CN111337603A - Method for measuring nicotine content in tobacco product and method for simultaneously measuring water, 1, 2-propylene glycol, glycerol and nicotine content - Google Patents
Method for measuring nicotine content in tobacco product and method for simultaneously measuring water, 1, 2-propylene glycol, glycerol and nicotine content Download PDFInfo
- Publication number
- CN111337603A CN111337603A CN202010376686.XA CN202010376686A CN111337603A CN 111337603 A CN111337603 A CN 111337603A CN 202010376686 A CN202010376686 A CN 202010376686A CN 111337603 A CN111337603 A CN 111337603A
- Authority
- CN
- China
- Prior art keywords
- nicotine
- tobacco product
- concentration
- glycerol
- content
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 title claims abstract description 252
- SNICXCGAKADSCV-JTQLQIEISA-N (-)-Nicotine Chemical compound CN1CCC[C@H]1C1=CC=CN=C1 SNICXCGAKADSCV-JTQLQIEISA-N 0.000 title claims abstract description 181
- 229960002715 nicotine Drugs 0.000 title claims abstract description 181
- SNICXCGAKADSCV-UHFFFAOYSA-N nicotine Natural products CN1CCCC1C1=CC=CN=C1 SNICXCGAKADSCV-UHFFFAOYSA-N 0.000 title claims abstract description 181
- 235000019505 tobacco product Nutrition 0.000 title claims abstract description 148
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 title claims abstract description 138
- 229960005150 glycerol Drugs 0.000 title claims abstract description 82
- 229960004063 propylene glycol Drugs 0.000 title claims abstract description 80
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 68
- 238000000034 method Methods 0.000 title claims abstract description 59
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical group OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 117
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims abstract description 105
- 239000003960 organic solvent Substances 0.000 claims abstract description 40
- 239000002904 solvent Substances 0.000 claims abstract description 24
- 239000007788 liquid Substances 0.000 claims abstract description 20
- 238000004817 gas chromatography Methods 0.000 claims abstract description 17
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 238000001514 detection method Methods 0.000 claims description 74
- SMUQFGGVLNAIOZ-UHFFFAOYSA-N quinaldine Chemical group C1=CC=CC2=NC(C)=CC=C21 SMUQFGGVLNAIOZ-UHFFFAOYSA-N 0.000 claims description 54
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 claims description 36
- DNIAPMSPPWPWGF-GSVOUGTGSA-N (R)-(-)-Propylene glycol Chemical compound C[C@@H](O)CO DNIAPMSPPWPWGF-GSVOUGTGSA-N 0.000 claims description 22
- 235000013772 propylene glycol Nutrition 0.000 claims description 22
- 238000003556 assay Methods 0.000 claims description 8
- 238000010813 internal standard method Methods 0.000 claims description 7
- 239000006228 supernatant Substances 0.000 claims description 5
- 238000000527 sonication Methods 0.000 claims description 4
- 230000000284 resting effect Effects 0.000 claims 2
- 238000000605 extraction Methods 0.000 abstract description 47
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 51
- 239000000243 solution Substances 0.000 description 35
- 230000000052 comparative effect Effects 0.000 description 33
- 238000004458 analytical method Methods 0.000 description 14
- 239000003795 chemical substances by application Substances 0.000 description 14
- 241000208125 Nicotiana Species 0.000 description 12
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 12
- 239000000126 substance Substances 0.000 description 12
- BZLVMXJERCGZMT-UHFFFAOYSA-N Methyl tert-butyl ether Chemical compound COC(C)(C)C BZLVMXJERCGZMT-UHFFFAOYSA-N 0.000 description 11
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 10
- 239000007789 gas Substances 0.000 description 9
- 239000000523 sample Substances 0.000 description 9
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 8
- 239000000203 mixture Substances 0.000 description 8
- 239000007864 aqueous solution Substances 0.000 description 6
- SMWDFEZZVXVKRB-UHFFFAOYSA-N Quinoline Chemical compound N1=CC=CC2=CC=CC=C21 SMWDFEZZVXVKRB-UHFFFAOYSA-N 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 239000000779 smoke Substances 0.000 description 5
- 229940083957 1,2-butanediol Drugs 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- BMRWNKZVCUKKSR-UHFFFAOYSA-N butane-1,2-diol Chemical compound CCC(O)CO BMRWNKZVCUKKSR-UHFFFAOYSA-N 0.000 description 4
- 235000019504 cigarettes Nutrition 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- NDJKXXJCMXVBJW-UHFFFAOYSA-N heptadecane Chemical compound CCCCCCCCCCCCCCCCC NDJKXXJCMXVBJW-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000012074 organic phase Substances 0.000 description 4
- 230000010355 oscillation Effects 0.000 description 4
- 230000001953 sensory effect Effects 0.000 description 4
- 238000004587 chromatography analysis Methods 0.000 description 3
- 238000007796 conventional method Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 238000011002 quantification Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 239000012086 standard solution Substances 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 239000012159 carrier gas Substances 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000010812 external standard method Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- FKSLYSSVKFYJKE-UHFFFAOYSA-N n,n-diethylethanamine;methanol Chemical compound OC.CCN(CC)CC FKSLYSSVKFYJKE-UHFFFAOYSA-N 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 230000001988 toxicity Effects 0.000 description 2
- 231100000419 toxicity Toxicity 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000007794 irritation Effects 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000003808 methanol extraction Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- -1 moisture Chemical compound 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 125000002943 quinolinyl group Chemical group N1=C(C=CC2=CC=CC=C12)* 0.000 description 1
- 238000000611 regression analysis Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 239000012488 sample solution Substances 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 230000000391 smoking effect Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- 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
-
- 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
- G01N30/62—Detectors specially adapted therefor
- G01N30/64—Electrical detectors
- G01N30/66—Thermal conductivity detectors
-
- 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
- G01N30/62—Detectors specially adapted therefor
- G01N30/64—Electrical detectors
- G01N30/68—Flame ionisation detectors
-
- 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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
Landscapes
- Physics & Mathematics (AREA)
- 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 relates to a method for measuring nicotine content in tobacco products, which comprises the following steps: mixing an organic solvent with the volume of V with the tobacco product with the mass of m, and extracting nicotine in the tobacco product to obtain an extract liquid, wherein the organic solvent is a methanol solvent containing triethylamine; analyzing the nicotine content of the extract liquor by adopting a gas chromatography to obtain the nicotine concentration in the extract liquor; calculating the nicotine content in the tobacco product according to V, m and the obtained nicotine concentration. In the invention, the nicotine in the tobacco product can be completely extracted, so that the nicotine in the tobacco product can be accurately measured. Meanwhile, the operation steps are reduced by adopting a one-step extraction method, so that the loss of nicotine in the extraction operation is reduced, and the accuracy of nicotine determination is further improved. The invention also relates to a method for simultaneously measuring the contents of water, 1, 2-propylene glycol, glycerol and nicotine in the tobacco products.
Description
Technical Field
The invention belongs to the technical field of detection analysis application, and particularly relates to a method for determining nicotine content in tobacco products and a method for simultaneously determining water, 1, 2-propylene glycol, glycerol and nicotine content
Background
The moisture content in the tobacco product which is not burned by heating not only affects the rolling of the tobacco product, but also directly affects the sensory quality of the product, such as the first bite smoke temperature. 1, 2-propylene glycol or glycerol with high content is usually added into a heating non-combustible tobacco product as an atomizing agent, and the types and the content of the atomizing agent are different, so that the smoke generation effect and the sensory quality are directly influenced; the nicotine is a key active ingredient of the tobacco products, and the total nicotine content in the tobacco products is closely related to the strength, the irritation and the like of smoke.
In order to extract nicotine from tobacco as completely as possible, the conventional method is to extract the nicotine by a two-step method, i.e., soaking tobacco material in a high-concentration sodium hydroxide aqueous solution, and then extracting the tobacco material with n-hexane or methyl tert-butyl ether. The organic phase obtained from the extraction of n-hexane or methyl tert-butyl ether was then subjected to GC-FID (gas chromatography-flame ionization Detector) analysis. However, the conventional nicotine determination method is complex in operation and has high operation requirements on detection personnel. In addition, the tobacco products measured by the conventional measuring method still have the problems of inaccurate measuring results and poor measuring result precision.
Disclosure of Invention
The invention aims to solve the problem that the nicotine in the tobacco products is inaccurate to measure in the prior art.
In order to solve the technical problem, the invention provides a method for measuring nicotine in tobacco products, which comprises the following steps:
mixing an organic solvent with the volume of V with the tobacco product with the mass of m, and extracting nicotine in the tobacco product to obtain an extract liquid, wherein the organic solvent is a methanol solvent containing triethylamine; analyzing the nicotine content of the extract liquor by adopting a gas chromatography to obtain the nicotine concentration in the extract liquor; calculating the nicotine content in the tobacco product according to V, m and the obtained nicotine concentration.
By adopting the technical scheme, the nicotine in the tobacco products can be completely extracted, so that the nicotine in the tobacco products can be accurately measured. Meanwhile, the operation steps are reduced by adopting a one-step extraction method, so that the loss of nicotine in the extraction operation is reduced, and the accuracy of nicotine determination is further improved.
Furthermore, the volume ratio concentration of triethylamine in the methanol solvent is 1-10%.
Further, the volume ratio concentration of triethylamine in the methanol solvent was 4%.
Further, the nicotine concentration in the extract is chromatographed by an internal standard method, wherein the internal standard substance comprises 2-methylquinoline.
Further, the concentration of 2-methylquinoline is 0.1mg/mL to 1 mg/mL.
Further, the concentration of 2-methylquinoline was 0.5 mg/mL.
Further, after mixing the organic solvent and the tobacco product, oscillating or ultrasonically treating the mixture, and then standing the mixture to obtain an extract.
Further, the time of oscillation or ultrasound was 3 hours, and the time of standing was 10 min.
Further, the tobacco product is a heat non-combustible tobacco product.
The invention also provides a method for simultaneously measuring water, 1, 2-propylene glycol, glycerol and nicotine in tobacco products, which comprises the following steps:
mixing an organic solvent with a volume of V with a tobacco product with a mass of m, and extracting water, 1, 2-propylene glycol, glycerol and nicotine in the tobacco product to obtain an extract liquid, wherein the organic solvent is a methanol solvent containing triethylamine; taking the extract as a first detection solution, and analyzing the water content of the first detection solution by adopting a gas chromatography to obtain the concentration of water in the first detection solution; taking the extract as a second detection solution, and analyzing the content of 1, 2-propylene glycol, glycerol and nicotine in the second detection solution by gas chromatography to obtain the concentration of 1, 2-propylene glycol, glycerol and nicotine in the second detection solution; and respectively calculating the water content, the 1, 2-propylene glycol content, the glycerol content and the nicotine content in the tobacco product according to V, m and the obtained water, 1, 2-propylene glycol, glycerol and nicotine concentrations.
By adopting the technical scheme, the contents of water, 1, 2-butanediol, glycerol and nicotine in the tobacco products can be measured simultaneously, the detection flow is obviously simplified, the analysis cost is reduced, and the detection efficiency is improved. Meanwhile, the operation steps are reduced by adopting a one-step extraction method, so that the loss of nicotine in the extraction operation is reduced, and the accuracy of nicotine determination is further improved.
Furthermore, the volume ratio concentration of triethylamine in the methanol solvent is 1-10%.
Further, the volume ratio concentration of triethylamine in the methanol solvent was 4%.
Further, performing chromatographic analysis on the concentrations of water, 1, 2-propylene glycol, glycerol and nicotine in the extract by using an internal standard method, wherein the internal standard substance comprises 1, 4-butanediol and 2-methylquinoline, the 1, 4-butanediol is used as an internal standard of water, 1, 2-propylene glycol and glycerol, and the 2-methylquinoline is used as an internal standard of nicotine.
Further, the concentration of 1, 4-butanediol is 0.5mg/mL to 10mg/mL, and the concentration of 2-methylquinoline is 0.1mg/mL to 1 mg/mL.
Further, the concentration of 1, 4-butanediol was 3mg/mL, and the concentration of 2-methylquinoline was 0.5 mg/mL.
Further, after mixing the organic solvent with the tobacco product, oscillating or ultrasonically treating the mixture, and then standing the mixture to obtain an extract.
Further, the time of oscillation or ultrasound was 3 hours, and the time of standing was 10 min.
Further, the tobacco product is a heat non-combustible tobacco product.
Detailed Description
The following description of the embodiments of the present invention is provided for illustrative purposes, and other advantages and effects of the present invention will become apparent to those skilled in the art from the present disclosure. While the invention will be described in conjunction with the preferred embodiments, it is not intended that features of the invention be limited to these embodiments. On the contrary, the invention is described in connection with the embodiments for the purpose of covering alternatives or modifications that may be extended based on the claims of the present invention. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. The invention may be practiced without these particulars. Moreover, some of the specific details have been left out of the description in order to avoid obscuring or obscuring the focus of the present invention. It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict.
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be described in further detail below.
In the traditional nicotine determination method, a two-step extraction method is used, wherein a tobacco product is soaked in a high-concentration sodium hydroxide aqueous solution in the first step, and the organic phase obtained by extracting n-hexane or methyl tert-butyl ether is subjected to gas chromatography in the second step. In order to extract nicotine from tobacco products as much as possible for detection in the conventional method, an excessive amount of sodium hydroxide aqueous solution is used, i.e. the concentration of sodium hydroxide in the aqueous solution reaches 5 mol/L-10 mol/L. The inventors have found that although a high concentration of aqueous sodium hydroxide solution is beneficial in maximizing the extraction of nicotine from tobacco products, the tobacco material becomes a pulpy material when added to a high concentration of aqueous sodium hydroxide solution, which adsorbs a portion of the nicotine. That is, when the conventional two-step extraction method is used, a high-concentration sodium hydroxide aqueous solution can adsorb part of nicotine, so that nicotine in tobacco products is not completely extracted by n-hexane or methyl tert-butyl ether, and a large amount of sodium hydroxide is used to cause raw material waste, and the experimental personnel can be injured if the operation is careless. Due to incomplete extraction, nicotine determination can be inaccurate. Moreover, after the second extraction step, the supernatant needs to be extracted, and the supernatant is easily contaminated by the aqueous phase in the process, which also causes inaccurate detection results. In addition, in the two-step extraction method, partial moisture can be mixed into the organic phase, and the chromatographic column is easily damaged when the moisture enters the gas chromatographic column for gas chromatographic analysis. The two-step extraction method has higher operation requirements on detection personnel and is easy to cause errors in the operation process, so that the nicotine determination is inaccurate.
Attempts have been made to reduce the concentration of sodium hydroxide to reduce the adsorption of the extracted nicotine by the aqueous sodium hydroxide solution, but once the concentration of sodium hydroxide is reduced, the amount of nicotine extracted from the tobacco product is also reduced. The nicotine in the tobacco products can not be efficiently extracted by only adopting the organic solvent.
Therefore, the invention provides a method for measuring nicotine in tobacco products, which comprises the following steps: mixing an organic solvent with the volume of V with the tobacco product with the mass of m, and extracting nicotine in the tobacco product to obtain an extract liquid, wherein the organic solvent is a methanol solvent containing triethylamine; analyzing the nicotine content of the extract by gas chromatography, namely, pumping the extract obtained by directly extracting the organic solvent into a gas chromatography instrument for analysis to obtain the nicotine concentration in the extract; calculating the nicotine content in the tobacco product according to V, m and the obtained nicotine concentration. The gas chromatography may be, for example, GC-FID, GC-MS (gas chromatography-mass spectrometer), or the like. In the invention, organic solvent is adopted for extraction, namely nicotine in tobacco products is extracted, and the extract obtained after extraction is the extract.
If an organic solvent is directly adopted instead of water when the nicotine is dissolved in the tobacco products, the supernatant in the organic extraction liquid can be directly extracted for chromatographic analysis without adding another organic solvent. However, the conventional organic solvent such as isopropanol cannot sufficiently extract nicotine in tobacco, because nicotine in tobacco products exists in both a bound state and a free state, and part of the bound nicotine cannot be directly extracted by the organic solvent. The inventor finds that the methanol has strong polarity and can extract nicotine in tobacco to a greater extent; however, the accuracy and precision of the detection only by methanol extraction still cannot be broken through. Through a plurality of experiments and researches of the inventor, the extraction efficiency of the nicotine is greatly improved when triethylamine is added into the methanol solution. Meanwhile, triethylamine is adopted to replace sodium hydroxide with strong corrosivity, so that the tobacco products are prevented from being corroded, and the determination result of nicotine is more accurate. In addition, the invention adopts a one-step extraction mode, thereby greatly reducing the complexity of the operation, and no water is added in the extraction process, thereby not damaging the gas chromatographic column.
For the detection method, the volume ratio concentration of triethylamine in the methanol solvent is not required to be very high, the effective extraction of nicotine in tobacco products can be ensured only by controlling the concentration to be 1-10%, the usage amount of triethylamine is reduced, and raw materials are saved. Moreover, triethylamine has toxicity, and experimental personnel can be protected from being injured by controlling the concentration of triethylamine.
Further, when the volume ratio concentration of triethylamine in the methanol solvent is 4%, the extraction effect is best.
In the invention, the nicotine concentration in the extract can be measured by adopting an external standard method or an internal standard method.
In another embodiment of the invention, the nicotine concentration is determined by internal standard method. The methanol solution contains internal standards such as 2-methylquinoline, quinoline, n-heptadecane, etc. Preferably, the internal standard is 2-methylquinoline. Preferably, the concentration of 2-methylquinoline is from 0.1mg/mL to 1 mg/mL. More preferably, the concentration of 2-methylquinoline is 0.5 mg/mL.
In one embodiment of the invention, after the organic solvent and the tobacco product are mixed, the mixture is oscillated or ultrasonically treated and then kept stand to obtain extract liquid; wherein, the oscillation or ultrasonic time is preferably 0.5h to 6h, and more preferably 3 h; the time for standing is preferably 2 to 30min, more preferably 10 min. The dissolution of nicotine in the organic solvent of the present invention can be further promoted by shaking or sonication of the mixture.
The tobacco product of the present invention may be a conventional cigarette, a heat non-combustible tobacco product, a smokeless tobacco product, a tobacco leaf, or a smoked cigarette filter. It is particularly useful for the detection of nicotine in heat-not-burn tobacco products, because they contain an atomizing agent such as 1, 2-propanediol, glycerol, etc. In the prior art, when the nicotine content in a heated non-combustible tobacco product is detected, the detection result is greatly influenced by an atomizing agent, so that the detection result is inaccurate and the accuracy is poor. The detection method provided by the invention is not interfered by the atomizing agent, and the detection result is more accurate.
The moisture content in the heated non-combustible tobacco product not only affects the wrapping of the tobacco product, but also directly affects the sensory quality of the heated non-combustible tobacco product, such as the first bite smoke temperature. High content of 1, 2-propylene glycol or glycerol is often required to be added into tobacco products as an atomizing agent, and the type and content of the atomizing agent can directly influence the smoke generation effect and sensory quality. Therefore, the accurate and rapid determination of the moisture, 1, 2-propylene glycol, glycerol and total nicotine content in the non-combustible heating tobacco product has important significance for the research and development of the non-combustible heating tobacco product and the control of the product quality.
Due to the different properties of moisture, nebulant and nicotine, moisture, 1, 2-propanediol and glycerol, nicotine are individually detected by several independent analytical methods in the traditional method. For example, specific solvents and methods are selected for extracting and detecting water, atomizing agent and nicotine in tobacco products respectively. For example, in conventional nicotine assay methods, a two-step extraction method is used, in which the tobacco product is first soaked with a high-concentration aqueous solution of sodium hydroxide, and the organic phase obtained by extraction with n-hexane or methyl t-butyl ether is subjected to gas chromatography in the second step. The traditional nicotine determination method can only be used for detecting nicotine, and can not effectively extract and detect the atomizing agent in the tobacco products, because the sodium hydroxide solution for extracting the nicotine reacts with 1, 2-propylene glycol and glycerol, thereby influencing the determination of the 1, 2-propylene glycol and the glycerol. For detection of 1, 2-propanediol and glycerol as the atomizing agents, the tobacco products are generally weighed separately and added with an organic solvent for extraction and detection. The detection of water content and nicotine in tobacco products requires extraction with different solvents respectively. This adds difficulty and cost to the analysis. The above-mentioned substances to be detected are intended to be extracted simultaneously by a one-step method, but there are problems that the extraction is incomplete and that the solvent or the substances to be detected affect each other. The extraction of water, 1, 2-propanediol and glycerol with organic solvents is attempted at the same time, but the extraction of nicotine is often not effective. This is because nicotine in tobacco products exists in both bound and free forms, and some of the bound nicotine cannot be extracted directly by organic solvents.
The inventors found that methanol has strong polarity, and can extract water and 1, 2-propanediol and glycerol at the same time, but the effect of extracting nicotine is not good. In an attempt to improve the extraction of nicotine in tobacco products by adding alkaline substances such as sodium hydroxide, ammonia water and the like into methanol, the alkaline substances such as sodium hydroxide, ammonia gas and the like are found to react with 1, 2-propylene glycol and glycerol, so that the extraction of 1, 2-propylene glycol and glycerol is inaccurate, and the detection of the content of 1, 2-propylene glycol and glycerol is greatly influenced. The inventor finds through research and experiments that when triethylamine is added into a methanol solution, the triethylamine can not only completely extract free nicotine and bound nicotine, but also effectively extract moisture in tobacco products without reaction with 1, 2-propylene glycol and glycerol to interfere the content detection. The tobacco product is treated by a methanol organic solvent containing triethylamine, and the obtained extracting solution contains water, 1, 2-propylene glycol, glycerol and nicotine, and the extracting solution does not generate test influence mutually. After extraction, the extract liquid is taken out in a targeted manner and is respectively subjected to gas chromatography detection, so that the content of water, 1, 2-propylene glycol, glycerol and nicotine in the tobacco product is analyzed by a one-step method.
Specifically, the method for simultaneously measuring the contents of water, 1, 2-propylene glycol, glycerol and nicotine in tobacco comprises the following steps:
mixing an organic solvent with a volume of V with a tobacco product with a mass of m, and extracting water, 1, 2-propylene glycol, glycerol and nicotine in the tobacco product to obtain an extract liquid, wherein the organic solvent is a methanol solvent containing triethylamine; taking the extract as a first detection solution, and analyzing the water content of the first detection solution by adopting a gas chromatography to obtain the concentration of water in the first detection solution; taking the extract as a second detection solution, and analyzing the content of 1, 2-propylene glycol, glycerol and nicotine in the second detection solution by gas chromatography to obtain the concentration of 1, 2-propylene glycol, glycerol and nicotine in the second detection solution; and respectively calculating the water content, the 1, 2-propylene glycol content, the glycerol content and the nicotine content in the tobacco product according to V, m and the obtained water, 1, 2-propylene glycol, glycerol and nicotine concentrations. In the invention, organic solvent is adopted for extraction, namely nicotine in tobacco products is extracted, and the extract obtained after extraction is the extract.
The method can simultaneously determine the contents of water, 1, 2-butanediol, glycerol and nicotine in the tobacco products, remarkably simplify the detection flow, reduce the analysis cost and improve the detection efficiency. Meanwhile, the methanol solution containing triethylamine is used for extracting the tobacco products, and the alkalinity of the triethylamine can fully neutralize acidic substances in the tobacco products, so that free nicotine and combined nicotine are completely extracted, and the accuracy of nicotine measurement is improved. Meanwhile, the triethylamine methanol solution can not adsorb nicotine in tobacco products, so that the accuracy of nicotine measurement is further improved, and the extraction of water and the atomizing agent can not be influenced. In addition, the invention also adopts a one-step extraction mode, thereby greatly reducing the complexity of the operation, and the addition of water is avoided in the extraction process, so that the gas chromatographic column is not damaged, and meanwhile, the operation steps can be reduced by adopting the one-step extraction method, thereby reducing the loss of nicotine in the extraction operation and further improving the accuracy of nicotine determination.
Further, the inventor finds that for the detection method of the invention, the volume ratio concentration of triethylamine in the methanol solution does not need to be very high, the effective extraction of nicotine in tobacco products can be ensured only by controlling the concentration to be 1-10%, the usage amount of triethylamine can be reduced, raw materials can be saved, and the detection of the content of 1, 2-propylene glycol and glycerol can not be influenced. Moreover, triethylamine has toxicity, and experimental personnel can be protected from being injured by controlling the concentration of triethylamine.
Further, when the volume ratio concentration of triethylamine in the methanol solvent is 4%, the extraction efficiency of nicotine is the best, and the content determination of 1, 2-propylene glycol and glycerol is not influenced.
In the invention, the concentrations of water, 1, 2-butanediol, glycerol and nicotine in the extract can be measured by adopting an external standard method or an internal standard method.
In another embodiment of the invention, the concentrations of water, 1, 2-butanediol, glycerol and nicotine were determined using internal standards. The methanol solution contains internal standards such as 2-methylquinoline, quinoline, n-heptadecane, etc. Preferably, 1, 4-butanediol is used as an internal standard substance for detecting moisture, 1, 4-butanediol can also be used as an internal standard substance for 1, 2-propanediol and glycerol, and 2-methylquinoline is used as an internal standard substance for nicotine. The concentration of the 1, 4-butanediol is 0.5 mg/mL-10 mg/mL, and the concentration of the 2-methylquinoline is 0.1 mg/mL-1 mg/mL. More preferably, the concentration of 1, 4-butanediol is 3mg/mL and the concentration of 2-methylquinoline is 0.5 mg/mL.
In another embodiment of the invention, after the organic solvent and the tobacco product are mixed, the mixture is oscillated or ultrasonically treated and then kept stand to obtain the extract liquid; wherein, the oscillation or ultrasonic time is preferably 0.5h to 6h, and more preferably 3 h; the time for standing is preferably 2 to 30min, more preferably 10 min. The mixture is subjected to vibration or ultrasonic treatment to further promote the dissolution of water, 1, 2-propanediol, glycerol and nicotine in the organic solvent of the present invention.
The tobacco product of the present invention may be a conventional cigarette, a heat non-combustible tobacco product, a smokeless tobacco product, a tobacco leaf, or a smoked cigarette filter. It is particularly useful for the detection of nicotine in heat-not-burn tobacco products, because they contain an atomizing agent such as 1, 2-propanediol, glycerol, etc. In the prior art, when the nicotine content in a heated non-combustible tobacco product is detected, the detection result is greatly influenced by an atomizing agent, so that the detection result is inaccurate and the accuracy is poor. The detection method provided by the invention is not interfered by the atomizing agent, and the detection result is more accurate.
In another embodiment of the present invention, the assay method comprises the following steps
1) Preparing an organic solvent: accurately weighing a certain amount of triethylamine, 1, 4-butanediol and 2-methylquinoline respectively, and metering the volume to a certain volume by using methanol to ensure that the concentration of the triethylamine is a11, 4-butanediol concentration of a2The concentration of 2-methylquinoline is a3. Wherein, 1, 4-butanediol is used as an internal standard of water, 1, 2-propanediol and glycerol, and 2-methylquinoline is used as an internal standard of nicotine.
2) Sample pretreatment: weighing a tobacco product with the mass m, adding an organic solvent with the volume V, oscillating or ultrasonically extracting for a certain time t, standing for a certain time, taking supernate, filtering, and then carrying out GC-FID and GC-TCD analysis. The quality of the tobacco product and the volume of the organic solvent can be selected according to the requirements of detection volume and the like, and the organic solvent has higher solubility to nicotine, so that the nicotine can be fully dissolved. For example, the volume of organic solvent is selected such that the smoking article is submerged.
3) Analyzing by an instrument: analyzing the clear liquid by GC-FID (gas chromatography-hydrogen flame ion detector) or GC-MS (gas chromatography-mass spectrometer) to obtain the concentrations of 1, 2-propylene glycol, glycerol and nicotine in the extract; analyzing the clear liquid by GC-TCD (gas chromatography-thermal conductivity detector) to obtain water concentration in the extractive solution, wherein the water concentration, 1, 2-propylene glycol, glycerol and nicotine concentration in the extractive solution are ci(mg/mL)。
The moisture, 1, 2-propanediol, glycerol and nicotine content in the tobacco is:
in the formula: xiThe content of moisture, 1, 2-propylene glycol, glycerol and nicotine in the tobacco is mg/g;
cithe content of water, 1, 2-propylene glycol, glycerol and nicotine in the extract is mg/mL;
v is the volume of the extraction liquid, and the unit is mL;
m is the tobacco mass in g.
The present invention is further illustrated below with reference to specific examples, which are intended to be illustrative only and not to limit the scope of the invention.
Example 1
1. Preparation of extract liquor
6.0000g of 1, 4-butanediol and 1.0000g of 2-methylquinoline are weighed out accurately, 80mL of triethylamine is weighed out, dissolved in 100mL of methanol, transferred to a 2L volumetric flask, and then the volume is determined with methanol.
2. Sample extraction
Accurately weighing 1.0000g of No. 1 tobacco product, adding 50mL of extract, shaking for extraction for 3h, standing for 10min, collecting supernatant, filtering with 0.45 μm organic filter membrane, and filling into chromatographic flask for detection.
3. Instrumental analysis
A system A is used for measuring water content, a chromatographic column is a DB-ALC (30m × 0.32.32 mm,1 mu m) capillary column, a detector is a TCD detector, a system B is used for measuring 1, 2-propylene glycol, glycerol and nicotine, the chromatographic column is a DB-ALC (30m × 0.32.32 mm,1 mu m) capillary column, the detector is a FID detector, the temperature programming is that the temperature is increased to 150 ℃ at the temperature of 10 ℃/min after being kept for 1min, the temperature is increased to 220 ℃ at the temperature of 30 ℃/min after being kept for 5 min.
System a conditions: sample inlet temperature: 150 ℃; carrier gas: he, 1.5 mL/min; sample introduction volume: 1 mu L of the solution; sample introduction mode: no shunt sampling; detector temperature: 250 ℃; b, system conditions: sample inlet temperature: 250 ℃; carrier gas: he, 3 mL/min; sample introduction volume: 1 mu L of the solution; sample introduction mode: split-flow sample introduction, split-flow ratio: 50: 1; tail blowing: n is a radical of230 mL/min; detector temperature: 275 ℃; h2：30mL/min，N2：400mL/min。
Comparative example 1 the water, 1, 2-propanediol, glycerol and nicotine contents of No. 1 tobacco product were measured by the prior art method, wherein the prior water content measurement method is different from the method of the present invention in that after No. 1 tobacco product was extracted with a methanol solution containing an internal standard isopropanol to obtain an extract, the water content of No. 1 tobacco product was measured by the same instrumental analysis method as in example 1; the existing detection method of 1, 2-propanediol is different from the method of the invention in that after the No. 1 tobacco product is extracted by using a methanol solution containing an internal standard substance of 1, 4-butanediol to obtain an extract liquid, the content of 1, 2-propanediol in the No. 1 tobacco product is detected by using the same instrument analysis method as the embodiment 1; the existing detection method of glycerol is different from the method of the invention in that after the No. 1 tobacco product is extracted by using a methanol solution containing an internal standard substance 1, 4-butanediol to obtain an extract liquid, the content of glycerol in the No. 1 tobacco product is detected by using the same instrument analysis method as the embodiment 1; the difference between the existing nicotine detection method and the method of the invention is that 7mol/L sodium hydroxide solution is used for soaking the No. 1 tobacco product, methyl tert-butyl ether containing internal standard 2-methylquinoline is added for extraction, and the nicotine content in the No. 1 tobacco product is detected by the same instrument analysis method as the embodiment 1 after the extract liquid is obtained.
Example 2
Taking the No. 2 tobacco product, the detection method is the same as that in the example 1, and the difference is that the contents of water, 1, 2-propylene glycol, glycerol and nicotine in the No. 2 tobacco product and the No. 1 tobacco product are different.
Comparative example 2 tobacco product No. 2 was tested for water, 1, 2-propanediol, glycerol, and nicotine content using the method of comparative example 1.
Example 3
Taking No. 3 tobacco product, the detection method is the same as that of example 1, and the difference is that the contents of water, 1, 2-propylene glycol, glycerol and nicotine in No. 3 tobacco product and No. 1 tobacco product are different.
Comparative example 3 tobacco product No. 3 was tested for water, 1, 2-propanediol, glycerol, and nicotine content using the method of comparative example 1.
Example 4
Taking No. 4 tobacco product, the detection method is the same as that of example 1, and the difference is that the contents of water, 1, 2-propylene glycol, glycerol and nicotine in No. 4 tobacco product and No. 1 tobacco product are different.
Comparative example 4 tobacco product No. 4 was tested for water, 1, 2-propanediol, glycerol, and nicotine content using the method of comparative example 1.
Example 5
The detection method of the No. 5 tobacco product is the same as that of the example 1, and the difference is that the No. 5 tobacco product and the No. 1 tobacco product have different contents of nicotine, water, 1, 2-propylene glycol and glycerol.
Comparative example 5 tobacco product No. 5 was tested for water, 1, 2-propanediol, glycerol, and nicotine content using the method of comparative example 1.
Example 6
Taking No. 6 tobacco product, the detection method is the same as that of example 1, and the difference is that the contents of water, 1, 2-propylene glycol, glycerol and nicotine in No. 6 tobacco product and No. 1 tobacco product are different.
Comparative example 6 tobacco product No. 6 was tested for water, 1, 2-propanediol, glycerol, and nicotine content using the method of comparative example 1.
After 6 detections were performed according to the detection methods of examples 1 to 6 and comparative examples 1 to 6, respectively, the calculated detection values and error values are shown in table 1. The method can realize the simultaneous extraction of the water, the 1, 2-propylene glycol, the glycerol and the nicotine by adopting a one-step extraction method, and compared with the existing methods for respectively extracting and detecting, the method can also achieve the results of small error of the measurement result and accurate nicotine determination result, and even can be better than the existing detection result in the aspects of accuracy and precision.
TABLE 1
Comparative example 7 the nicotine content was measured by the conventional method for measuring nicotine, 1, 2-propanediol and glycerol, which is different from the method of the present invention in that the sample solution obtained by extracting No. 1 tobacco product with methanol solution containing 2-methylquinoline as an internal standard was used, and the nicotine content in No. 1 tobacco product was measured by the same instrumental analysis method as in example 1.
Comparative example 8 the nicotine content of tobacco product No. 2 was determined using the method of comparative example 7.
Comparative example 9 the nicotine content of tobacco product No. 3 was determined using the method of comparative example 7.
Comparative example 10 the nicotine content of tobacco product No. 4 was determined using the method of comparative example 7.
Comparative example 11 the nicotine content of tobacco product No. 5 was determined using the method of comparative example 7.
Comparative example 12 the nicotine content of tobacco product No. 6 was determined using the method of comparative example 7.
After 6 detections were performed according to the detection methods of comparative examples 7 to 12, the calculated detection values and error values are shown in table 2. Compared with the method for extracting nicotine by directly using methanol for detection in the prior art, the nicotine detection method adopted by the invention can extract more nicotine, the result of nicotine determination is more accurate, and even the accuracy of the method is better than that of the nicotine detection method.
TABLE 2
| Index (I) | Nicotine content/(mg/g) ± error value/(mg/g) |
| Comparative example 7 | 0.68±0.01 |
| Comparative example 8 | 1.38±0.02 |
| Comparative example 9 | 1.55±0.02 |
| Comparative example 10 | 1.40±0.01 |
| Comparative example 11 | 2.61±0.02 |
| Comparative example 12 | 1.50±0.02 |
Example 7
Taking No. 7 tobacco product, the detection method is the same as that of example 1, and the difference is that the contents of water, 1, 2-propylene glycol, glycerol and nicotine in No. 7 tobacco product and No. 1 tobacco product are different.
The test method of comparative example 13 replaced the methanol solvent in example 7 with ethanol.
The test method of comparative example 14 replaced the methanol solvent of example 7 with isopropanol.
The detection methods according to the methods of example 7 and comparative examples 13 and 14 were carried out 6 times of detection, and the calculated detection values and error values are shown in table 3. It can be seen that the methanol used in the present invention as an organic solvent can extract more water, 1, -2 propylene glycol, glycerol and nicotine in the tobacco product than ethanol or isopropanol, so that the detected water, 1, -2 propylene glycol, glycerol and nicotine content is more accurate and even more precise.
TABLE 3
EXAMPLE 8 determination of working Curve, detection Limit and quantification Limit of the detection method
Triethylamine-methanol is used as a solvent, series of standard solutions of water, 1, 2-propylene glycol, glycerol and nicotine with different concentrations are prepared respectively, GC analysis is carried out respectively under the conditions of the instruments, the water is detected by a TCD detector, and the 1, 2-propylene glycol, the glycerol and the nicotine are detected by an FID detector. Then, internal standard method is adopted for quantification (the internal standard of water, 1, 2-propylene glycol and glycerol is 1, 4-butanediol, the internal standard of nicotine is quinoline), the peak area ratio of each target and the internal standard thereof is used as a vertical coordinate (Y), the concentration of each target is used as a horizontal coordinate (X, mg/mL), regression analysis is carried out, and regression equations and relevant coefficients of water, 1, 2-propylene glycol, glycerol and nicotine are obtained, and are shown in Table 4. As can be seen from Table 4, the linear relationship among the standard curves for moisture, 1, 2-propanediol, glycerol and nicotine is good, and r is2Between 0.9997 and 1.0000. Diluting the standard solution with lowest concentration, performing GC analysis, and determining LOD and LOQ of water, 1, 2-propylene glycol, glycerol and nicotine by using 3 times of signal-to-noise ratio as detection Limit (LOD) and 10 times of signal-to-noise ratio as quantification Limit (LOQ)0.01 to 0.04 percent and 0.03 to 0.14 percent respectively. The method has higher sensitivity and is suitable for quantitative analysis of moisture, 1, 2-propylene glycol, glycerol and nicotine in the tobacco products.
TABLE 4
Example 9 recovery and precision
1.0g of tobacco products with known moisture, 1, 2-propylene glycol, glycerol and nicotine content are taken, standard solutions are added to the tobacco products according to 3 addition levels of low, medium and high, then the tobacco products are processed according to the described tobacco product pretreatment method, each addition level is measured in parallel for 6 times, the recovery rate and the precision are measured, and the experimental results are shown in Table 5. As can be seen from Table 5, the average normalized recovery of water, 1, 2-propanediol, glycerol and nicotine was 91.1% to 99.8%, and the average relative standard deviation (RSD%) was 0.1% to 5.4%, which satisfied the quantitative requirement.
TABLE 5
While the invention has been described with reference to certain preferred embodiments thereof, it will be understood by those skilled in the art that the foregoing is a more particular description of the invention than is possible with reference to the specific embodiments, which are not to be construed as limiting the invention. Various changes in form and detail, including simple deductions or substitutions, may be made by those skilled in the art without departing from the spirit and scope of the invention.
Claims (18)
1. The method for measuring the nicotine content in the tobacco product is characterized by comprising the following steps of:
selecting an organic solvent with the volume of V to be mixed with a tobacco product with the mass of m, and extracting nicotine in the tobacco product to obtain an extract liquid, wherein the organic solvent is a methanol solvent containing triethylamine;
analyzing the nicotine content of the extract by adopting a gas chromatography to obtain the nicotine concentration in the extract;
calculating the nicotine content in the tobacco product according to the V, the m and the obtained nicotine concentration.
2. The assay method according to claim 1, wherein the concentration of the triethylamine in the methanol solvent is 1% to 10% by volume.
3. The assay of claim 2, wherein the triethylamine is present in the methanol solvent at a concentration of 4% by volume.
4. The assay of any one of claims 1 to 3, wherein the nicotine concentration in the extract is chromatographed using an internal standard, wherein the internal standard is 2-methylquinoline.
5. The method according to claim 4, wherein the concentration of 2-methylquinoline is 0.1mg/mL to 1 mg/mL.
6. The assay of claim 5, wherein the concentration of 2-methylquinoline is 0.5 mg/mL.
7. The assay of any one of claims 1 to 3, wherein the organic solvent is mixed with the tobacco product, shaken or sonicated, and then allowed to stand to obtain the extract.
8. The method of claim 7, wherein the shaking or sonication time is 3 hours and the resting time is 10 min.
9. The assay of any one of claims 1 to 3, wherein the tobacco product is a heat-not-burn tobacco product.
10. The method for simultaneously measuring the contents of water, 1, 2-propylene glycol, glycerol and nicotine in the tobacco products is characterized by comprising the following steps of:
mixing an organic solvent with a volume of V with a tobacco product with a mass of m, and extracting water, 1, 2-propylene glycol, glycerol and nicotine in the tobacco product to obtain an extract liquid, wherein the organic solvent is a methanol solvent containing triethylamine;
taking the extract as a first detection liquid, and analyzing the water content of the first detection liquid by adopting a gas chromatography to obtain the concentration of water in the first detection liquid;
taking the extract as a second detection solution, and analyzing the content of 1, 2-propylene glycol, glycerol and nicotine in the second detection solution by adopting a gas chromatography to obtain the concentration of 1, 2-propylene glycol, glycerol and nicotine in the second detection solution;
and calculating the water content, the 1, 2-propylene glycol content, the glycerol content and the nicotine content in the tobacco product according to the V, the m and the obtained concentrations of the water, the 1, 2-propylene glycol, the glycerol and the nicotine.
11. The method of claim 10, wherein the triethylamine is present in the methanol solvent at a concentration of 1% to 10% by volume.
12. The method of claim 11, wherein the triethylamine is present in the methanol solvent at a concentration of 4% by volume.
13. The method of any one of claims 10-12, wherein the concentrations of water, 1, 2-propanediol, glycerol, and nicotine in the extract are chromatographed using an internal standard method, wherein the internal standard comprises 1, 4-butanediol and 2-methylquinoline.
14. The method of claim 13, wherein the 1, 4-butanediol is present at a concentration of 0.5mg/mL to 10mg/mL and the 2-methylquinoline is present at a concentration of 0.1mg/mL to 1 mg/mL.
15. The method according to claim 14, wherein the concentration of 1, 4-butanediol is 3mg/mL and the concentration of 2-methylquinoline is 0.5 mg/mL.
16. The method according to any one of claims 10 to 12, wherein the organic solvent is mixed with the tobacco product, subjected to shaking or sonication, and then allowed to stand, and the supernatant is taken to obtain the extract.
17. The method of claim 16, wherein the shaking or sonication time is 3 hours and the resting time is 10 min.
18. The method of any one of claims 10 to 12, wherein the tobacco product is a heat-not-burn tobacco product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010376686.XA CN111337603A (en) | 2020-05-07 | 2020-05-07 | Method for measuring nicotine content in tobacco product and method for simultaneously measuring water, 1, 2-propylene glycol, glycerol and nicotine content |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010376686.XA CN111337603A (en) | 2020-05-07 | 2020-05-07 | Method for measuring nicotine content in tobacco product and method for simultaneously measuring water, 1, 2-propylene glycol, glycerol and nicotine content |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111337603A true CN111337603A (en) | 2020-06-26 |
Family
ID=71184880
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010376686.XA Pending CN111337603A (en) | 2020-05-07 | 2020-05-07 | Method for measuring nicotine content in tobacco product and method for simultaneously measuring water, 1, 2-propylene glycol, glycerol and nicotine content |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111337603A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112505227A (en) * | 2020-12-29 | 2021-03-16 | 广西中烟工业有限责任公司 | Analysis method for simultaneously determining 11 components in electronic cigarette liquid |
| CN114062579A (en) * | 2021-11-13 | 2022-02-18 | 红云红河烟草(集团)有限责任公司 | Parallel detection device for gas chromatograph and cigarette total particulate matter determination method |
| CN115201351A (en) * | 2021-04-14 | 2022-10-18 | 湖南中烟工业有限责任公司 | Sample preparation and detection method for measuring fogging agent in tobacco and tobacco products |
| CN115201345A (en) * | 2021-04-12 | 2022-10-18 | 湖南中烟工业有限责任公司 | Sample pretreatment and detection method for moisture and/or nicotine in tobacco and tobacco products |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104655766A (en) * | 2015-03-20 | 2015-05-27 | 中国烟草总公司郑州烟草研究院 | Method for simultaneously determining nicotine, propylene alcohol and glycerin in electronic cigarette liquid |
| CN108776184A (en) * | 2018-06-13 | 2018-11-09 | 湖北中烟工业有限责任公司 | A method of cigarette smoke component of not burning is heated in detection |
-
2020
- 2020-05-07 CN CN202010376686.XA patent/CN111337603A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104655766A (en) * | 2015-03-20 | 2015-05-27 | 中国烟草总公司郑州烟草研究院 | Method for simultaneously determining nicotine, propylene alcohol and glycerin in electronic cigarette liquid |
| CN108776184A (en) * | 2018-06-13 | 2018-11-09 | 湖北中烟工业有限责任公司 | A method of cigarette smoke component of not burning is heated in detection |
Non-Patent Citations (6)
| Title |
|---|
| 张丽 等: "气相色谱法测定新型卷烟气溶胶中水、烟碱、1,2-丙二醇和丙三醇的含量", 《理化检验(化学分册)》 * |
| 温光和 等: "加热不燃烧卷烟烟草材料中1,2-丙二醇、丙三醇和烟碱的测定", 《中国烟草科学》 * |
| 王康 等: "GC-TCD法同时检测加热不燃烧卷烟气溶胶水分,及烟碱、丙三醇、1,2-丙二醇、三乙酸甘油酯和薄荷醇的释放量", 《烟草科技》 * |
| 王维维 等: "气相色谱法同时测定烟草中水分及1,2-丙二醇与丙三醇的含量", 《贵州农业科学》 * |
| 肯生叶 等: "GC-TCD法同时检测加热不燃烧卷烟烟草材料中的水分、1,2-丙二醇、烟碱和丙三醇", 《烟草科技》 * |
| 韩冰 等: "卷烟主流烟气中挥发和半挥发性成分分析", 《烟草科技》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112505227A (en) * | 2020-12-29 | 2021-03-16 | 广西中烟工业有限责任公司 | Analysis method for simultaneously determining 11 components in electronic cigarette liquid |
| CN115201345A (en) * | 2021-04-12 | 2022-10-18 | 湖南中烟工业有限责任公司 | Sample pretreatment and detection method for moisture and/or nicotine in tobacco and tobacco products |
| CN115201351A (en) * | 2021-04-14 | 2022-10-18 | 湖南中烟工业有限责任公司 | Sample preparation and detection method for measuring fogging agent in tobacco and tobacco products |
| CN114062579A (en) * | 2021-11-13 | 2022-02-18 | 红云红河烟草(集团)有限责任公司 | Parallel detection device for gas chromatograph and cigarette total particulate matter determination method |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111337603A (en) | Method for measuring nicotine content in tobacco product and method for simultaneously measuring water, 1, 2-propylene glycol, glycerol and nicotine content | |
| CN110208414B (en) | Analysis method for quantitatively determining more than target flavor components in tobacco | |
| CN102012407B (en) | Method for detecting tobacco-specific nitrosamines | |
| CN107764917B (en) | Method for determining key volatile components in cigarette blasting beads | |
| CN109085270A (en) | Method that is a kind of while measuring a variety of tobacco-specific nitrosamines in human plasma | |
| Zhang et al. | Fully automated analysis of four tobacco-specific N-nitrosamines in mainstream cigarette smoke using two-dimensional online solid phase extraction combined with liquid chromatography–tandem mass spectrometry | |
| CN108303477B (en) | Method for detecting alcohols and other compounds in mainstream smoke of cigarette without burning during heating | |
| CN102353741A (en) | Method for measuring contents of four kinds of tobacco-specific nitrosamines in cigarette mainstream smoke | |
| CN104614466A (en) | Method for measuring preservatives in tobacco juice of electronic cigarettes | |
| CN104807906A (en) | Method for detecting piperazine residue in poultry with high efficiency | |
| CN104142374A (en) | Method for measuring content of carbonyl compound in electronic tobacco juice by adopting direct derivation/high performance liquid chromatography | |
| Cho et al. | Use of a gas-tight syringe sampling method for the determination of tobacco-specific nitrosamines in E-cigarette aerosols by liquid chromatography-tandem mass spectrometry | |
| CN103558319B (en) | Method for measuring methyl eugenol in mainstream smoke of cigarettes | |
| CN106442753B (en) | A kind of method of TSNAs content in measurement cigarette mainstream flue gas | |
| CN112578069A (en) | Analysis method for simultaneously measuring 11 components in electronic smoke sol | |
| CN102331462B (en) | Method for measuring ammonia content in water base adhesive for tobaccos | |
| CN108931596A (en) | Method that is a kind of while detecting acetic acid and nicotine in cigarette mainstream flue gas | |
| CN114577915A (en) | Method for measuring free-state and proton-state nicotine content in tobacco juice | |
| CN112505227A (en) | Analysis method for simultaneously determining 11 components in electronic cigarette liquid | |
| CN103149297B (en) | High performance liquid chromatography-mass spectrum-mass spectrum (HPLC-MS-MS) combined detection method for (S)-NNAL and (R)-NNAL in urine | |
| CN109975443B (en) | Method for detecting aldehydes in cigarette filter | |
| CN111650189A (en) | Method for measuring content of formaldehyde in special slice for cigarette without burning during heating | |
| CN111855866A (en) | Method for rapidly determining formaldehyde in tobacco additive | |
| CN111983111B (en) | Method for measuring retention rate of cigarette filter stick on hydroxypyridine | |
| CN111337604A (en) | Method for measuring nicotine content in tobacco product |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20200626 |