, the nicotine salt can be completely cracked at the injection port of the gas chromatography within the range, and the measured total nicotine content is accurate.
Example 4
The method provided by the invention is applied to determine the total nicotine content in the electronic cigarette liquid containing nicotine salt, wherein the nicotine salt in the electronic cigarette liquid is as follows: nicotine tartrate (molar ratio of nicotine to acid 1: 1). Wherein the extractant selects isopropanol, n-heptadecane as an internal standard, the injection port temperature is 300 ℃, the split ratio is 25:1, and the nicotine concentration at the injection port is 0.0005 mg/mL. The content of the total nicotine in the electronic cigarette liquid is measured to be 36.20mg/g, and the actual value is 36.57 mg/g. The ratio of measured value/actual value was 99%.
The same sample is diluted by isopropanol solution containing heptadecane by the method in CN111323490A, the injection inlet temperature is 250 ℃, the split ratio is 5:1, and the nicotine concentration at the injection inlet is 0.01 mg/mL. The content of the total nicotine in the electronic cigarette liquid is 32.91mg/g by GC method, and the actual value is 36.57 mg/g. The ratio of measured value/actual value was 90%. Therefore, it can be seen that the method of the present invention is more accurate.
Example 5
The method is used for measuring the total nicotine content in 30-port aerosol of the tartrate nicotine salt electronic cigarette liquid with the nicotine concentration of 36.57mg/mL, isopropanol is selected as an extracting agent, n-heptadecane is used as an internal standard, the injection port temperature is 300 ℃, the split ratio is 25:1, the nicotine concentration at the injection port is 0.001mg/mL, and the measurement result is shown in Table 1.
The method in CN111323490A is adopted for the same sample, the total nicotine content in 30-port aerosol of the tartrate nicotine salt electronic cigarette liquid with the nicotine concentration of 36.57mg/mL is measured, a filter disc for collecting the aerosol is added with 5mL of isopropanol solution containing heptadecane internal standard, oscillation is carried out for 30min, the nicotine content in the aerosol is measured by a gas phase method, the injection port temperature is 250 ℃, the split ratio is 5:1, and the nicotine concentration at the injection port is 0.01 mg/mL. The results are shown in Table 1.
TABLE 1 comparison of total nicotine content in 30-mouth aerosol of tartaric nicotine salt electronic cigarette liquid with total nicotine content in corresponding cigarette liquid
It can be seen that the total nicotine content in the 30-mouth aerosol of the electronic cigarette liquid containing tartaric acid nicotine salt is less than the total nicotine content in the corresponding cigarette liquid, which indicates that the total nicotine in the electronic cigarette liquid does not completely migrate into the electronic cigarette aerosol during the smoking process of the electronic cigarette, and the mobility into the aerosol is 74.94%. According to the prior art, part of nicotine content in the electronic smoke sol is not tested, and the tested mobility is only 69.02%. It can be seen that the detection accuracy of the invention is higher.
Claims (8)
1. A method for measuring total nicotine in electronic cigarette liquid and aerosol containing nicotine salt is characterized by comprising the following steps:
s1, preparation of an extracting agent: transferring a certain amount of n-heptadecane to an isopropanol solution for dilution, and shaking up to be used as an extracting agent, wherein the concentration range of the diluted n-heptadecane in the isopropanol solution is 0.01 mg/mL-0.1 mg/mL;
s2, preparing a standard series solution of nicotine: dissolving nicotine in isopropanol solution, preparing 5 series of standard solutions, covering the concentration range of nicotine detected in the electronic cigarette sample, and drawing a standard curve;
s3, diluting the electronic cigarette liquid containing nicotine salt or the Cambridge filter disc for collecting the electronic smoke aerosol containing nicotine salt with an extracting agent, and analyzing the diluent by adopting a GC ‒ FID method;
s4, calculating the nicotine content according to the standard curve;
the electronic cigarette liquid containing nicotine salt or the Cambridge filter for collecting the electronic cigarette aerosol in the step S3 is diluted by an extracting agent until the concentration of nicotine is less than or equal to 0.001 mg/mL.
2. The method of claim 1, wherein the standard solution in step S2 has a concentration of 0.0002 mg/mL, 0.0004 mg/mL, 0.008mg/mL, 0.0016 mg/mL, 0.0032 mg/mL.
3. The method of claim 1, wherein the nicotine salt-containing e-liquid or cambridge filter used to collect e-smoke aerosol of step S3 is diluted with an extractant to a nicotine concentration of 0.0005 mg/mL.
4. The method according to claim 1, wherein the suction parameters of the suction scheme adopted by the cambridge filter for collecting the e-smoke aerosol in step S3 are as follows: the suction capacity is 55mL, the suction time is 3s, the suction interval is 30s, and 30-port smoke aerosol is collected; the pumping curves are triangular, square and bell shaped.
5. The method according to claim 1, wherein the smoking machine used in the Cambridge filter for collecting the electronic smoke aerosol in step S3 is a linear smoking machine, the diameter of the Cambridge filter is 44mm, and the smoking room is a constant temperature and humidity environment.
6. The method according to claim 1, wherein the GC ‒ FID in step S3 employs a chromatography column of DB ‒ ALC1(30m x 0.32mm x 0.118 μm) capillary gas chromatography column; instrument conditions in the GC ‒ FID method described in step S3: the temperature of a sample inlet is 250-300 ℃; the split ratio is 5-50: 1.
7. The method as claimed in claim 6, wherein the injection port temperature is 280-300 ℃.
8. The method according to claim 6, wherein the split ratio is 5-25: 1.
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