CN103698458A - Method for measuring main carbonyl compounds in main stream smoke of cigarette through ultra high performance convergence chromatography - Google Patents

Method for measuring main carbonyl compounds in main stream smoke of cigarette through ultra high performance convergence chromatography Download PDF

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CN103698458A
CN103698458A CN201310736700.2A CN201310736700A CN103698458A CN 103698458 A CN103698458 A CN 103698458A CN 201310736700 A CN201310736700 A CN 201310736700A CN 103698458 A CN103698458 A CN 103698458A
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cigarette
main
solution
ultra
carbonyl compounds
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CN201310736700.2A
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CN103698458B (en
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张洪非
唐纲岭
姜兴益
吴帅宾
李中皓
范子彦
边照阳
刘珊珊
杨飞
王颖
张艳革
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国家烟草质量监督检验中心
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Abstract

A method for measuring main carbonyl compounds in a main stream smoke of a cigarette through ultra high performance convergence chromatography is a method for measuring butyraldehyde, 2-butanone, propionaldehyde, crotonaldehyde, acrolein, acetone, acetaldehyde and formaldehyde in the main stream smoke. The method is characterized in that a filter leaf processed with a derivatization reagent is used to gather the main carbonyl compounds in the main stream smoke of the cigarette, the analyzing and measuring method is used to obtain the contents of the eight carbonyl compounds in the main stream smoke through ultra high performance convergence chromatography (UPC2). When the method provided by the invention is used to detect the contents of the main carbonyl compounds in the main stream smoke of the cigarette rapidly and effectively, the pretreatment is simple, the average relative standard deviation is less than 7%, and the average recovery rate of various indexes is between 75%-94%. The method has the advantages of rapidness, accuracy, high flexibility and good repeatability.

Description

A kind of method of using ultra high efficiency to close phase chromatographic determination main carbonyl compounds in main stream cigarette smoke
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Technical field
The invention belongs to the physical and chemical inspection technical field of cigarette mainstream flue gas, a kind of method that use ultra high efficiency is closed phase chromatographic determination main carbonyl compounds in main stream cigarette smoke (butyraldehyde, 2-butanone, propionic aldehyde, crotonaldehyde, acryl aldehyde, acetone, acetaldehyde, formaldehyde) specifically, the method is quick, efficient, environmental protection, be conducive to improve the efficiency that carbonyls in cigarette mainstream flue gas is detected, greatly reduce the loss of organic solvent, reduce the pollution to environment simultaneously.
Background technology
Carbonyls is the important objectionable constituent of a class in cigarette mainstream flue gas, the control composition inventory that is put into 46 kinds of objectionable constituent lists of Canadian government and WHO " tobacco product control research group " suggestion, thereby the volatilization carbonyls in Accurate Determining cigarette smoke is significant for cigarette Evaluation of Harmfulness.At present, in domestic relevant cigarette mainstream flue gas, the detection of carbonyls generally adopts the high performance liquid chromatography of < < YC/T 254-2008 > > defined, the shortcoming of the method is that the sample determination time is long, consumes organic solvent many.Ultra high efficiency is closed phase chromatogram (Ultra performance convergence chromatography, UPC 2) technology is a kind of isolation technics proposing recently, it comes from supercritical fluid chromatography technology, because it is with supercritical CO 2therefore for main mobile phase, have that viscosity is low, mass-transfer performance good, separation efficiency is high, the advantage of environmental protection; Meanwhile, the UPLC of this system based on Waters maturation tMtechnology platform, and the chromatographic column chemical technology of sub-2 μ m, make instrument can handling, there is the progress of a matter aspect such as reappearance, precision.
Therefore, adopt UPC 2set up a kind of can be fast, the method for carbonyls is necessary in the mensuration cigarette mainstream flue gas of efficient, environmental protection, and current open source literature there is not yet the relevant report of this type of technology.
summary of the invention:
Object of the present invention is intended to overcome prior art defect, and a kind of use UPC is provided 2measure the method for carbonyls in cigarette mainstream flue gas.Utilize assay method provided by the invention, the content that energy fast, efficient, environmental protection ground detects carbonyls in cigarette mainstream flue gas.
The object of the invention is to be achieved through the following technical solutions:
A kind of method of using ultra high efficiency to close phase chromatographic determination main carbonyl compounds in main stream cigarette smoke, measure the method for butyraldehyde in main flume, 2-butanone, propionic aldehyde, crotonaldehyde, acryl aldehyde, acetone, acetaldehyde, formaldehyde, to utilize the filter disc that derivatization reagent was processed to trap the main carbonyl compounds in cigarette mainstream flue gas, by efficiently closing phase chromatography (UPC 2) analyze method for measuring, and then draw the content of eight kinds of carbonyls in main flume, concrete steps are as follows:
The preparation of a, derivatization reagent: take the DNPH solid of 1.5g through purifying and add in 80mL acetonitrile, be heated to 50 ℃, vibration is dissolved, add after 200 μ L70% perchloric acid, with acetonitrile, be settled to 100mL after being cooled to room temperature, before use, be heated to 50 ℃, vibration is dissolved, and uses after being cooled to room temperature; The described DNPH solid through purifying is to be prepared from by recrystallization, concrete grammar is: get 50gDNPH and join in 800mL acetonitrile, heating is back to DNPH and dissolves completely, be transferred to that in beaker, to seal lucifuge naturally cooling, standing over night, DNPH crystallization, through suction filtration, acetonitrile washing, proceeds to the rear lucifuge low temperature of brown bottle sealing and preserves after vacuum drying.
The preparation of b, filter disc: be that 44mm glass fiber filter stacks by two diameters, with transfer pipet or liquid-transfering gun, evenly add 2mLDNPH derivatization reagent, in being positioned in vacuum dryer, lucifuge is dried, before cigarette smoking, on the filter disc drying, accurately add 1mLDNPH derivatization reagent, filter disc adds after derivatization reagent smoking cigarette at once;
The preparation of c, extraction solution: pyridine/acetonitrile (v/v) solution of configuration 2%;
The preparation of d, sample: according to GB/T 5606.1, extract cigarette samples, select the cigarette that weight and resistance to suction are qualified (weight: mean value ± 20mg, resistance to suction: mean value ± 50Pa), at 22 ± 2 ℃ of temperature and 60 ± 5% times balance 48h of relative humidity; According to GB/T16450 < < conventional analysis, with smoking machine definition and standard conditions > >, adjust and check smoking machine suction parameter, on BORGWALDT-KC 5 duct smoking machines, aspirate the cigarette after balance, with the cambridge filter of processing through derivatization reagent, collect total particulate matter in mainstream smoke; After cigarette smoking finishes, 2 mouthfuls of suctions, take out drip catcher, place 3 minutes, carbonyls in flue gas is fully reacted with DNPH, then take out filter disc, be transferred in 150mL conical flask at once, pyridine/acetonitrile (v/v) solution that accurately adds 100mL 2% with digital adjustable type bottleneck divider, mechanical oscillation 10min(oscillation frequency: 160-200 rev/min), standing 2min, gets appropriate extract with after 0.22 μ m organic phase membrane filtration, move on in 2mL chromatogram bottle, can carry out UPC 2analyze;
e,the preparation of standard operation solution : minuteaccurately do not take the acetone of 30mg, acryl aldehyde, propionic aldehyde, crotonaldehyde, 2-butanone, 2 of butyraldehyde, 4-dinitro benzene hydazone derivative standard items, 2 of 40mg formaldehyde and 50mg acetaldehyde, 4-dinitro benzene hydazone derivative standard items are to the volumetric flask of different 25mL, be accurate to 0.1mg, use respectively acetonitrile constant volume as one-level storing solution, then pipette respectively the acetaldehyde DNPH solution of 1.0mL, the acetone DNPH solution of 0.75 mL, 0.5mL formaldehyde, acryl aldehyde, propionic aldehyde, crotonaldehyde, 2-butanone, the DNPH solution of butyraldehyde is to same 25mL volumetric flask, with acetonitrile, be settled to scale, this is secondary reserves liquid, then pipette 0.05mL, 0.2mL, 0.4mL, 0.8mL, 2.0mL, 4.0mL, the secondary reserves liquid of 7.0mL and 10.0mL is to the volumetric flask of 10mL, with 8 grades of standard operation solution with finite concentration gradient of acetonitrile constant volume configuration,
F, ultra high efficiency are closed phase chromatogram (UPC 2) measure: utilize ultra high efficiency to close phase chromatogram (joining UV-detector) standard operation solution and sample preparation liquid are detected, it is as follows that its ultra high efficiency is closed the separated testing conditions of phase chromatogram:
Chromatographic column: ACQUITY UPC 2bEH 2-EP chromatographic column (1.7 μ m, 3 mm * 150 mm);
Column temperature: 40 ℃;
Mobile phase A: carbon dioxide;
Mobile phase B: methyl alcohol;
Post flow: 1.5ml/min;
Sampling volume: 1 μ L;
Gradient: binary solvent eluent gradient is as shown in table 1:
Table 1 gradient table
Detecting device: UV-detector, it is 365nm that detecting device detects wavelength.
The calculating of g, cigarette mainstream flue gas main carbonyl compounds measurement result
With external standard method, carry out the quantitative test of volatile carbonyl compound, the chromatographic peak area with target carbonyls carries out regretional analysis to its respective concentration, obtain typical curve, to prepare sample measure, record the chromatographic peak area that detects target carbonyls, substitution typical curve, obtains respectively the content of butyraldehyde in sample, 2-butanone, propionic aldehyde, crotonaldehyde, acryl aldehyde, acetone, acetaldehyde, formaldehyde.
Computing formula is:
In formula:
The content of carbonyl composition in m-every cigarette mainstream flue gas, unit is every of microgram (μ g/cig);
The concentration of carbonyls in A-extract (μ g/mL);
100-extraction solution volume (mL);
4-test the number (cig) of smoking cigarette at every turn.
 
Compared with prior art the present invention has overcome the deficiency of prior art sample detection method, has optimized instrument testing conditions, and the present invention has following effect:
(1) detection time is short: adopting the present invention to measure the main carbonyl compounds in main stream cigarette smoke cycle only needed about 10 minutes;
(2) it is accurate, highly sensitive and reproducible that the present invention has operation, the advantage of environmental protection (consuming organic reagent few).
1. the typical curve of the inventive method and detection limit:
Take butyraldehyde, 2-butanone, propionic aldehyde, crotonaldehyde, acryl aldehyde, acetone, acetaldehyde, formaldehyde as detecting index, the working stamndard solution of 8 kinds of carbonyls of preparation, through ultra high efficiency, close analysis of hplc, with object chromatographic peak area, its respective concentration is carried out to regretional analysis, obtain typical curve and regression equation thereof, related coefficient, utilizing least concentration mark liquid signal to noise ratio (S/N ratio) is to calculate detection limit at 3 o'clock.As shown in Table 2, the chromatographic condition adopting makes 8 kinds of carbonyls have compound chromatographic peak all better separated, and all has good correlativity, and detection limit is between 0.07 μ g/cig-0.15 μ g/cig.
Typical curve and the detection limit of table 2 cigarette mainstream flue gas carbonyls
Note: 1. detection limit calculates with 3 times of signal to noise ratio (S/N ratio)s (S/N=3).
2. the repeatability of the inventive method and recovery of standard addition:
The recovery of table 3 cigarette mainstream flue gas carbonyls and repeatability (n=5)
Sample is carried out to the standard solution recovery of standard addition test of high, medium and low variable concentrations level, each sample is measured respectively 5 times, calculate the various main carbonyl compounds in main stream cigarette smokes of this method the recovery and mark-on after the relative standard deviation of measured value, the results are shown in Table 3.As can be seen from Table 3, in 3 mark-on levels, utilize the recovery of the method detection main carbonyl compounds in main stream cigarette smoke between 75% ~ 94%.The mean relative deviation of sample test result is less than 7%; The recovery that this law is described is higher, and repeatability better.
Accompanying drawing explanation
Fig. 1 assay method process flow diagram of the present invention;
The mixed mark of Fig. 2 solution chromatogram;
Fig. 3 cigarette sample chromatogram.
In Fig. 2,3: 1. butyraldehyde, 2.2-butanone, 3. propionic aldehyde, 4. crotonaldehyde, 5. acryl aldehyde, 6. acetone, 7. acetaldehyde, 8. formaldehyde.
Embodiment
The present invention is described further in conjunction with example.
Example 1:
1. reagent and instrument:
Standard items: 2 of formaldehyde, acetaldehyde, acetone, acryl aldehyde, propionic aldehyde, crotonaldehyde, 2-butanone, butyraldehyde, 4-dinitro benzene hydazone derivative standard items (TCI company);
Reagent: acetonitrile, methyl alcohol (chromatographically pure, Korea S Duksan pure chemicals company).Carbon dioxide (food stage, Henan Yuan Zheng development in science and technology company limited).Experimental water is the made deionized water of Milli-Q pure water system; DNPH (DNPH) is analytical reagent (recrystallization before using); Perchloric acid is analytical reagent;
Instrument: BORGWALDT-KC 5 duct effluent smoking machines (BORGWALDT-KC, German); Water generation ACQUITY UPC 2system, joins ACQUITY UPC 2pDA detecting device (U.S. Waters company).ACQUITY UPC 2bEH 2-EP chromatographic column (1.7 μ m, 3 mm * 150 mm) (U.S. Waters company).GB204 electronic balance, sensibility reciprocal: 0.0001 g(Switzerland Mettler company).Kunshan KQ-700DB table type numerical control Ultrasound Instrument (Kunshan Ultrasonic Instruments Co., Ltd.).Organic phase pin type filter, 13 mm * 0.22 μ m(Town in Shanghai spectrum scientific instrument company limiteds).
2. sample preparation:
According to GB/T 5606.1, extract cigarette samples, select the cigarette that weight and resistance to suction are qualified (weight: mean value ± 20mg, resistance to suction: mean value ± 50Pa), at 22 ± 2 ℃ of temperature and 60 ± 5% times balance 48h of relative humidity; According to GB/T16450 < < conventional analysis, with smoking machine definition and standard conditions > >, adjust and check smoking machine suction parameter, on BORGWALDT-KC 5 duct smoking machines, aspirate the cigarette after balance, with the cambridge filter of processing through derivatization reagent, collect total particulate matter in mainstream smoke; After cigarette smoking finishes, 2 mouthfuls of suctions, take out drip catcher, place 3 minutes, carbonyls in flue gas is fully reacted with DNPH, then take out filter disc, be transferred in 150mL conical flask at once, pyridine/acetonitrile (v/v) solution that accurately adds 100mL 2% with digital adjustable type bottleneck divider, mechanical oscillation 10min(oscillation frequency: 160-200 rev/min), standing 2min, gets appropriate extract with after 0.22 μ m organic phase membrane filtration, move on in 2mL chromatogram bottle, can carry out UPC 2analyze;
3. standard operation solution preparation:
Standard operation solution preparation: accurately take respectively 30mg acetone, acryl aldehyde, propionic aldehyde, crotonaldehyde, 2-butanone, butyraldehyde 2,4-dinitro benzene hydazone derivative standard items, 2 of 40mg formaldehyde and 50mg acetaldehyde, 4-dinitro benzene hydazone derivative standard items are to the volumetric flask of different 25mL, be accurate to 0.1mg, use respectively acetonitrile constant volume as one-level storing solution, this solution is sealed in 4 ℃ and deposits, and the term of validity is 1 year; Then pipette respectively the acetaldehyde DNPH solution of 1.0mL, the acetone DNPH solution of 0.75 mL, the DNPH solution of 0.5mL formaldehyde, acryl aldehyde, propionic aldehyde, crotonaldehyde, 2-butanone, butyraldehyde is to 25mL volumetric flask, with acetonitrile, be settled to scale, this is secondary reserves liquid, be sealed in 4 ℃ and deposit, the term of validity is 20 days; Then pipette the secondary reserves liquid of 0.05mL, 0.2mL, 0.4mL, 0.8mL, 2.0mL, 4.0mL, 7.0mL and 10.0mL to the volumetric flask of 10mL, with 8 grades of standard operation solution with finite concentration gradient of acetonitrile constant volume configuration, the term of validity is 20 days.Standard solution is placed in Refrigerator store, is placed under normal temperature while taking, and can use after reaching normal temperature.Each index concentration is as shown in table 4:
Table 4 concentration of standard solution
Title 1#μg/mL 2#μg/mL 3#μg/mL 4#μg/mL 5#μg/mL 6#μg/mL 7#μg/mL 8#μg/mL
Butyraldehyde 0.0265 0.1061 0.2122 0.4243 1.0608 2.1216 3.7128 5.3040
2-butanone 0.0312 0.1250 0.2500 0.5000 1.2499 2.4998 4.3747 6.2495
Propionic aldehyde 0.0303 0.1211 0.2423 0.4846 1.2115 2.4230 4.2402 6.0574
Crotonaldehyde 0.0305 0.1222 0.2444 0.4888 1.2220 2.4440 4.2769 6.1099
Acryl aldehyde 0.0305 0.1221 0.2441 0.4882 1.2205 2.4411 4.2719 6.1027
Acetone 0.0455 0.1818 0.3637 0.7274 1.8184 3.6368 6.3643 9.0919
Acetaldehyde 0.0844 0.3375 0.6749 1.3499 3.3747 6.7494 11.8114 16.8734
Formaldehyde 0.0226 0.0904 0.1807 0.3614 0.9035 1.8070 3.1623 4.5176
4. assay method:
Chromatographic peak area with target carbonyls carries out regretional analysis to its respective concentration, obtains typical curve.The sample preparing is measured, recorded the chromatographic peak area that detects target carbonyls, substitution typical curve, obtains respectively the content of butyraldehyde in sample, 2-butanone, propionic aldehyde, crotonaldehyde, acryl aldehyde, acetone, acetaldehyde, formaldehyde, the results are shown in Table 5.
Table 5 main carbonyl compounds in main stream cigarette smoke testing result
Compound Content (μ g/cig)
Butyraldehyde 42.2
2-butanone 62.5
Propionic aldehyde 58.5
Crotonaldehyde 20.2
Acryl aldehyde 60.5
Acetone 248
Acetaldehyde 574.8
Formaldehyde 82.7
Ultra high efficiency is closed the separated testing conditions of phase chromatogram:
Chromatographic column: ACQUITY UPC 2bEH 2-EP chromatographic column (1.7 μ m, 3 mm * 150 mm)
Column temperature: 40 ℃;
Mobile phase A: carbon dioxide;
Mobile phase B: methyl alcohol;
Post flow: 1.5ml/min;
Sampling volume: 1 μ L;
Gradient: binary solvent eluent gradient is as shown in table 1;
Detecting device: UV-detector;
Select excellently, it is 365nm that detecting device detects wavelength.
 
Example 2:
Concrete steps as described in Example 1, are selected another trade mark cigarette (sample B), record the content of main carbonyl compounds in main stream cigarette smoke in Table 6.
Table 6 main carbonyl compounds in main stream cigarette smoke testing result
Compound Content (μ g/cig)
Butyraldehyde 39.6
2-butanone 57.6
Propionic aldehyde 61.9
Crotonaldehyde 20.4
Acryl aldehyde 70
Acetone 246.5
Acetaldehyde 606.5
Formaldehyde 108.2
Example 3:
Concrete steps as described in Example 1, are selected another trade mark cigarette (sample C), record the content of main carbonyl compounds in main stream cigarette smoke in Table 7.
Table 7 main carbonyl compounds in main stream cigarette smoke testing result
Compound Content (μ g/cig)
Butyraldehyde 40.9
2-butanone 58.5
Propionic aldehyde 63.2
Crotonaldehyde 22.3
Acryl aldehyde 71.3
Acetone 245.8
Acetaldehyde 596.2
Formaldehyde 108.8
Example 4:
Concrete steps as described in Example 1, are selected objectionable constituent reference cigarette (sample D), record the content of main carbonyl compounds in main stream cigarette smoke in Table 8.
Table 8 main carbonyl compounds in main stream cigarette smoke testing result
Compound Content (μ g/cig)
Butyraldehyde 44.9
2-butanone 64.7
Propionic aldehyde 62.1
Crotonaldehyde 21.8
Acryl aldehyde 65.8
Acetone 270.1
Acetaldehyde 627.0
Formaldehyde 73.5

Claims (4)

1. a method of using ultra high efficiency to close phase chromatographic determination main carbonyl compounds in main stream cigarette smoke, measure the method for butyraldehyde in main flume, 2-butanone, propionic aldehyde, crotonaldehyde, acryl aldehyde, acetone, acetaldehyde, formaldehyde, it is characterized in that: be to utilize the filter disc that derivatization reagent was processed to trap the main carbonyl compounds in cigarette mainstream flue gas, by efficiently closing phase chromatography (UPC 2) analyze method for measuring, and then draw the content of eight kinds of carbonyls in main flume, concrete steps are as follows:
The preparation of a, derivatization reagent: take the DNPH solid of 1.5g through purifying and add in 80mL acetonitrile, be heated to 50 ℃, vibration is dissolved, add after 200 μ L70% perchloric acid, with acetonitrile, be settled to 100mL after being cooled to room temperature, before use, be heated to 50 ℃, vibration is dissolved, and uses after being cooled to room temperature;
The preparation of b, filter disc: be that 44mm glass fiber filter stacks by two diameters, with transfer pipet or liquid-transfering gun, evenly add 2mLDNPH derivatization reagent, in being positioned in vacuum dryer, lucifuge is dried, before cigarette smoking, on the filter disc drying, accurately add 1mLDNPH derivatization reagent, filter disc adds after derivatization reagent smoking cigarette at once;
The preparation of c, extraction solution: pyridine/acetonitrile (v/v) solution of configuration 2%;
The preparation of d, sample: according to GB/T 5606.1, extract cigarette samples, select the cigarette that weight and resistance to suction are qualified (weight: mean value ± 20mg, resistance to suction: mean value ± 50Pa), at 22 ± 2 ℃ of temperature and 60 ± 5% times balance 48h of relative humidity; According to GB/T16450 < < conventional analysis, with smoking machine definition and standard conditions > >, adjust and check smoking machine suction parameter, on BORGWALDT-KC 5 duct smoking machines, aspirate the cigarette after balance, with the cambridge filter of processing through derivatization reagent, collect total particulate matter in mainstream smoke; After cigarette smoking finishes, 2 mouthfuls of suctions, take out drip catcher, place 3 minutes, carbonyls in flue gas is fully reacted with DNPH, then take out filter disc, be transferred in 150mL conical flask at once, pyridine/acetonitrile (v/v) solution that accurately adds 100mL 2% with digital adjustable type bottleneck divider, mechanical oscillation 10min(oscillation frequency: 160-200 rev/min), standing 2min, gets appropriate extract with after 0.22 μ m organic phase membrane filtration, move on in 2mL chromatogram bottle, can carry out UPC 2analyze;
E, standard operation solution preparation: the acetone that accurately takes respectively 30mg, acryl aldehyde, propionic aldehyde, crotonaldehyde, 2-butanone, 2 of butyraldehyde, 4-dinitro benzene hydazone derivative standard items, 2 of 40mg formaldehyde and 50mg acetaldehyde, 4-dinitro benzene hydazone derivative standard items are to the volumetric flask of different 25mL, be accurate to 0.1mg, use respectively acetonitrile constant volume as one-level storing solution, then pipette respectively the acetaldehyde DNPH solution of the 1.0mL in aforementioned one-level storing solution, the acetone DNPH solution of 0.75 mL, 0.5mL formaldehyde, acryl aldehyde, propionic aldehyde, crotonaldehyde, 2-butanone, the DNPH solution of butyraldehyde is to same 25mL volumetric flask, with acetonitrile, be settled to scale, this is secondary reserves liquid, then pipette 0.05mL, 0.2mL, 0.4mL, 0.8mL, 2.0mL, 4.0mL, the secondary reserves liquid of 7.0mL and 10.0mL is to the volumetric flask of 10mL, with 8 grades of standard operation solution with finite concentration gradient of acetonitrile constant volume configuration,
F, ultra high efficiency are closed phase chromatogram (UPC 2) measure: utilize ultra high efficiency to close phase chromatogram (joining UV-detector) standard operation solution and sample preparation liquid are detected;
The calculating of g, cigarette mainstream flue gas main carbonyl compounds measurement result
With external standard method, carry out the quantitative test of volatile carbonyl compound, the chromatographic peak area with target carbonyls carries out regretional analysis to its respective concentration, obtain typical curve, to prepare sample measure, record the chromatographic peak area that detects target carbonyls, substitution typical curve, obtains respectively the content of butyraldehyde in sample, 2-butanone, propionic aldehyde, crotonaldehyde, acryl aldehyde, acetone, acetaldehyde, formaldehyde.
2. the method that use ultra high efficiency according to claim 1 is closed phase chromatographic determination main carbonyl compounds in main stream cigarette smoke, it is characterized in that: the DNPH solid through purifying described in step a is to be prepared from by recrystallization, concrete grammar is: get 50gDNPH and join in 800mL acetonitrile, heating is back to DNPH and dissolves completely, be transferred to that in beaker, to seal lucifuge naturally cooling, standing over night, DNPH crystallization, through suction filtration, acetonitrile washing, proceeds to the rear lucifuge low temperature of brown bottle sealing and preserves after vacuum drying.
3. the method that use ultra high efficiency according to claim 1 is closed phase chromatographic determination main carbonyl compounds in main stream cigarette smoke, is characterized in that: it is as follows that ultra high efficiency is closed the separated testing conditions of phase chromatogram:
Chromatographic column: ACQUITY UPC 2bEH 2-EP chromatographic column (1.7 μ m, 3 mm * 150 mm);
Column temperature: 40 ℃;
Mobile phase A: carbon dioxide;
Mobile phase B: methyl alcohol;
Post flow: 1.5ml/min;
Sampling volume: 1 μ L;
Gradient: binary solvent eluent gradient is as shown in table 1:
Table 1 gradient table
Detecting device: UV-detector, it is 365nm that detecting device detects wavelength.
4. the method that use ultra high efficiency according to claim 1 is closed phase chromatographic determination main carbonyl compounds in main stream cigarette smoke, is characterized in that: in the cigarette mainstream flue gas in g step, the computing formula of carbonyls is:
In formula:
The content of carbonyl composition in m-every cigarette mainstream flue gas, unit is every of microgram (μ g/cig);
The concentration of carbonyls in A-extract (μ g/mL);
100-extraction solution volume (mL);
4-test the number (cig) of smoking cigarette at every turn.
CN201310736700.2A 2013-12-26 2013-12-26 Method for measuring main carbonyl compounds in main stream smoke of cigarette through ultra high performance convergence chromatography CN103698458B (en)

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CN106841454A (en) * 2017-03-10 2017-06-13 国家烟草质量监督检验中心 The chiral analysis of nicotine close phase chromatographic tandem mass spectrography in a kind of bolete
CN106896173A (en) * 2017-03-10 2017-06-27 国家烟草质量监督检验中心 The chiral analysis of nicotine close phase chromatographic tandem mass spectrography in a kind of electronic cigarette liquid
CN106814155A (en) * 2017-03-10 2017-06-09 国家烟草质量监督检验中心 The chiral analysis of nicotine close phase chromatographic tandem mass spectrography in a kind of tomato
CN106814155B (en) * 2017-03-10 2019-05-17 国家烟草质量监督检验中心 The chiral analysis of nicotine closes phase chromatographic tandem mass spectrography in a kind of tomato
CN106841454B (en) * 2017-03-10 2019-05-10 国家烟草质量监督检验中心 The chiral analysis of nicotine closes phase chromatographic tandem mass spectrography in a kind of bolete
CN107490636A (en) * 2017-08-09 2017-12-19 国家烟草质量监督检验中心 A kind of assay method for heating 8 kinds of carbonyls in the cigarette mainstream flue gas that do not burn
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CN108535387A (en) * 2018-07-13 2018-09-14 国家烟草质量监督检验中心 The one conjunction phase chromatographic tandem measuring method of mass spectrum for growing tobacco middle NNK and NNN
CN108535387B (en) * 2018-07-13 2020-04-28 国家烟草质量监督检验中心 Combined phase chromatography tandem mass spectrometry determination method of NNK and NNN in tobacco

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