CN103399118A - Method used for detecting caffeic acid content in cigarette sidestream smoke by high performance liquid chromatography-tandem mass spectrum - Google Patents
Method used for detecting caffeic acid content in cigarette sidestream smoke by high performance liquid chromatography-tandem mass spectrum Download PDFInfo
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Abstract
The invention discloses a method used for detecting caffeic acid content in cigarette sidestream smoke by high performance liquid chromatography-tandem mass spectrum. The method comprises following steps: (1) total particulate matters in smoke are collected by a fishtail cover and a filter disc; (2) the filter disc is placed in a methanol solution containing internal standard substances for extraction so as to obtain an extract; (3) the extract is filtered, and then is detected by a high performance liquid chromatography-tandem mass spectrometer; and (4) the content of caffeic acid is quantitatively analyzed by internal standard method. According to the method used for detecting caffeic acid content in cigarette sidestream smoke by high performance liquid chromatography-tandem mass spectrum, pre-treatment is simple, separating effect is excellent, qualitative analysis is accurate, sample analysis time is short, and detection sensitivity is high.
Description
Technical field
The present invention relates to tobacco and technical field of chemistry, particularly relate to the assay method of caffeinic high performance liquid chromatography-tandem mass in a kind of cigarette side-stream smoke.
Background technology
Caffeic acid is on molecular level, this compound can cause the fracture of DNA double chain structure in experiment in vitro, on cellular level, this compound is found also may cause chromosome aberration and sister chromatid exchange, international cancer research institution of the World Health Organization (WHO) (IARC) is classified as 2B class carcinogen by it, about this compound, the impact of health is subject to extensive concern always.Calendar year 2001 Hoffmann and its researcher have carried out amendment and supplement to the objectionable constituent inventory of 1991, caffeic acid is classified as to one of 69 kinds of objectionable constituent of cigarette smoke, Rodgman in 2002 and Green sum up the objectionable constituent of having reported in flue gas, also caffeic acid are classified as to one of 149 kinds of cigarette smoke objectionable constituent.
In the traditional Chinese medicine materials such as dandelion, caulis lonicerae, the achene of Siberian cocklebur, the report of the assay method of caffeic acid content is more, what mainly adopt is high performance liquid chromatography, UV-detector is carried out quantitative test, and the detection method of high performance liquid chromatography-tandem mass also has a small amount of report.(the Journal of Analytical Science such as Xu Gaoyan, 2006,22 (5): 567-569.) by the ultrasonic extraction of methyl alcohol of water-soluble Rosmarinus officinalis extract, after the extracting liquid filtering film, directly adopt high performance liquid chromatography-tandem mass to measure wherein caffeinic content, detecting of method for building up is limited to 5ng/mL.Caffeic acid is also a kind of of tobacco leaf polyphenol substance, and certain content distribution is also arranged in tobacco leaf.(assay laboratory, 2006,25 (2): 92-96.) by tobacco leaf drying, pulverize, adopt capillary electrophoresis with electrochemical detection to measure simultaneously and contain the content of caffeic acid at interior several polyhydric phenol Peng Youyuan etc. after the ultrasonic extraction of ethanol water.(assay laboratory, 2009,28 (10): 108-112.) also reported and adopted high performance liquid chromatography-tandem mass to measure the method for caffeic acid content in tobacco leaf such as Zhu Ruizhi.
Mensuration about phenolic compounds in cigarette smoke mainly concentrates on several phenolic compounds of showing great attention to such as o-benzenediol, p-benzenediol, phenol, o-cresols, m-cresol.A kind of method of measuring several main phenolic compounds such as o-benzenediol in cigarette mainstream flue gas, p-benzenediol, phenol, o-cresols, m-cresol is disclosed as Chinese patent 200910066382.7, this assay method is to utilize glass fiber filter to capture the main phenolic compound in cigarette mainstream flue gas, with after the acetic acid aqueous solution extraction, filtering, adopt two-dimensional liquid chromatography piece-rate system series connection fluorescence detector to detect, measure the content of these several phenolic compounds in cigarette mainstream flue gas.(the tobacco science and technology such as Xie Fuwei, 2004,5:6-10.) adopt 1% acetum to extract the flue gas TPM, extract directly carries out the HPLC analysis after filtering with microporous membrane, adopt fluorescence detector to detect, set up in cigarette main flow and side-stream smoke adjacent,, p-benzenediol, phenol, adjacent,, the detection method of 7 kinds of phenols components such as p-Cresol.
But, cigarette is in combustion process, the multiple physical and chemical reactions such as distillation, destructive distillation, pyrolysis, synthetic, condensation have occurred, form a large amount of Xinshenghua compounds, and whether distribute in cigarette side-stream smoke about caffeic acid, the pertinent literature report how to measure is less, and so far, not yet finding has any patent and the bibliographical information that adopts the high performance liquid chromatography-tandem mass instrument to measure caffeic acid content in cigarette side-stream smoke both at home and abroad.And smoke components is very complicated, and matrix interference is serious, and the content of caffeic acid in flue gas is lower again, and it is on the knees of the gods that can the detection method of the phenolic compound in smoke of having set up be applicable in flue gas caffeinic mensuration.
Environmental tobacco smoke (ETS) is important indoor pollutant, and what the involuntary smoker experienced is exactly this kind material, and the side-stream smoke of cigarette is the main source of environmental tobacco smoke, accounts for 85% of environmental tobacco smoke.Along with the growing interest of the public to smoking and health problem, in cigarette, the objectionable constituent burst size becomes the focus that people pay close attention to gradually, at present, relevant law has been formulated in some countries and regions such as Canada, requires the production of cigarettes business that the burst size of harmful constituents in cigarette flue gas is provided.In view of this, set up the detection method of caffeic acid content in a kind of cigarette side-stream smoke, in research cigarette smoking process, the regularity of distribution important in inhibiting of caffeic acid in cigarette main flow and side-stream smoke, also be conducive to the size of objective evaluation cigarette harmfulness.
Summary of the invention
Technical matters to be solved by this invention is to provide a kind of method that high performance liquid chromatography-tandem mass is measured caffeic acid content in cigarette side-stream smoke, provide namely that a kind of pre-treatment is simple, good separating effect, qualitative accurately, the assay method of caffeinic high performance liquid chromatography-tandem mass in sample analysis time is short, detection sensitivity is high cigarette side-stream smoke.
The technical solution used in the present invention is to provide a kind of method that high performance liquid chromatography-tandem mass is measured caffeic acid content in cigarette side-stream smoke, and the method comprises the steps:
(1) with fish tail cover and filter disc, capture the TPM in flue gas;
(2) filter disc is placed in to methanol solution and extracts to obtain extract;
(3) filter extract, with high performance liquid chromatography/mass spectrometer, filtrate is measured;
(4) adopt the inner mark method ration analysis to draw caffeic acid content.
Preferably, the described capture of step (1) refers to cigarette to be measured is stipulated in the Atmospheric Condition of GB/T16447-2004 tobacco and tobacco product adjusting and test environmental baseline balance 48h; Determine the stub length with the mark smoking cigarette, the side-stream smoke suction method of stipulating in mensuration according to T/N in cigarette side-stream smoke in YC/T185, the suction flow of regulating the effluent smoking machine is 3000mL/min, aspirate 5 cigarette, with fish tail cover and glass fiber filter, capture the side-stream smoke TPM.
Preferably, the described methanol solution of step (2) contains internal standard compound.
Preferably, described internal standard compound is salicylic acid.
Preferably, the described filtration of step (3) refers to that extract is through the organic phase membrane filtration.
Preferably, the described high performance liquid chromatograph condition of step (3) is: C18 reversed-phase column, 30 ℃ of detected temperatures, sample size 1 μ L～10 μ L, flow velocity 0.2～0.4mL/min, gradient elution; Mobile phase A is deionized water, and Mobile phase B is methyl alcohol; Described mass spectrometer condition is: ionization mode is electron spray, and scan pattern is negative ion, atomization gas 25～35psi, gas curtain gas 10psi, auxiliary heating gas 20～30psi, collision gas 5psi, ion gun injection electric 5000～5800V, 350～400 ℃ of ion source temperatures.
Preferably, the condition of described gradient elution is as follows:
| Time/min | Flow velocity/mL ﹒ min-1 | Mobile phase A % | Mobile phase B % |
| 0 | 0.2 | 80 | 20 |
| 5 | 0.2 | 80 | 20 |
| 6 | 0.4 | 0 | 100 |
| 16 | 0.2 | 0 | 100 |
| 17 | 0.2 | 80 | 20 |
| 27 | 0.2 | 80 | 20 |
Preferably, the caffeinic detected parameters of described mass spectrometer detection is: quota ion is 179.0/134.9 to m/z, and qualitative ion pair m/z is 179.0/106.8, and residence time is 200ms, and impact energy is-22.0V.
Preferably, the salicylic detected parameters of described mass spectrometer detection is: quota ion is 136.9/93.1 to m/z, and qualitative ion pair m/z is 136.9/64.5, and residence time is 200ms, and impact energy is-25.0V.
preferably, external standard method is adopted in the described quantitative test of step (4), the caffeic acid series standard working solution of preparation 10ng/mL～300ng/mL, concentration gradient is more than 5 and be uniformly distributed, the concentration of the contained internal standard compound of standard solution at different levels is 90-110ng/mL, utilize the high performance liquid chromatography-tandem mass instrument to detect standard solution, using the ratio of the caffeic acid peak area that obtains and interior mark peak area as ordinate, caffeic acid concentration and internal standard compound concentration ratio are as horizontal ordinate, the drawing standard curve also obtains regression equation, then under the same conditions sample is detected, by in the peak area ratio substitution equation of the caffeic acid that obtains and internal standard compound, can calculate caffeinic content.
The invention has the beneficial effects as follows that having proposed first the employing high performance liquid chromatography-tandem mass measures caffeinic method in cigarette side-stream smoke.Method of the present invention adopts multiple-reaction monitoring pattern (MRM) to carry out quantitative and qualitative analysis, can effectively improve the sensitivity of qualitative accuracy and method, the recovery of standard addition of sample is between 91.42～103.75%, repeatability is not more than 5%, the quantitative limit of cigarette sample can reach 1.17ng/mL, is applicable to caffeinic batch in all kinds of cigarette side-stream smokes and measures.
The accompanying drawing explanation
Fig. 1 is the chromatogram of standard solution;
Fig. 2 is caffeinic chromatogram in embodiment 1 side-stream smoke.
Embodiment
Below in conjunction with drawings and Examples, the present invention further is illustrated.
Instrument, reagent and material:
The triple quadrupole rods tandem mass spectrometry instrument of the U.S.'s API3200 of Applied Biosystems company type, be furnished with electric spray ion source and Analyst system software, U.S. Agilent company 1200 type high performance liquid chromatographs, the band automatic sampler, Germany Borgwaldt RM20H type smoking machine, electronic balance (sensibility reciprocal 0.1mg), convolution adjustable mechanical oscillator.
Methyl alcohol is chromatographically pure, deionized water; The caffeic acid standard items, Chun Du>=98%.
Reagent and solution preparation:
The preparation of standard reserving solution: accurately take the urethanes of about 25mg in the 25mL beaker, be accurate to 0.0001g, add about 10mL methyl alcohol, after dissolving fully, be transferred in the 25mL volumetric flask, with a small amount of methyl alcohol, swing and wash beaker 3～5 times, cleansing solution is transferred in volumetric flask in the lump, then with methanol constant volume to scale.
The preparation of primary standard solution: the standard inventory solution that accurately pipettes 1.0mL with transfer pipet in the 50mL volumetric flask, with methanol constant volume to scale.
The preparation of interior mark storing solution: accurately take the salicylic acid of about 20mg in the 50mL beaker, be accurate to 0.0001g, after adding about 20mL methyl alcohol to dissolve fully, be transferred in the 100mL volumetric flask, with a small amount of methyl alcohol, swing and wash beaker 3～5 times, cleansing solution is transferred in volumetric flask in the lump, then with acetonitrile, is settled to scale.
The preparation of one-level inner mark solution: the interior mark stock solution that accurately pipettes 2.00mL with transfer pipet in the 100mL volumetric flask, with methanol constant volume to scale.
The preparation of secondary inner mark solution: the standard inventory solution that accurately pipettes 5.00mL with transfer pipet in the 250mL volumetric flask, with methanol constant volume to scale.
The preparation of series standard working solution: accurately pipette respectively the primary standard solution of 0.025mL, 0.05mL, 0.25mL, 0.5mL, 1.0mL and 1.50mL secondary inner mark solution in the 50mL volumetric flask, with methanol constant volume to scale, obtain the standard solution of 5 different series concentration, adopt high performance liquid chromatography-tandem mass successively this series standard working solution to be measured, the production standard curve.According to typical curve, obtain regression equation.
Embodiment 1
A kind of high performance liquid chromatography-tandem mass is measured the method for caffeic acid content in cigarette side-stream smoke, and the method comprises the steps:
1. the collection of sample: by certain brand cigarette to be measured balance 48 hours under (22 ± 1) ℃, relative humidity (60 ± 3) % condition, then determine the stub length with the mark smoking cigarette, according to side-stream smoke suction method in YC/T185, the suction flow of regulating the effluent smoking machine is 3000mL/min, aspirate 5 cigarette, with fish tail cover and glass fiber filter, capture the side-stream smoke TPM.
2. filter disc extracts and sample determination: filter disc is placed in to the 100mL conical flask, add wherein 10mL to contain to have an appointment the methanol solution of 120 nanograms (ng) internal standard compound, and divide the clean fish hood 2～3 times with 10mL methyl alcohol, cleaning fluid is transferred in conical flask in the lump, and conical flask is placed on oscillator the 30min that vibrates; Extract adopts high performance liquid chromatography/mass spectrometer (LC-MS/MS) to measure after the organic phase membrane filtration.
3. adopt high performance liquid chromatography-tandem mass to measure:
The high performance liquid chromatograph condition is: the C18 reversed-phase column, and 30 ℃ of detected temperatures, sample size 1 μ L～10 μ L, flow velocity 0.2～0.4mL/min, the first alcohol and water carries out gradient elution as mobile phase; Mobile phase A is deionized water, and Mobile phase B is methyl alcohol; Condition of gradient elution is as shown in table 1:
Table 1 condition of gradient elution
| Time/min | Flow velocity/mL ﹒ min -1 | Mobile phase A % | Mobile phase B % |
| 0 | 0.2 | 80 | 20 |
| 5 | 0.2 | 80 | 20 |
| 6 | 0.4 | 0 | 100 |
| 16 | 0.2 | 0 | 100 |
| 17 | 0.2 | 80 | 20 |
| 27 | 0.2 | 80 | 20 |
The mass spectrometer condition is: ionization mode is electron spray; Scan pattern is negative ion; Atomization gas 25～35psi; Gas curtain gas 10psi; Auxiliary heating gas 20～30psi; Collision gas 5psi; Ion gun injection electric 5000～5800V; 350～450 ℃ of ion source temperatures; Detecting caffeinic detected parameters is: quota ion is 179.0/134.9 to m/z, and qualitative ion pair m/z is 179.0/106.8, and residence time is 200ms, and impact energy is-22.0V; Detecting salicylic detected parameters is: quota ion is 136.9/93.1 to m/z, and qualitative ion pair m/z is 136.9/64.5, and residence time is 200ms, and impact energy is-25.0V.
4. caffeinic content in the calculating cigarette smoke:
Be calculated as follows and obtain caffeinic content in every cigarette side-stream smoke:
In formula:
The caffeinic content of m-every cigarette, unit are nanogram/(ng/cig);
A-caffeic acid peak area;
As-salicylic peak area;
B-drawn by equation of linear regression;
Mark content in ms-sample solution, unit is nanogram (ng);
A-drawn by equation of linear regression;
N-cigarette quantity, unit is for propping up.
Sample is carried out to mensuration twice, then using the mean value of twice mensuration as final measurement result, result is accurate to 0.01ng/cig.Relative deviation between twice measurement result is in 10%, and the mean value of mensuration is in Table 2.
Embodiment 2
A kind of high performance liquid chromatography-tandem mass is measured the method for caffeic acid content in cigarette side-stream smoke, and the method comprises the steps:
1. the collection of sample: by certain brand cigarette balance 48 hours under (22 ± 1) ℃, relative humidity (60 ± 3) % condition, then determine the stub length with the mark smoking cigarette, according to side-stream smoke suction method in YC/T185, the suction flow of regulating the effluent smoking machine is 3000mL/min, aspirate 5 cigarette, with fish tail cover and glass fiber filter, capture the side-stream smoke TPM.
2. filter disc extracts and sample determination: filter disc is placed in to the 100mL conical flask, add wherein 10mL to contain to have an appointment the methanol solution of 120 nanograms (ng) internal standard compound, and divide the clean fish hood 2～3 times with 10mL methyl alcohol, cleaning fluid is transferred in conical flask in the lump, and conical flask is placed on oscillator the 30min that vibrates; Extract adopts high performance liquid chromatography/mass spectrometer (LC-MS/MS) to measure after the organic phase membrane filtration.
3. adopt high performance liquid chromatography-tandem mass to measure:
The high performance liquid chromatograph condition is: the C18 reversed-phase column, and 30 ℃ of detected temperatures, sample size 1 μ L～10 μ L, flow velocity 0.2～0.4mL/min, the first alcohol and water carries out gradient elution as mobile phase; Mobile phase A is deionized water, and Mobile phase B is methyl alcohol; Condition of gradient elution is as shown in table 1:
Table 1 condition of gradient elution
| Time/min | Flow velocity/mL ﹒ min -1 | Mobile phase A % | Mobile phase B % |
| 0 | 0.2 | 80 | 20 |
| 5 | 0.2 | 80 | 20 |
| 6 | 0.4 | 0 | 100 |
| 16 | 0.2 | 0 | 100 |
| 17 | 0.2 | 80 | 20 |
| 27 | 0.2 | 80 | 20 |
The mass spectrometer condition is: ionization mode is electron spray; Scan pattern is negative ion; Atomization gas 25～35psi; Gas curtain gas 10psi; Auxiliary heating gas 20～30psi; Collision gas 5psi; Ion gun injection electric 5000～5800V; 350～450 ℃ of ion source temperatures; Detecting caffeinic detected parameters is: quota ion is 179.0/134.9 to m/z, and qualitative ion pair m/z is 179.0/106.8, and residence time is 200ms, and impact energy is-22.0V; Detecting salicylic detected parameters is: quota ion is 136.9/93.1 to m/z, and qualitative ion pair m/z is 136.9/64.5, and residence time is 200ms, and impact energy is-25.0V.
4. caffeinic content in the calculating cigarette smoke:
Be calculated as follows and obtain caffeinic content in every cigarette side-stream smoke:
In formula:
The caffeinic content of m-every cigarette, unit are nanogram/(ng/cig);
A-caffeic acid peak area;
As-salicylic peak area;
B-drawn by equation of linear regression;
Mark content in ms-sample solution, unit is nanogram (ng);
A-drawn by equation of linear regression;
N-cigarette quantity, unit is for propping up.
Sample is carried out to mensuration twice, then using the mean value of twice mensuration as final measurement result, result is accurate to 0.01ng/cig.Relative deviation between twice measurement result is in 10%, and the mean value of mensuration is in Table 2.
Caffeic acid content in the cigarette flow measurement flue gas that table 2 embodiment 1,2 measures
| Cigarette sample | Caffeic acid (ng/cig) |
| Embodiment 1 | 17.39 |
| Embodiment 2 | 14.81 |
To the sample replicate determination of embodiment 16 times, the repeated result that obtains sample is as shown in table 3:
The repeatability of table 3 embodiment 1 measurement result
| Parallel | 1# | 2# | 3# | 4# | 5# | 6# | Mean value | RSD(%) |
| Content (ng/cig) | 16.36 | 17.28 | 15.41 | 15.87 | 16.4 | 17.54 | 16.48 | 4.93 |
Result in table 3 shows, the relative standard deviation of measurement result is less than 5%, show can the Accurate Measurement cigarette side-stream smoke in caffeinic content.
With the standard specimen of least concentration (10.0ng/mL), repeat sample introduction 10 times, by the concentration value that records, count standard deviation, detectability (LOD) is tried to achieve with 3 times of standard deviations, this method quantitatively be limited to 1.17ng/mL, show that the sensitivity of method is higher.
The recovery
Caffeic acid reference material to adding respectively 66ng, 132ng and 198ng on the cigarette filter disc of embodiment 1, record the caffeic acid content value under three levels of basic, normal, high mark-on, and each horizontal parallel is measured three times, and mean value is in Table 4.The recovery of result presentation method is 91.42～103.75%, shows that the inventive method has the higher recovery.
Table 4 recovery of standard addition
| Caffeic acid addition ng/cig | Yield ng/cig | Average recovery rate % |
| 22.00 | 20.11 | 91.42 |
| 44.00 | 41.91 | 95.24 |
| 66.00 | 68.47 | 103.75 |
The above embodiment of the present invention is only for example of the present invention clearly is described, is not the restriction to embodiments of the present invention.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here can't give all embodiments exhaustive.Everyly belong to the row that apparent variation that technical scheme of the present invention extends out or change still are in protection scope of the present invention.
Claims (10)
1. a high performance liquid chromatography-tandem mass is measured the method for caffeic acid content in cigarette side-stream smoke, it is characterized in that: comprise the steps:
(1) with fish tail cover and filter disc, capture the TPM in flue gas;
(2) filter disc is placed in to methanol solution and extracts to obtain extract;
(3) filter extract, with high performance liquid chromatography/tandem mass spectrometer, filtrate is measured;
(4) adopt the inner mark method ration analysis to draw caffeic acid content.
2. method according to claim 1 is characterized in that: the described capture of step (1) refer to by cigarette to be measured the GB/T16447-2004 tobacco and tobacco product is regulated and the Atmospheric Condition of test in the environmental baseline balance 48h that stipulates; Determine the stub length with the mark smoking cigarette, the side-stream smoke suction method of stipulating in mensuration according to T/N in cigarette side-stream smoke in YC/T185, the suction flow of regulating the effluent smoking machine is 3000mL/min, aspirate 5 cigarette, with fish tail cover and glass fiber filter, capture the side-stream smoke TPM.
3. method according to claim 1, it is characterized in that: the described methanol solution of step (2) contains internal standard compound.
4. method according to claim 3, it is characterized in that: described internal standard compound is salicylic acid.
5. method according to claim 1, it is characterized in that: the described filtration of step (3) refers to that extract is through the organic phase membrane filtration.
6. method according to claim 1, it is characterized in that: the described high performance liquid chromatograph condition of step (3) is: C18 reversed-phase column, 30 ℃ of detected temperatures, sample size 1 μ L～10 μ L, flow velocity 0.2～0.4mL/min, gradient elution; Mobile phase A is deionized water, and Mobile phase B is methyl alcohol; Described mass spectrometer condition is: ionization mode is electron spray, and scan pattern is negative ion, atomization gas 25～35psi, gas curtain gas 10psi, auxiliary heating gas 20～30psi, collision gas 5psi, ion gun injection electric 5000～5800V, 350～400 ℃ of ion source temperatures.
7. method according to claim 6, it is characterized in that: the condition of described gradient elution is as follows:
8. method according to claim 6 is characterized in that: described mass spectrometer detects caffeinic condition and is: quota ion is 179.0/134.9 to m/z, and qualitative ion pair m/z is 179.0/106.8, and residence time is 200ms, and impact energy is-22.0V.
9. method according to claim 6 is characterized in that: described mass spectrometer detects salicylic testing conditions and is: quota ion is 136.9/93.1 to m/z, and qualitative ion pair m/z is 136.9/64.5, and residence time is 200ms, and impact energy is-25.0V.
10. method according to claim 1, it is characterized in that: external standard method is adopted in the described quantitative test of step (4), the caffeic acid series standard working solution of preparation 10ng/mL～300ng/mL, concentration gradient is more than 5 and be uniformly distributed, the concentration of the contained internal standard compound of standard solution at different levels is 90-110ng/mL, utilize the high performance liquid chromatography-tandem mass instrument to detect standard solution, using the ratio of the caffeic acid peak area that obtains and interior mark peak area as ordinate, caffeic acid concentration and internal standard compound concentration ratio are as horizontal ordinate, the drawing standard curve also obtains regression equation, then under the same conditions sample is detected, in the regression equation that the peak area ratio substitution of the caffeic acid that obtains and internal standard compound is obtained, can calculate caffeinic content.
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| CN103792306A (en) * | 2014-02-28 | 2014-05-14 | 江苏中烟工业有限责任公司 | GC-MS/MS combined method for detecting urotropin content in cigarette sidestream smoke |
| CN103792317A (en) * | 2014-02-28 | 2014-05-14 | 江苏中烟工业有限责任公司 | Method for detecting urotropine in cigarette side stream smoke through high performance liquid chromatography-tandem mass spectrometry |
| CN103792317B (en) * | 2014-02-28 | 2015-04-01 | 江苏中烟工业有限责任公司 | Method for detecting urotropine in cigarette side stream smoke through high performance liquid chromatography-tandem mass spectrometry |
| CN103792306B (en) * | 2014-02-28 | 2015-04-01 | 江苏中烟工业有限责任公司 | GC-MS/MS combined method for detecting urotropin content in cigarette sidestream smoke |
| CN107635478A (en) * | 2015-03-06 | 2018-01-26 | 英国质谱公司 | The fabric analysis carried out by mass spectrum or ion mobility spectrometry |
| CN113049631A (en) * | 2021-03-24 | 2021-06-29 | 海南红塔卷烟有限责任公司 | Instillation micro-extraction method for quantitative analysis of thermogravimetric escaping substances |
| CN113049631B (en) * | 2021-03-24 | 2022-10-04 | 海南红塔卷烟有限责任公司 | Instillation micro-extraction method for quantitative analysis of thermogravimetric escaping substances |
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