CN104865335A - Detection method of 2-nitropropane in cigarette mainstream smoke - Google Patents
Detection method of 2-nitropropane in cigarette mainstream smoke Download PDFInfo
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- CN104865335A CN104865335A CN201510274681.5A CN201510274681A CN104865335A CN 104865335 A CN104865335 A CN 104865335A CN 201510274681 A CN201510274681 A CN 201510274681A CN 104865335 A CN104865335 A CN 104865335A
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Abstract
The invention discloses a detection method of 2-nitropropane in cigarette mainstream smoke. The detection method comprises the following steps: using a silica gel solid-phase extraction column to catch the 2-nitropropane in the cigarette mainstream smoke; after the smoke is sucked, taking out the silica gel solid-phase extraction column for collecting all cigarette smoke samples, performing drip washing and elution by adopting n-pentane and a n-pentane and diethyl ether mixed solution, collecting an eluent and blending, directly sampling to perform ammonia chemical ionization and gas chromatography tandem mass spectrum combined analysis, and using an external standard method to be quantitative. A multi-reaction monitoring (MRM) mode is adopted for qualitative and quantitative detection, so that the accuracy and the sensitivity of the method can be effectively improved; a repeated elution solid-phase extraction purification method is adopted in a pretreatment process, so that the matrix interference can be effectively reduced, and the experimental repeatability and recovery rate are good. Therefore the detection method is suitable for quantitative analysis of the 2-nitropropane in all kinds of cigarette mainstream smoke.
Description
Technical field
The invention belongs to cigarette smoke technical field of analysis and detection, be specifically related to the detection method of 2-nitropropane in cigarette mainstream flue gas.
Background technology
Correlative study shows, 2-nitropropane is one of objectionable constituent in cigarette smoke, and its harmfulness is comparatively large, by sucking, eating and percutaneous absorbtion enters in body, has spread effect, suck high concentration and cause anesthetic action eye and respiratory mucosa.Calomel poisoning person causes chemical tracheobronchitis; Moderate intoxication person is chemical pneumonia; Can chemical pulmonary edema be there is in severe intoxication person.2-nitropropane is classified as 2B class carcinogenic substance (may be carcinogenic to people) by the international cancer research institution (IARC) of the World Health Organization (WHO), is also one of main objectionable constituent of 69 kinds of Hoffmann inventories simultaneously.Therefore, the detection method of 2-nitropropane in systematic study main flume, for full appreciation safety cigarette and " smoking with healthy " problem all tool be of great significance.
At present about the analytical approach research of 2-nitropropane in cigarette mainstream flue gas, rarely has report both at home and abroad.Therefore, 2-nitropropane in a kind of simple, sensitive, high-throughout method detection cigarette mainstream flue gas is set up very necessary.
Summary of the invention
Goal of the invention of the present invention is to provide a kind of simple, sensitive, qualitative, quantitative and uses ammonia chemi-ionization-gas chromatography tandem mass spectrum connection method to detect the method for 2-nitropropane in cigarette mainstream flue gas accurately.
The object of the invention is to be achieved through the following technical solutions:
In a kind of cigarette mainstream flue gas, the detection method of 2-nitropropane comprises the following steps:
1. preparing standard solution: the 2-nitropropane standard solution with normal hexane compound concentration being 5.0mg/mL;
2. the drafting of typical curve: the 2-nitropropane standard solution accurately pipetting 0.010mL, 0.025mL, 0.050mL, 0.125mL, 0.625mL respectively, in the brown volumetric flask of 25mL, is diluted to scale with normal hexane, carries out GC-MS/MS detection; Using the peak area of 2-nitropropane as ordinate, the concentration of 2-nitropropane, as horizontal ordinate, sets up the calibration curve of 2-nitropropane.
3. the suction of cigarette: aspirated according to GB/T19609 specified standard condition by the cigarette sample smoking machine to be measured balanced, aspirates 20 cigarette, with the 2-nitropropane in silica gel solid phase extraction column trapping cigarette mainstream flue gas;
4. sample pre-treatments and analysis: after cigarette smoking, take off silica gel solid phase extraction column, be the n-pentane/ether mixed solution drip washing 1 time of 85:15 successively by 15mL n-pentane drip washing 2 times, 7mL volume ratio, then be the n-pentane/ether mixed solution wash-out 3 times of 85:15 by 5mL volume ratio, collect all eluents, after shaken well, GC-MS/MS analysis is carried out in direct sample.
Described step 2. and 4. in chromatographic condition as follows:
Chromatographic column, DB-624 (60m × 0.25mm × 1.4 μm);
GC input mode: sample size 1 μ L, split ratio 10:1;
Solvent delay: 8min;
Injector temperature: 180 DEG C;
Carrier gas is He, and flow velocity is 1.5mL/min;
Initial temperature: initial temperature 60 DEG C, keep 6min, 20 DEG C/min rises to 220 DEG C, keeps 16min.
Described step 2. and 4. in Mass Spectrometry Conditions as follows:
Ionization mode: ammonia chemi-ionization;
Transmission line temperature: 230 DEG C;
Ammonia flow: 2mL/min;
Quadrupole rod temperature: 150 DEG C;
Collision gas: nitrogen;
Scan mode: multiple-reaction monitoring pattern (MRM), 2-nitropropane quota ion, qualitative ion pair are respectively 41,39, and impact energy is 25.
Advantage of the present invention is:
The instrument and equipment that the present invention uses is laboratory conventional analysis equipment, and inventive method is easy to promote, and testing cost is low;
The present invention proposes the analytical approach adopting ammonia chemi-ionization-gas chromatography tandem mass spectrum connection method to measure 2-nitropropane in cigarette mainstream flue gas first; Method of the present invention adopts multiple-reaction monitoring pattern (MRM) to carry out row quantitative and qualitative analysis, effectively can improve the sensitivity of accuracy and method; Method of the present invention adopts repeatedly wash-out Solid phase extraction method in pretreatment process, effectively can reduce matrix interference, and the repeatability of experiment and the recovery are all fine, are applicable to the quantitative test of 2-nitropropane in all kinds of cigarette mainstream flue gas.
Accompanying drawing explanation
Fig. 1 is the typical sample chromatogram that the present invention obtains.
Embodiment
The present invention is described further with the following Examples:
1. preparing standard solution: the 2-nitropropane standard solution with normal hexane compound concentration being 5.0mg/mL; 2. the drafting of typical curve: the 2-nitropropane standard solution accurately pipetting 0.010mL, 0.025mL, 0.050mL, 0.125mL, 0.625mL respectively, in the brown volumetric flask of 25mL, is diluted to scale with normal hexane, carries out GC-MS/MS detection; Using the peak area of 2-nitropropane as ordinate, the concentration of 2-nitropropane, as horizontal ordinate, sets up the calibration curve of 2-nitropropane.3. the suction of cigarette: aspirated according to GB/T19609 specified standard condition by the cigarette sample smoking machine to be measured balanced, aspirates 20 cigarette, with the 2-nitropropane in silica gel solid phase extraction column trapping cigarette mainstream flue gas;
4. sample pre-treatments and analysis: after cigarette smoking, take off silica gel solid phase extraction column, be the n-pentane/ether mixed solution drip washing 1 time of 85:15 successively by 15mL n-pentane drip washing 2 times, 7mL volume ratio, then be the n-pentane/ether mixed solution wash-out 3 times of 85:15 by 5mL volume ratio, collect all eluents, after shaken well, GC-MS/MS analysis is carried out in direct sample.
Chromatograph mass spectrum analysis:
Chromatographic column: DB-624 (60m × 0.25mm × 1.4 μm);
GC input mode: sample size 1 μ L, split ratio 10:1;
Solvent delay: 8min;
Injector temperature: 180 DEG C;
Carrier gas is He, and flow velocity is 1.5mL/min;
Initial temperature: initial temperature 60 DEG C, keep 6min, 20 DEG C/min rises to 220 DEG C, keeps 16min.
Ionization mode: ammonia chemi-ionization;
Transmission line temperature: 230 DEG C;
Ammonia flow: 2mL/min;
Quadrupole rod temperature: 150 DEG C;
Collision gas: nitrogen;
Scan mode: multiple-reaction monitoring pattern (MRM), 2-nitropropane quota ion, qualitative ion pair are respectively 41,39, and impact energy is 25.
The range of linearity of table 1 analytical approach and detectability
Detection limit: with signal to noise ratio (S/N ratio) S/N=3 corresponding concentration determination detection limit, result is as shown in table 1.
The recovery: adopt sample mark-on method to carry out the mensuration of the recovery to same fume sample on high, medium and low three contents levels, result shows, the result of average recovery rate is between 89.2% ~ 95.3%, and the recovery is higher.
Typical sample measurement result: 6 cigarette samples are measured, wherein Virginian-type cigarette 3, blended type cigarette 3.Measurement result is in table 2:
Table 2 fume sample measurement result (μ g/ props up)
Typical sample chromatogram is shown in Fig. 1.
Claims (2)
1. the detection method of 2-nitropropane in cigarette mainstream flue gas, it is characterized in that, the method comprises the following steps:
1. preparing standard solution: the 2-nitropropane standard solution with normal hexane compound concentration being 5.0mg/mL;
2. the drafting of typical curve: the 2-nitropropane standard solution accurately pipetting 0.010mL, 0.025mL, 0.050mL, 0.125mL, 0.625mL respectively, in the brown volumetric flask of 25mL, is diluted to scale with normal hexane, carries out GC-MS/MS detection; Using the peak area of 2-nitropropane as ordinate, the concentration of 2-nitropropane, as horizontal ordinate, sets up the calibration curve of 2-nitropropane;
3. the suction of cigarette: aspirated according to GB/T19609 specified standard condition by the cigarette sample smoking machine to be measured balanced, aspirates 20 cigarette, with the 2-nitropropane in silica gel solid phase extraction column trapping cigarette mainstream flue gas;
4. sample pre-treatments and analysis: after cigarette smoking, take off silica gel solid phase extraction column, be the n-pentane/ether mixed solution drip washing 1 time of 85:15 successively by 15mL n-pentane drip washing 2 times, 7mL volume ratio, then be the n-pentane/ether mixed solution wash-out 3 times of 85:15 by 5mL volume ratio, collect all eluents, after shaken well, GC-MS/MS analysis is carried out in direct sample;
Described step 2. and 4. in chromatographic condition as follows:
Chromatographic column, DB-624,60m × 0.25mm × 1.4 μm;
GC input mode: sample size 1 μ L, split ratio 10:1;
Solvent delay: 8min;
Injector temperature: 180 DEG C;
Carrier gas is He, and flow velocity is 1.5mL/min;
Initial temperature: initial temperature 60 DEG C, keep 6min, 20 DEG C/min rises to 220 DEG C, keeps 16min.
2. the detection method of 2-nitropropane in a kind of cigarette mainstream flue gas according to claim 1, is characterized in that: described step 2. and 4. in Mass Spectrometry Conditions as follows:
Ionization mode: ammonia chemi-ionization;
Transmission line temperature: 230 DEG C;
Ammonia flow: 2mL/min;
Quadrupole rod temperature: 150 DEG C;
Collision gas: nitrogen;
---scan mode: multiple-reaction monitoring pattern (MRM), 2-nitropropane quota ion, qualitative ion pair are respectively 41,39, and impact energy is 25.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20120209023A1 (en) * | 2011-02-14 | 2012-08-16 | Kulamani Parida | Modified layered double hydroxide (ldh) and a process for preparation thereof for c-c bond forming reactions |
| CN103209606A (en) * | 2010-10-06 | 2013-07-17 | 塞拉尼斯醋酸纤维有限公司 | Smoke filters for smoking devices with porous masses having a carbon particle loading and an encapsulated pressure drop |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103209606A (en) * | 2010-10-06 | 2013-07-17 | 塞拉尼斯醋酸纤维有限公司 | Smoke filters for smoking devices with porous masses having a carbon particle loading and an encapsulated pressure drop |
| US20120209023A1 (en) * | 2011-02-14 | 2012-08-16 | Kulamani Parida | Modified layered double hydroxide (ldh) and a process for preparation thereof for c-c bond forming reactions |
Non-Patent Citations (4)
| Title |
|---|
| J. DIEKMANN: "《Joerg Diekmann 2-Nitropropane》", 15 February 2006 * |
| JAMES A. BALLANTINE ET AL: "Relative Molecular Mass Information from Aliphatic Nitro Compounds: a Chemical Ionization Study", 《ORGANIC MASS SPECTROMETRY》 * |
| RESTEK COPORATION: "Are Your Volatiles Methods Slowing You Down? Minimize Downtime with an Rxi®-624Sil MS and Our Synchronized GC Conditions", 《THE RESTEK ADVANTAGE》 * |
| TESTAMERICA LABORATORIES, INC.: "《Re: Supplemental Source Area Investigation Work Plan Wichita USD259 School Service Center Site, Wichita, Kansas》", 19 June 2014 * |
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