CN104764851A - Method for measuring sixteen polycyclic aromatic hydrocarbons in cigarette liquid of electronic cigarette - Google Patents
Method for measuring sixteen polycyclic aromatic hydrocarbons in cigarette liquid of electronic cigarette Download PDFInfo
- Publication number
- CN104764851A CN104764851A CN201510233951.8A CN201510233951A CN104764851A CN 104764851 A CN104764851 A CN 104764851A CN 201510233951 A CN201510233951 A CN 201510233951A CN 104764851 A CN104764851 A CN 104764851A
- Authority
- CN
- China
- Prior art keywords
- kinds
- liquid
- sample
- palycyclic
- preparation
- 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.)
- Granted
Links
Landscapes
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention provides a method for measuring sixteen polycyclic aromatic hydrocarbons in cigarette liquid of an electronic cigarette. The method is characterized in that a small amount of water is added to a cigarette liquid sample of the electronic cigarette, a mixture vibrates evenly, so that the mixture is fully dispersed in a kieselguhr solid phase supporting liquid-liquid extraction column, cyclohexane is used for extraction, and after extraction liquid is concentrated, the sixteen polycyclic aromatic hydrocarbons in the cigarette liquid of the electronic cigarette are measured through a GC-MS. Compared with a commonly-used polycyclic aromatic hydrocarbon analysis method, the method for measuring the sixteen polycyclic aromatic hydrocarbons has the advantages that sample pretreatment is greatly simplified, the use amount of organic solvents is saved, experiment repeatability is good, the experiment recovery rate is high, and the method is suitable for treating samples automatically on a large scale.
Description
Technical field
The invention belongs to tobacco juice for electronic smoke determination techniques field, be specifically related to the assay method of 16 kinds of palycyclic aromatics in a kind of tobacco juice for electronic smoke.The method adds a small amount of water by tobacco juice for electronic smoke sample, shaken well, is well dispersed in zeyssatite solid phase and supports, in liquid-liquid extraction post, to extract with cyclohexane, after extract is concentrated, gas chromatograph-mass spectrometer (GCMS) (GC-MS) is adopted to realize the mensuration of 16 kinds of palycyclic aromatics in tobacco juice for electronic smoke.
Background technology
Electronic cigarette (electrical cigarette, e-cigarette), have another name called electronics nicotine transfer system (electronic nicotine delivery systems, ENDS), being a kind of electronic installation being transmitted nicotine by electrons heat means to respiratory system, is a kind of new paragon sucking nicotine.Tobacco juice for electronic smoke is formed primarily of nicotine, propylene glycol, glycerine or polyglycol, can add a small amount of essence in addition, make different tastes to cater to consumer demand and hobby.
Palycyclic aromatic is the staying quality poison material of a quasi-representative, has carcinogenic, teratogenesis and mutagenicity.The Polycyclic aromatic hydrocarbons and Derivatives found at present is more than 400 kinds, and wherein 16 kinds of palycyclic aromatics are classified as the organic contaminant of priority acccess control by Environmental Protection Agency (US Environmental Protection Agency).These 16 kinds of palycyclic aromatics are common environment and food contaminant, and its carcinogenicity is comparatively strong, even trace, still the health of the mankind in serious threat.But its assay in tobacco juice for electronic smoke, rarely has report.
At present, analyze the pre-treatment detecting palycyclic aromatic and mostly adopt solid phase extraction (Solid-Phase Extraction), its process is divided into the steps such as activation, drip washing, wash-out, loaded down with trivial details consuming time.Because tobacco juice for electronic smoke matrix is comparatively simple and be mainly polar component, pre-treatment of the present invention adopts solid phase to support liquid-liquid technique (Supported Liquid Extraction), for a kind of novel liquid-liquid extracting process, it is on the basis of traditional liquid-liquid extraction, be medium by a kind of inertia porous mass-calcined diatomite, when aqueous samples is through later, tripolite filling material surface is distributed in the form of liquid film of thin layer, after adding organic solvent, immiscible two-phase extracts and occurs immediately while zeyssatite surface contact, achieve efficient, extraction process fast.
Summary of the invention
The assay method of 16 kinds of palycyclic aromatics in a kind of tobacco juice for electronic smoke provided for above current condition is provided, the method adopts inner mark method ration, liquid-liquid technique makes sample pre-treatments simplify to utilize solid phase to support, accuracy, reproducible, the recovery is high.
The object of the invention is to be realized by following scheme:
The assay method of 16 kinds of palycyclic aromatics in a kind of tobacco juice for electronic smoke, add a small amount of water by tobacco juice for electronic smoke sample, shaken well, being well dispersed in zeyssatite solid phase supports in liquid-liquid extraction post, extract with cyclohexane, after extract is concentrated, adopt gas chromatograph-mass spectrometer (GCMS) (GC-MS) to realize the mensuration of 16 kinds of palycyclic aromatics in tobacco juice for electronic smoke, concrete determination step is as follows:
(1) extraction of testing sample and concentrated: accurately take 0.1 ~ 3 g electronic cigarette liquid in conical flask, add D
8-Nai, D
10-Fei, D
12mark and 0.9 ~ 3 mL water in-benzo [a] pyrene 3 kinds, all proceeding to solid phase after vibration 2 ~ 10 min supports in liquid-liquid extraction post, pressurization makes testing sample solution fully spread in column packing, leave standstill 2 ~ 10 min, add 5 ~ 24 mL cyclohexane wash-outs, collect eluent, be concentrated into about 0.2 ~ 1 mL, detect with GC-MS;
(2) preparation of standard working solution: preparation to have in 16 kinds of palycyclic aromatics of concentration gradient and 3 kinds target cyclohexane solution as hybrid standard working solution;
(3) analysis of sample:
GC-MS analysis condition:
Injector temperature: 280 DEG C; Sample size: 1 μ L; Splitless injecting-Sample; Carrier gas: helium, constant current flow velocity 1mL/min; Chromatographic column: DB-5MS, specification 30m × 0.25mm × 0.25 μm; Temperature programme: 60 DEG C keep 1min, then rise to 110 DEG C with the speed of 20 DEG C/min, then rise to 280 DEG C with the speed of 5 DEG C/min, keep 10min.
Ionization mode: EI; Transmission line temperature: 280 DEG C; Ion source temperature: 230 DEG C.
Scan mode: SIM, Selective ion mode, see table 1, is 50ms to the monitoring time of each ion.
(4) Specification Curve of Increasing and result calculate: carry out area integral to the response of series standard solution, do calibration curve, carry out matching, obtain unary linear regression equation with straight line with the ratio of often kind of palycyclic aromatic and interior target response area comparison content.The sample of preparation is measured, records often kind of palycyclic aromatic in sample and interior mark peak area ratio, bring unary linear regression equation into, calculate often kind of polycyclic aromatic hydrocarbon content.
The preparation method of hybrid standard working solution is as follows:
1) preparation of hybrid standard stock solution: accurately take 10 mg, 16 kinds of palycyclic aromatics respectively in the brown volumetric flask of 100 mL, dissolve constant volume with cyclohexane.The preparation of mark stock solution in mixing: accurately take 10 mg D respectively
8-Nai, D
10-Fei, D
12-benzo [a] pyrene, in the brown volumetric flask of 100 mL, dissolves constant volume with cyclohexane.
2) preparation of hybrid standard working solution: accurately add 5 uL respectively, 10 uL, 20 uL, 40 uL, in 80 uL hybrid standard stock solutions and 40 uL mix, mark stock solution is in 50 mL volumetric flasks, uses cyclohexane constant volume.
In the present invention, the column packing of employing is zeyssatite.
The water adopted is high purity water.
Fully diffusion institute plus-pressure can not more than 10 psi in column packing for sample solution.
Before sample solution extraction, keep sample solution in pillar, can not flow out.
When sample solution wash-out, control the eluent rate of outflow about 2 mL/min(1 drop/sec).
Method of the present invention is utilized to measure target standard article in following 16 kinds of palycyclic aromatics and 3 kinds, its retention time, qualitative, quota ion is as shown in table 1:
Show target mass spectrophotometry parameter in 1:16 kind palycyclic aromatic and 3 kinds
| Compound | Retention time (min) | Qualitative ion | Quota ion |
| D8-naphthalene | 6.74 | 134 | 136 |
| Naphthalene | 6.86 | 129,127 | 128 |
| Acenaphthylene | 11.78 | 151,153 | 152 |
| Acenaphthene | 12.47 | 154,152 | 153 |
| Fluorenes | 14.44 | 165,167 | 166 |
| D10-is luxuriant and rich with fragrance | 18.66 | 184 | 188 |
| Luxuriant and rich with fragrance | 18.71 | 179,176 | 178 |
| Anthracene | 18.93 | 179,176 | 178 |
| Fluoranthene | 24.17 | 200,203 | 202 |
| Pyrene | 25.15 | 200,203 | 202 |
| Benzo [a] anthracene | 30.81 | 229,226 | 228 |
| Bend | 30.87 | 229,226 | 228 |
| Benzo [b] fluoranthene | 35.46 | 253,250 | 252 |
| Benzo [k] fluoranthene | 35.58 | 253,250 | 252 |
| D12-benzo [a] pyrene | 36.50 | 263 | 264 |
| Benzo [a] pyrene | 36.61 | 253,250 | 252 |
| Indenols [1,2,3-cd] pyrene | 41.53 | 277,138 | 276 |
| Dibenzo [a, h] anthracene | 41.78 | 276,139 | 278 |
| Benzo [g, h, i] perylene | 42.77 | 277,138 | 276 |
A certain tobacco juice for electronic smoke sample is added 16 kinds of palycyclic aromatic standard solution of high, medium and low three contents levels, do recovery experiment, the in a few days repeatability of simultaneously carrying out the method measures with repeated in the daytime, and represent by the relative standard deviation (RSD) of measurement result, result is as shown in table 2.Visible, this method repeatability and the recovery very well, are applicable to the analysis of batch samples.
Table 2: the repeatability of method and recovery testing result
| Compound | In RSD(day, %) | Between RSD(day, %) | The recovery (%) |
| Naphthalene | 2.74 | 3.04 | 92.1 |
| Acenaphthylene | 3.21 | 5.03 | 94.2 |
| Acenaphthene | 3.29 | 5.64 | 91.2 |
| Fluorenes | 4.54 | 6.59 | 98.5 |
| Luxuriant and rich with fragrance | 5.21 | 6.29 | 100.2 |
| Anthracene | 6.54 | 7.56 | 100.8 |
| Fluoranthene | 3.71 | 4.94 | 94.5 |
| Pyrene | 3.42 | 5.93 | 92.6 |
| Benzo [a] anthracene | 2.29 | 3.64 | 99.5 |
| Bend | 3.51 | 4.59 | 92.2 |
| Benzo [b] fluoranthene | 2.21 | 3.28 | 98.5 |
| Benzo [k] fluoranthene | 4.54 | 6.52 | 99.2 |
| Benzo [a] pyrene | 2.71 | 4.94 | 99.8 |
| Indenols [1,2,3-cd] pyrene | 3.52 | 5.93 | 94.5 |
| Dibenzo [a, h] anthracene | 2.59 | 3.64 | 92.6 |
| Benzo [g, h, i] perylene | 3.61 | 4.69 | 98.3 |
The present invention, compared with existing detection method, has following technical advantage:
1, solid phase is supported that liquid-liquid technique is applied to the mensuration of 16 kinds of palycyclic aromatics in tobacco juice for electronic smoke by the present invention first, by inertia porous mass-calcined diatomite medium, extraction step only needs a step to complete, for a kind of novel liquid-liquid extracting process, instead of separating funnel, simplify extraction step and emulsion can not occur.Because tobacco juice for electronic smoke principal ingredient is polar solvent, be suitable for solid phase and support liquid-liquid technique, can avoid adopting and measure the conventional solid phase extraction of palycyclic aromatic, eliminate the steps such as loaded down with trivial details activation, drip washing, wash-out, enormously simplify sample pre-treatments, be applicable to the analysis of batch samples, save organic solvent use, more environmental protection simultaneously.
2, this method recovery is between 91.2%-100.8%, and withinday precision is between 2.74%-6.54%, and day to day precision is between 3.04%-7.56%, and the method recovery and reproducible is described, actual application value is high.
Accompanying drawing explanation
Target standard colors spectrogram in Fig. 1: 16 kinds of palycyclic aromatics and 3 kinds,
In figure: 1-D
8-naphthalene; 2-naphthalene; 3-acenaphthylene; 4-acenaphthene, 5-fluorenes, 6-D
10-Fei, 7-luxuriant and rich with fragrance, 8-anthracene, 9-fluoranthene, 10-pyrene, 11-benzo [a] anthracene, 12-bend, 13-benzo [b] fluoranthene, 14-benzo [k] fluoranthene, 15-D
12-benzo [a] pyrene, 16-benzo [a] pyrene, 17-indenols-[1,2,3-cd] pyrene, 18-dibenzo [a, h] anthracene, 19-benzo [g, h, i] perylene.
Fig. 2: the chromatogram of tobacco juice for electronic smoke A,
In figure: 1-D
8-naphthalene; 2-naphthalene; 3-D
10-Fei, 4-luxuriant and rich with fragrance, 5-fluoranthene, 6-pyrene.
Embodiment
Below by embodiment, the present invention is further described:
Embodiment 1
1, the extraction of testing sample and concentrated: accurately take about 0.1 g electronic cigarette liquid in conical flask, add D
8-Nai, D
10-Fei, D
12mark and 0.9 mL water in-benzo [a] pyrene, all proceed to solid phase and support that, in liquid-liquid extraction post, pressurization makes testing sample solution fully spread in column packing after 2 min that vibrate, leave standstill 5min, add 5 mL cyclohexane wash-outs, collect eluent, be concentrated into about 0.2 mL, detect with GC-MS;
2, GC-MS analysis condition: injector temperature: 280 DEG C; Sample size: 1 μ L; Splitless injecting-Sample; Carrier gas: helium, constant current flow velocity 1mL/min; Chromatographic column: DB-5MS, specification 30m × 0.25mm × 0.25 μm; Temperature programme: 60 DEG C keep 1min, then rise to 110 DEG C with the speed of 20 DEG C/min, then rise to 280 DEG C with the speed of 5 DEG C/min, keep 10min.Ionization mode: EI; Transmission line temperature: 280 DEG C; Ion source temperature: 230 DEG C.Scan mode: SIM, Selective ion mode, see table 1, is 50ms to the monitoring time of each ion.
3, the preparation method of hybrid standard working solution is: the 1) preparation of hybrid standard stock solution: accurately take 10mg 16 kinds of palycyclic aromatics respectively in the brown volumetric flask of 100mL, dissolve constant volume with cyclohexane.The preparation of mark stock solution in mixing: how accurately take 10mg D8-respectively, D10-is luxuriant and rich with fragrance, and D12-benzo [a] pyrene, in the brown volumetric flask of 100mL, dissolves constant volume with cyclohexane.2) preparation of hybrid standard working solution: accurately add 5 uL respectively, 10 uL, 20 uL, 40 uL, in 80 uL hybrid standard stock solutions and 40 uL mix, mark stock solution is in the brown volumetric flask of 50mL, uses cyclohexane constant volume.
4, Specification Curve of Increasing and result calculate: carry out area integral to the response of series standard solution, do calibration curve, carry out matching, obtain unary linear regression equation, coefficient R with straight line with the ratio of often kind of palycyclic aromatic and interior target response area comparison content
2should 0.999 be not less than.The sample of preparation is measured, records often kind of palycyclic aromatic in sample and interior mark peak area ratio, bring unary linear regression equation into, calculate often kind of polycyclic aromatic hydrocarbon content.
According to the method for the assay method of 16 kinds of palycyclic aromatics in foregoing a kind of tobacco juice for electronic smoke, select a kind of tobacco juice for electronic smoke A, record wherein how, the content of phenanthrene, fluoranthene, pyrene is respectively 35.35 ng/g, 11.87 ng/g, 3.28 ng/g, 2.53 ng/g, as shown in Figure 2, other palycyclic aromatics do not detect.
Embodiment 2
1, the extraction of testing sample and concentrated: accurately take about 3 g electronic cigarette liquids in conical flask, add D
8-Nai, D
10-Fei, D
12mark and 2 mL water in-benzo [a] pyrene, all proceed to solid phase and support that, in liquid-liquid extraction post, pressurization makes testing sample solution fully spread in column packing after 5 min that vibrate, leave standstill 5min, add 24 mL cyclohexane wash-outs, collect eluent, be concentrated into about 1 mL, detect with GC-MS;
2, GC-MS analysis condition: injector temperature: 280 DEG C; Sample size: 1 μ L; Splitless injecting-Sample; Carrier gas: helium, constant current flow velocity 1mL/min; Chromatographic column: DB-5MS, specification 30m × 0.25mm × 0.25 μm; Temperature programme: 60 DEG C keep 1min, then rise to 110 DEG C with the speed of 20 DEG C/min, then rise to 280 DEG C with the speed of 5 DEG C/min, keep 10min.Ionization mode: EI; Transmission line temperature: 280 DEG C; Ion source temperature: 230 DEG C.Scan mode: SIM, Selective ion mode, see table 1, is 50ms to the monitoring time of each ion.
3, the preparation method of hybrid standard working solution is: the 1) preparation of hybrid standard stock solution: accurately take 10mg 16 kinds of palycyclic aromatics respectively in the brown volumetric flask of 100mL, dissolve constant volume with cyclohexane.The preparation of mark stock solution in mixing: how accurately take 10mg D8-respectively, D10-is luxuriant and rich with fragrance, and D12-benzo [a] pyrene, in the brown volumetric flask of 100mL, dissolves constant volume with cyclohexane.2) preparation of hybrid standard working solution: accurately add 5 uL respectively, 10 uL, 20 uL, 40 uL, in 80 uL hybrid standard stock solutions and 40 uL mix, mark stock solution is in the brown volumetric flask of 50mL, uses cyclohexane constant volume.
4, Specification Curve of Increasing and result calculate: carry out area integral to the response of series standard solution, do calibration curve, carry out matching, obtain unary linear regression equation, coefficient R with straight line with the ratio of often kind of palycyclic aromatic and interior target response area comparison content
2should 0.999 be not less than.The sample of preparation is measured, records often kind of palycyclic aromatic in sample and interior mark peak area ratio, bring unary linear regression equation into, calculate often kind of polycyclic aromatic hydrocarbon content.
According to foregoing assay method, select a kind of tobacco juice for electronic smoke B, how record wherein, the content of phenanthrene, anthracene, fluoranthene, pyrene is respectively 38.06 ng/g, 7.97 ng/g, 2.32 ng/g, 4.33 ng/g, 2.80 ng/g, other palycyclic aromatics do not detect.
Claims (5)
1. the assay method of 16 kinds of palycyclic aromatics in a tobacco juice for electronic smoke, it is characterized in that: the method adds a small amount of water by tobacco juice for electronic smoke sample, shaken well, being well dispersed in zeyssatite solid phase supports in liquid-liquid extraction post, extract with cyclohexane, after extract is concentrated, gas chromatograph-mass spectrometer (GCMS) (GC-MS) is adopted to realize the mensuration of 16 kinds of palycyclic aromatics in tobacco juice for electronic smoke; Concrete determination step is as follows:
(1) extraction of testing sample and concentrated: accurately take 0.1 ~ 3 g electronic cigarette liquid in conical flask, add D
8-Nai, D
10-Fei, D
12mark and 0.9 ~ 3 mL water in-benzo [a] pyrene 3 kinds, all proceeding to solid phase after vibration 2 ~ 10 min supports in liquid-liquid extraction post, pressurization makes testing sample solution fully spread in column packing, leave standstill 2 ~ 10 min, add 5 ~ 24 mL cyclohexane wash-outs, collect eluent, be concentrated into about 0.2 ~ 1 mL, detect with GC-MS;
(2) preparation of standard working solution: preparation to have in 16 kinds of palycyclic aromatics of concentration gradient and 3 kinds target cyclohexane solution as hybrid standard working solution;
(3) GC-MS of sample analyzes,
(4) Specification Curve of Increasing and result calculate.
2. the assay method of 16 kinds of palycyclic aromatics in tobacco juice for electronic smoke according to claim 1, is characterized in that: GC-MS analysis condition:
Injector temperature: 280 DEG C; Sample size: 1 μ L; Splitless injecting-Sample; Carrier gas: helium, constant current flow velocity 1mL/min; Chromatographic column: DB-5MS, specification 30m × 0.25mm × 0.25 μm; Temperature programme: 60 DEG C keep 1min, then rise to 110 DEG C with the speed of 20 DEG C/min, then rise to 280 DEG C with the speed of 5 DEG C/min, keep 10min;
Ionization mode: EI; Transmission line temperature: 280 DEG C; Ion source temperature: 230 DEG C;
Scan mode: SIM, Selective ion mode, see table 1, is 50ms to the monitoring time of each ion.
3. the assay method of 16 kinds of palycyclic aromatics in tobacco juice for electronic smoke according to claim 1, is characterized in that: the preparation method of hybrid standard working solution is as follows:
1) preparation of hybrid standard stock solution: accurately take 10 mg, 16 kinds of palycyclic aromatics respectively in the brown volumetric flask of 100 mL, dissolve constant volume with cyclohexane; The preparation of mark stock solution in mixing: accurately take 10 mg D respectively
8-Nai, D
10-Fei, D
12-benzo [a] pyrene, in the brown volumetric flask of 100 mL, dissolves constant volume with cyclohexane;
2) preparation of hybrid standard working solution: accurately add 5 uL respectively, 10 uL, 20 uL, 40 uL, in 80 uL hybrid standard stock solutions and 40 uL mix, mark stock solution is in 50 mL volumetric flasks, uses cyclohexane constant volume.
4. the assay method of 16 kinds of palycyclic aromatics in tobacco juice for electronic smoke according to claim 1, it is characterized in that: Specification Curve of Increasing and result calculate specific as follows: carry out area integral to the response of series standard solution, calibration curve is done with the ratio of often kind of palycyclic aromatic and interior target response area comparison content, carry out matching with straight line, obtain unary linear regression equation; The sample of preparation is measured, records often kind of palycyclic aromatic in sample and interior mark peak area ratio, bring unary linear regression equation into, calculate often kind of polycyclic aromatic hydrocarbon content.
5. the assay method of 16 kinds of palycyclic aromatics in tobacco juice for electronic smoke according to claim 1, is characterized in that: when sample solution wash-out, and controlling the eluent rate of outflow is 2 mL/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510233951.8A CN104764851B (en) | 2015-05-11 | 2015-05-11 | The assay method of 16 kinds of palycyclic aromatics in a kind of tobacco juice for electronic smoke |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510233951.8A CN104764851B (en) | 2015-05-11 | 2015-05-11 | The assay method of 16 kinds of palycyclic aromatics in a kind of tobacco juice for electronic smoke |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104764851A true CN104764851A (en) | 2015-07-08 |
| CN104764851B CN104764851B (en) | 2016-02-24 |
Family
ID=53646812
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510233951.8A Active CN104764851B (en) | 2015-05-11 | 2015-05-11 | The assay method of 16 kinds of palycyclic aromatics in a kind of tobacco juice for electronic smoke |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104764851B (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105136931A (en) * | 2015-09-07 | 2015-12-09 | 国家烟草质量监督检验中心 | Method for determining polyaromatic hydrocarbons in smokeless tobacco product by utilization of on-line solid phase extraction high performance liquid chromatography |
| CN105181857A (en) * | 2015-09-07 | 2015-12-23 | 国家烟草质量监督检验中心 | Method for measuring polycyclic aromatic hydrocarbons in cigarette cut tobacco by on-line solid phase extraction and high performance liquid chromatography |
| CN106226417A (en) * | 2016-07-12 | 2016-12-14 | 吉林烟草工业有限责任公司 | Polyol ethers and the detection method of ester type compound thereof in a kind of tobacco juice for electronic smoke |
| CN106248835A (en) * | 2016-09-28 | 2016-12-21 | 云南省烟草质量监督检测站 | The method of 22 kinds of multiring aromatic hydrocarbon substance content in detection cigarette smoke simultaneously |
| CN106645444A (en) * | 2016-09-28 | 2017-05-10 | 云南省烟草质量监督检测站 | Method for detecting polycyclic aromatic hydrocarbon content in smokeless tobacco products |
| CN108627591A (en) * | 2017-03-24 | 2018-10-09 | 上海安谱实验科技股份有限公司 | The extracting method of polycyclic aromatic hydrocarbon in PA6 products |
| CN109828050A (en) * | 2019-03-08 | 2019-05-31 | 中钢集团鞍山热能研究院有限公司 | A kind of method of 3,4- BaP content in quick measurement coal tar, coal tar pitch |
| CN110927264A (en) * | 2019-11-08 | 2020-03-27 | 河北省医疗器械与药品包装材料检验研究院(河北省医疗器械技术审评中心) | Method and kit for detecting glucocorticoid in serum |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1999052616A1 (en) * | 1998-04-16 | 1999-10-21 | Envirol, Inc. | Extraction using a nonpolar polymer adsorbent |
| CN102879484A (en) * | 2011-07-14 | 2013-01-16 | 中国烟草总公司郑州烟草研究院 | Method for determining content of benzo[a]pyrene in cigarette mainstream smoke |
| CN103323543A (en) * | 2013-05-21 | 2013-09-25 | 上海烟草集团有限责任公司 | Method for detecting 17 polycyclic aromatic hydrocarbons in cigarette gas |
| CN103439443A (en) * | 2013-08-29 | 2013-12-11 | 中国烟草总公司郑州烟草研究院 | Method for simultaneously measuring 16 polyaromatic hydrocarbons in mainstream smoke of cigarettes |
| CN203502394U (en) * | 2013-09-23 | 2014-03-26 | 江苏中烟工业有限责任公司 | Device for extracting and purifying polyaromatic hydrocarbon in cigarette smoke |
| EP2840398A1 (en) * | 2013-08-21 | 2015-02-25 | Biotage AB | Sample preparation workstation |
-
2015
- 2015-05-11 CN CN201510233951.8A patent/CN104764851B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1999052616A1 (en) * | 1998-04-16 | 1999-10-21 | Envirol, Inc. | Extraction using a nonpolar polymer adsorbent |
| CN102879484A (en) * | 2011-07-14 | 2013-01-16 | 中国烟草总公司郑州烟草研究院 | Method for determining content of benzo[a]pyrene in cigarette mainstream smoke |
| CN103323543A (en) * | 2013-05-21 | 2013-09-25 | 上海烟草集团有限责任公司 | Method for detecting 17 polycyclic aromatic hydrocarbons in cigarette gas |
| EP2840398A1 (en) * | 2013-08-21 | 2015-02-25 | Biotage AB | Sample preparation workstation |
| CN103439443A (en) * | 2013-08-29 | 2013-12-11 | 中国烟草总公司郑州烟草研究院 | Method for simultaneously measuring 16 polyaromatic hydrocarbons in mainstream smoke of cigarettes |
| CN203502394U (en) * | 2013-09-23 | 2014-03-26 | 江苏中烟工业有限责任公司 | Device for extracting and purifying polyaromatic hydrocarbon in cigarette smoke |
Non-Patent Citations (8)
| Title |
|---|
| MOHAMMED ZOUGAGH 等: "Direct automatic screening and individual determination of polycyclic aromatic hydrocarbons using supercritical fluid extraction coupled on-line with liquid chromatography and fluorimetric detection", 《ANALYTICA CHIMICA ACTA》, vol. 524, no. 12, 25 October 2004 (2004-10-25), pages 279 - 285 * |
| STEVEN G. CARMELLA 等: "High Throughput Liquid and Gas Chromatography–Tandem Mass Spectrometry Assays for Tobacco-Specific Nitrosamine and Polycyclic Aromatic Hydrocarbon Metabolites Associated with Lung Cancer in Smokers", 《CHEM. RES. TOXICOL》, vol. 26, no. 8, 9 July 2013 (2013-07-09), pages 1209 - 1217 * |
| 刁春燕 等: "土壤、沉积物和植物样品中多环芳烃（PAHs）不同提取与净化方法比较", 《农业环境科学学报》, vol. 30, no. 12, 31 December 2011 (2011-12-31), pages 2399 - 2407 * |
| 包建民 等: "一种以含硅藻土的复合材料为介质的支撑液液萃取柱的制备及其应用", 《色谱》, vol. 30, no. 8, 31 August 2012 (2012-08-31), pages 798 - 803 * |
| 孙闰霞 等: "超声提取/气相色谱-质谱法测定海洋生物中的多环芳烃", 《分析测试学报》, vol. 32, no. 1, 31 January 2013 (2013-01-31), pages 57 - 63 * |
| 杨左军 等: "气相色谱-串联质谱法同时测定纸质食品接触材料中多环芳烃", 《中国造纸》, vol. 33, no. 4, 30 April 2014 (2014-04-30), pages 22 - 28 * |
| 毛婷 等: "气相色谱/质谱法测定烧烤肉制品中15种欧盟优控多环芳烃", 《分析化学》, vol. 38, no. 10, 31 October 2010 (2010-10-31), pages 1439 - 1444 * |
| 王丽 等: "固相支持液液萃取-气相色谱法测定淡水鱼及水体中共平面多氯联苯", 《现代预防医学》, vol. 39, no. 23, 31 December 2012 (2012-12-31), pages 6238 - 6241 * |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105136931A (en) * | 2015-09-07 | 2015-12-09 | 国家烟草质量监督检验中心 | Method for determining polyaromatic hydrocarbons in smokeless tobacco product by utilization of on-line solid phase extraction high performance liquid chromatography |
| CN105181857A (en) * | 2015-09-07 | 2015-12-23 | 国家烟草质量监督检验中心 | Method for measuring polycyclic aromatic hydrocarbons in cigarette cut tobacco by on-line solid phase extraction and high performance liquid chromatography |
| CN106226417A (en) * | 2016-07-12 | 2016-12-14 | 吉林烟草工业有限责任公司 | Polyol ethers and the detection method of ester type compound thereof in a kind of tobacco juice for electronic smoke |
| CN106226417B (en) * | 2016-07-12 | 2018-12-25 | 吉林烟草工业有限责任公司 | The detection method of polyol ethers and its ester type compound in a kind of tobacco juice for electronic smoke |
| CN106248835A (en) * | 2016-09-28 | 2016-12-21 | 云南省烟草质量监督检测站 | The method of 22 kinds of multiring aromatic hydrocarbon substance content in detection cigarette smoke simultaneously |
| CN106645444A (en) * | 2016-09-28 | 2017-05-10 | 云南省烟草质量监督检测站 | Method for detecting polycyclic aromatic hydrocarbon content in smokeless tobacco products |
| CN106248835B (en) * | 2016-09-28 | 2019-05-31 | 云南省烟草质量监督检测站 | The method for detecting 22 kinds of multiring aromatic hydrocarbon substance contents in cigarette smoke simultaneously |
| CN106645444B (en) * | 2016-09-28 | 2019-06-04 | 云南省烟草质量监督检测站 | A kind of method of multiring aromatic hydrocarbon substance content in detection smoke-free tobacco product |
| CN108627591A (en) * | 2017-03-24 | 2018-10-09 | 上海安谱实验科技股份有限公司 | The extracting method of polycyclic aromatic hydrocarbon in PA6 products |
| CN109828050A (en) * | 2019-03-08 | 2019-05-31 | 中钢集团鞍山热能研究院有限公司 | A kind of method of 3,4- BaP content in quick measurement coal tar, coal tar pitch |
| CN110927264A (en) * | 2019-11-08 | 2020-03-27 | 河北省医疗器械与药品包装材料检验研究院(河北省医疗器械技术审评中心) | Method and kit for detecting glucocorticoid in serum |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104764851B (en) | 2016-02-24 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104764851B (en) | The assay method of 16 kinds of palycyclic aromatics in a kind of tobacco juice for electronic smoke | |
| CN104655766B (en) | Assay method while nicotine, propylene glycol and glycerol in a kind of tobacco juice for electronic smoke | |
| CN105866267B (en) | The extraction of residual solvent, detection method and kit and purposes in packaging material | |
| CN106324130A (en) | Chiral analysis method for nicotine in cigarette cut tobacco | |
| CN103675134B (en) | Method for detecting benzene series pollutants in gas by using internal standard method | |
| CN110412174B (en) | Headspace microdroplet extraction-chromatographic detection method for residual solvent in grease | |
| CN106841442B (en) | Method for simultaneously determining vinyl acetate and six benzene series in water-based adhesive | |
| Jiang et al. | Ultrasonic nebulization headspace ionic liquid-based single drop microextraction of flavour compounds in fruit juices | |
| CN106645444B (en) | A kind of method of multiring aromatic hydrocarbon substance content in detection smoke-free tobacco product | |
| CN105424845A (en) | Method for analyzing aroma components of flavoring material through GC/MS based on thermal desorption | |
| CN104237438B (en) | Tenax makes analogies-GCMS and measures the method for the migration amount of aromatic amine in paper and cardboard | |
| CN105067728A (en) | Method for measuring solvent compositions in nicotine liquid by combining gas chromatography and mass spectrometry | |
| CN106645443A (en) | Method for detecting short-chain chlorinated paraffin (SCCP) and medium-chain chlorinated paraffin (MCCP) in consumer goods | |
| CN106248835A (en) | The method of 22 kinds of multiring aromatic hydrocarbon substance content in detection cigarette smoke simultaneously | |
| CN104655753A (en) | Method for determining 3-acetyl-2, 5-thioxene in food additive | |
| Escuderos | Olive oil aroma evaluation by gas chromatographic method: a critical review | |
| CN101539549A (en) | Photoionization gas chromatography detection method of organic volatile compounds in air | |
| CN103743844A (en) | Determination method of alcohol content in methanol | |
| CN104198605B (en) | A kind of assay method of cigarette hot melt adhesive phenol antioxidant content | |
| Mokhtar et al. | Direct ionic liquid extractant injection for volatile chemical analysis–a gas chromatography sampling technique | |
| CN107167534A (en) | A kind of method for detecting seven kinds of benzene compounds in cigarette paper thermal cracking products | |
| CN104280474B (en) | High performance liquid chromatography fluorescence detection method for simultaneously detecting 4 forbidden additives in tobacco flavor and fragrance | |
| Sotnikov et al. | Gas-chromatographic determination of 1, 1-dimethylhydrazine in water | |
| CN105572240A (en) | Method for detecting content of pharmaceutic adjuvant carmine by using high performance liquid chromatography | |
| CN104062378B (en) | The detection method of diaminotoluene isomeride |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| EXSB | Decision made by sipo to initiate substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |