CN101701941A - Method fro determining content of volatile carbonyl compound in main stream smoke of cigarette - Google Patents

Method fro determining content of volatile carbonyl compound in main stream smoke of cigarette Download PDF

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CN101701941A
CN101701941A CN200910066381A CN200910066381A CN101701941A CN 101701941 A CN101701941 A CN 101701941A CN 200910066381 A CN200910066381 A CN 200910066381A CN 200910066381 A CN200910066381 A CN 200910066381A CN 101701941 A CN101701941 A CN 101701941A
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China
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cigarette
carbonyl compound
volatile carbonyl
assay
acetonitrile
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CN200910066381A
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Chinese (zh)
Inventor
王昇
夏巧玲
谢复炜
刘惠民
颜权平
刘克建
张晓纲
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中国烟草总公司郑州烟草研究院
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Priority to CN200910066381A priority Critical patent/CN101701941A/en
Publication of CN101701941A publication Critical patent/CN101701941A/en

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Abstract

The invention discloses a method for determining content of volatile carbonyl compound in main stream smoke of cigarette. 2, 4-dinitrophenylhydrazine is utilized to gather volatile carbonyl compound in main stream smoke of cigarette, so as to form hydrazone compound, and the content of the hydrazone compound is determined by a high performance liquid chromatograph by adopting external standard method; and the high performance liquid chromatograph adopts chromatographic column. The determination method of the invention adopts chromatographic column, has excellent separating effect on nitro substituted arene derivative, especially on hydrazone compound formed after reaction of 2, 4-dinitrophenylhydrazine and volatile carbonyl compound, and meanwhile chromatographic analysis condition is optimized, thus achieving complete separation of volatile carbonyl compound and interfering component in main stream smoke of cigarette and improving accuracy of determination.

Description

The assay method of content of volatile carbonyl compound in a kind of cigarette mainstream flue gas
Technical field
The present invention relates to the assay method of content of volatile carbonyl compound in a kind of cigarette mainstream flue gas, belong to tobacco and technical field of chemistry.
Background technology
Volatile carbonyl compound is one of main composition in the cigarette smoke, and wherein low grade aldehyde has the strong impulse smell, and along with the increase of molecular weight, the penetrating odor reduction also produces fragrance gradually.Relevant report (Wyder E.L., Hoffman, Tobacco and Tobacco smoke (1967), AcademicPress, New York, p417-418 and Collins.P.F., Tob.Sci. (1970) 14:p182) show, the rudimentary volatile carbonyl compound in the cigarette such as the toxicity of ciliations such as formaldehyde, acetaldehyde and acryl aldehyde, the breathing decorum and the sense organ of meeting stimulation human body in various degree in the sucking process of cigarette, long-term suction meeting causes serious harm to human body.Along with domestic and international increase day by day to smoking and health problem concern, the volatile carbonyl compound in the analysis of cigarette main flume of system, and the content of quantitative these volatile carbonyl compounds of mensuration seems very necessary.At present, the assay method that passes through to be adopted mainly contains spectrophotometric method, gas sampling method, paper chromatography, high performance liquid chromatography and vapor-phase chromatography, wherein utilize 2, the 4-dinitrophenylhydrazine can be generated as the character of comparatively stable hydrazone compounds with the volatile carbonyl compound reaction under acid condition, adopt vapor-phase chromatography (GC) or high performance liquid chromatography (HPLC) all can accurately detect this hydrazone compounds.
Crotonaldehyde is representational objectionable constituent in the cigarette smoke volatile carbonyl compound, is the index composition of evaluating cigarette harmfulness height.The analytical approach of crotonaldehyde is mainly vapor-phase chromatography (GC), GC-MS(gas chromatography-mass spectrography) (GC/MS) and liquid chromatography (LC), liquid chromatograph mass spectrography method (LC/MS), assay method in the existing industry standard " the mensuration high performance liquid chromatography of main volatile carbonyls in the cigarette mainstream flue gas " (YC/T 254-2008) is: use to add DNPH (2, the 4-dinitrophenylhydrazine) cambridge filter of derivatization reagent captures the crotonaldehyde in the cigarette mainstream flue gas, generate the DNPH derivant of crotonaldehyde, carry out separation detection with the liquid chromatography of being furnished with ultraviolet or diode array detector then.Crotonaldehyde is the minimum component of content in the cigarette mainstream flue gas main volatile carbonyls, and through spectrum and mass spectrophotometry, interfering component is all more similar with character to the structure of crotonaldehyde, and the difficulty of separating fully on chromatogram is very big, has therefore influenced the accuracy of measuring.
Summary of the invention
The assay method that the purpose of this invention is to provide content of volatile carbonyl compound in the high cigarette mainstream flue gas of a kind of good separating effect, detection accuracy.
In order to realize above purpose, the assay method of content of volatile carbonyl compound is in the cigarette mainstream flue gas of the present invention: utilize 2, the 4-dinitrophenylhydrazine captures the formation hydrazone compounds to the volatile carbonyl compound in the cigarette mainstream flue gas, utilizes high performance liquid chromatograph to adopt external standard method that this hydrazone compounds content is measured; The liquid-phase chromatographic column that is adopted in the described high performance liquid chromatograph is The Explosive chromatographic column.
Other parameter of described high performance liquid chromatograph is:
Detecting device: ultraviolet or diode array detector;
Sample size: 1-50 microlitre;
Flow velocity: 0.5-1.5ml/min;
Moving phase: deionized water and acetonitrile;
Temperature: 20 ℃-60 ℃;
Gradient elution: the acetonitrile solution of 0min 40%-70%;
The acetonitrile solution of 40min 50%-100%;
Detect wavelength: 365nm or 380nm.
Described volatile carbonyl compound comprises formaldehyde, acetaldehyde, acetone, acryl aldehyde, propionic aldehyde, crotonaldehyde, 2-butanone or butyraldehyde.
Described assay method specifically comprises the steps:
1) preparation of solution:
2,4 dinitrophenyl hydrazine reagent preparation: take by weighing the 2,4 dinitrophenyl hydrazine solid and be dissolved in the acetonitrile solvent, add perchloric acid, use the acetonitrile constant volume;
The preparation of standard solution: the 2,4 dinitrophenyl hydrazine derivative compound standard items with volatile carbonyl compound to be measured are solute, are mixed with the standard solution of 3 above variable concentrations gradients;
2) cigarette mainstream flue gas sample collection: two glass fibre filter discs are stacked, soak into described filter disc with 2,4 dinitrophenyl hydrazine reagent, then cigarette mainstream flue gas is captured by above-mentioned filter disc, placement treats that volatile carbonyl compound fully reacts in 2,4 dinitrophenyl hydrazine and the main flume;
3) processing of sample: the filter disc after will collecting extracts with the acetonitrile solution of pyridine, and filter the extraction back;
4) detect: utilize high performance liquid chromatograph that the standard solution of various concentration is detected respectively, the chromatographic peak area of the volatile carbonyl compound that obtains and the concentration of respective standard solution are drawn the typical curve of various volatile carbonyl compounds respectively and obtained regression equation, under the same conditions sample is detected then, the chromatographic peak area of the volatile carbonyl compound to be measured that obtains is brought in the corresponding regression equation, obtained the content of corresponding volatile carbonyl compound in the sample.
The mass concentration 0.01-0.05g/ml of described 2,4 dinitrophenyl hydrazine, the percent by volume of perchloric acid is 0.1-0.5%.
Described standard solution is 8 variable concentrations gradients.
Described standard solution is to be 0.14~39.44 μ g/ml in concentration.
Step By Condition to the suction of cigarette when described cigarette mainstream flue gas is collected is: with cigarette balance 48 hours under 22 ± 1 ℃, relative humidity 60 ± 2% conditions, under this condition, use smoking machine that cigarette is aspirated then, the main flume of suction is collected by filter disc, every mouthful was aspirated 2 seconds, draw volume 35mL, every mouthful of interval 58 seconds, 2 cigarette of every group of suction.
The percent by volume of the pyridine in the acetonitrile solution of described pyridine is 1-5%.
The described filtration of step 3) is the membrane filtration that adopts 0.45 μ m.
Assay method of the present invention utilizes high performance liquid chromatography that the content of volatile carbonyl compound in the cigarette mainstream flue gas is measured, and wherein the chromatographic column that is adopted is The Explosive chromatographic column, the arene derivatives that nitro is replaced has splendid separating effect, particularly to the present invention 2, the reacted hydrazone compounds of 4-dinitrophenylhydrazine and volatile carbonyl compound has good separating effect, also chromatographiccondition is optimized simultaneously, reached separating fully of volatility carbonyl compound and interfering component in the cigarette smoke, thereby improved the accuracy of measuring, especially for crotonaldehyde, and acetaldehyde DNPH derivant, the mensuration effect of the cis-trans-isomer of propionic aldehyde DNPH derivant and 2-butanone DNPH derivant has reached the separation of baseline.
Description of drawings
Fig. 1 is the chromatogram of standard solution;
Fig. 2 is the chromatogram enlarged drawing of two kinds of isomeride of acetaldehyde DNPH derivant among Fig. 1,1,2 chromatographic peaks that are respectively two kinds of isomeride of acetaldehyde DNPH derivant among the figure;
Fig. 3 is the chromatogram enlarged drawing of two kinds of isomeride of propionic aldehyde DNPH derivant among Fig. 1,3,4 chromatographic peaks that are respectively two kinds of isomeride of propionic aldehyde DNPH derivant among the figure;
Fig. 4 is the chromatogram enlarged drawing of two kinds of isomeride of 2-butanone DNPH derivant among Fig. 1,5,6 chromatographic peaks that are respectively two kinds of isomeride of 2-butanone DNPH derivant among the figure;
Fig. 5 is the chromatogram of volatile carbonyl compound in certain plate cigarette mainstream flue gas, and 8 retention time is 32.27min among the figure;
Fig. 6 is the enlarged drawing of crotonaldehyde part among Fig. 5;
Fig. 7 is the chromatogram of cigarette sample A;
Fig. 8 is the chromatogram of cigarette sample B, and 6 retention time is 29.80min among the figure;
Fig. 9 is the chromatogram of cigarette sample C, and 8 retention time is 32.30min among the figure;
Mark among Fig. 1,5,7,8,9 is the chromatographic peak of volatile carbonyl compound, wherein 1 is formaldehyde DNPH derivant, 2 is acetaldehyde DNPH derivant, 3 is acetone DNPH derivant, 4 is third rare aldehyde DNPH derivant, and 5 is propionic aldehyde DNPH derivant, and 6 is crotonaldehyde DNPH derivant, 7 is 2-butanone DNPH derivant, and 8 is butyraldehyde DNPH derivant.
Embodiment
Below the assay method of content of volatile carbonyl compound in the cigarette mainstream flue gas of the present invention is further detailed:
1, instrument and reagent
The high performance liquid chromatograph of being furnished with automatic sampler and column oven, diode array detector or UV-detector, smoking machine, ten thousand/electronic balance, ultrapure water (R>18M Ω), acetonitrile (chromatographically pure); The DNPH derivative compound standard items of formaldehyde, acetaldehyde, acetone, acryl aldehyde, propionic aldehyde, crotonaldehyde, 2-butanone, butyraldehyde; 2,4 dinitrophenyl hydrazine, pyridine and perchloric acid (analytical reagent).
2, the preparation of solution
DNPH derivatization reagent preparation: take by weighing 1.5g and be dissolved in about 80mL acetonitrile through the DNPH solid of acetonitrile recrystallization ethanol, add 200 μ L perchloric acid after, the use acetonitrile is settled to 100mL.
Standard solution preparation: formaldehyde, acetaldehyde, acetone, acryl aldehyde, propionic aldehyde, crotonaldehyde, 2-butanone, butyraldehyde 2 in the 50mL beaker about the about 50mg of difference weighing, 4-dinitrophenylhydrazone derivative compound (being the DNPH derivative compound) standard items, accurately to 0.0001g, add after about 80mL acetonitrile dissolves fully, be transferred in the volumetric flask of 100mL, be settled to scale with acetonitrile.
Pipette the 10mL standard reserving solution to the 50mL volumetric flask, be diluted to scale, be primary standard solution with the acetonitrile constant volume.Accurately pipette 0.1mL, 0.2mL, 0.5mL, 1mL, 5mL, 10mL, 25mL primary standard solution respectively to the 50mL volumetric flask, be settled to the standard solution that scale obtains other 7 variable concentrations with acetonitrile, with these 7 standard solution and primary standard solution feed liquor analysis of hplc, production standard curve.
3, the capture of sample
The processing of glass fibre filter disc and preparation: two glass fibre filter discs are stacked, evenly add the 2mLDNPH derivatization reagent, dry in being positioned in the vacuum dryer with transfer pipet.Before cigarette smoking, on the filter disc that dries, accurately add the 1mLDNPH derivatization reagent.
The suction of cigarette: with cigarette balance 48 hours under 22 ± 1 ℃, relative humidity 60 ± 2% conditions, under this condition, adopt smoking machine that cigarette is aspirated then, the main flume of suction is captured by the glass fibre filter disc.Every mouthful of suction 2 seconds, draw volume 35mL, every mouthful of interval 58 seconds, 2 cigarette of every group of suction.
Sample extraction: take out and capture the glass fibre filter disc that the main flume granule phase substance is arranged, be transferred in the 100mL conical flask, accurately add the acetonitrile solution that 50mL contains the pyridine of 2% (v/v) with transfer pipet, mechanical oscillation 10min, leave standstill 2min, get an amount of extract with 0.45 μ m membrane filtration after, move on in the 2mL chromatogram bottle, can carry out liquid-phase chromatographic analysis.
4, detect
The high performance liquid chromatograph condition:
Detecting device: ultraviolet or diode array detector;
Liquid-phase chromatographic column: The Explosive liquid-phase chromatographic column;
Sample size: 1-50 microlitre;
Flow velocity: 0.5-1.5ml/min;
Moving phase: deionized water and acetonitrile;
Temperature: 20 ℃-60 ℃;
Gradient elution: the acetonitrile solution of 0min 40%-70%,
The acetonitrile solution of 40min 50%-100%;
Detect wavelength: 365nm or 380nm.
Detect step: at first the standard solution with various concentration carries out the high performance liquid chromatography detection, obtain the chromatographic peak area (deduction is blank) of various volatile carbonyl compounds to be measured, concentration according to chromatographic peak area and respective standard solution obtains calibration curve then, calculate the regression equation of calibration curve, the testing result of various volatile carbonyl compound standard models is as shown in table 1:
The testing result of the various volatile carbonyl compound standard models of table 1
Compound Content (μ g/ml) Regression equation Related coefficient Retention time (min)
Formaldehyde ??0.14-14.38 ??y=4957x-35.712 ??0.9998 ??11.67
Acetaldehyde ??0.39-39.44 ??y=4100x+79.479 ??0.9999 ??16.03
Acetone ??0.24-24.19 ??y=3139x+48.929 ??0.9999 ??21.98
Acryl aldehyde ??0.18-17.87 ??y=3994x+0.9805 ??0.9999 ??23.28
Propionic aldehyde ??0.15-15.01 ??y=2894x+63.484 ??0.9999 ??25.55
Crotonaldehyde ??0.15-14.57 ??y=3357x-71.047 ??0.9999 ??29.78
The 2-butanone ??0.17-16.86 ??y=3230x+59.728 ??0.9999 ??30.88
Butyraldehyde ??0.15-15.49 ??y=4763x-14.99 ??0.9999 ??32.27
Secondly, adopt identical method that sample is detected, obtain the chromatographic peak area (deduction is blank) of each volatile carbonyl compound in the sample, then chromatographic peak area is brought in the corresponding regression equation, obtain the content of corresponding volatile carbonyl compound in the sample.
Fig. 1 is the chromatogram of standard solution, from the figure as can be seen, adopt liquid chromatography detecting method of the present invention that various volatile carbonyl compound DNPH derivants are had good separating effect, and realized the baseline separation (shown in Fig. 2,3,4) of acetaldehyde DNPH derivant, propionic aldehyde DNPH derivant and 2-butanone DNPH derivant cis-trans-isomer.For the stratographic analysis of certain brand cigarette sample as shown in Figure 5, each volatile carbonyl compound also has good separating effect, guarantee the accuracy that each volatile carbonyl compound is quantitative, particularly for crotonaldehyde, as shown in Figure 6, realize baseline separation, further improved the accuracy of separating effect and detection.
5, the precision of assay method of the present invention, the recovery and detectability are as shown in table 2:
The precision of table 2 method, the recovery and detectability result
Carbonyls Formaldehyde Acetaldehyde Acetone Acryl aldehyde Propionic aldehyde Crotonaldehyde The 2-butanone Butyraldehyde
Precision (n=5) (%) ??8.0 ??6.4 ??4.8 ??8.8 ??8.3 ??6.1 ??4.0 ??4.8
The recovery (%) ??100.7 ??98.7 ??97.0 ??93.6 ??93.7 ??92.4 ??95.2 ??93.4
Detectability (μ g/mL) ??0.035 ??0.096 ??0.090 ??0.039 ??0.053 ??0.044 ??0.056 ??0.075
6, the calculating of content
The measurement result of 8 kinds of volatile carbonyl compounds in the main flume of every cigarette, calculate according to following formula:
m = A × L n
In the formula:
M is the transmission quantity of volatile carbonyl compound in every cigarette mainstream flue gas, and unit is every of microgram (μ g/cig);
A is the concentration of volatile carbonyl compound in the extraction sample, and unit is every milliliter of microgram (μ g/mL);
L is extraction solution volume (mL);
N is the number of each test smoking cigarette, and unit is (cig);
Embodiment
Adopt the assay method that further specifies in the embodiment, cigarette sample A, B, C are detected, the chromatographic condition that is adopted is as shown in table 3 with the difference that further specifies:
The difference chromatographic condition of table 3 embodiment
Sample Sample size Flow velocity Temperature Detect wavelength DNPH concentration (g/ml) The perchloric acid percent by volume The percent by volume of pyridine solution
??A ??10μL ??0.5ml/min ??20℃ ??365nm ??0.01 ??0.3% ??1%
??B ??50μL ??1ml/min ??40℃ ??365nm ??0.05 ??0.1% ??3%
??C ??20μL ??1.5ml/min ??60℃ ??380nm ??0.03 ??0.5% ??5%
Other chromatographic condition such as moving phase are identical with the chromatographic condition that further specifies of the present invention with gradient elution etc.The chromatogram that detection obtains is respectively shown in Fig. 7,8,9.The results are shown in Table shown in 4 after final the calculating.
Transmission quantity (the unit: μ g/cig) of volatile carbonyl compound in three kinds of sample cigarette mainstream flue gas of table 4
Compound ??A ??B ??C
Formaldehyde ??118.38 ??25.47 ??131.71
Acetaldehyde ??560.07 ??590.49 ??607.97
Acetone ??210.51 ??259.32 ??228.76
Acryl aldehyde ??59.67 ??37.58 ??71.97
Propionic aldehyde ??41.27 ??45.58 ??48.88
Crotonaldehyde ??17.16 ??14.65 ??16.35
The 2-butanone ??43.73 ??66.06 ??49.49
Butyraldehyde ??33.52 ??36.68 ??37.08

Claims (10)

1. the assay method of content of volatile carbonyl compound in the cigarette mainstream flue gas, it is characterized in that: utilize 2, the 4-dinitrophenylhydrazine captures the formation hydrazone compounds to the volatile carbonyl compound in the cigarette mainstream flue gas, utilizes high performance liquid chromatograph to adopt external standard method that this hydrazone compounds content is measured; The liquid-phase chromatographic column that is adopted in the described high performance liquid chromatograph is The Explosive chromatographic column.
2. assay method according to claim 1 is characterized in that: other parameter of described high performance liquid chromatograph is:
Detecting device: ultraviolet or diode array detector;
Sample size: 1-50 microlitre;
Flow velocity: 0.5-1.5ml/min;
Moving phase: deionized water and acetonitrile;
Temperature: 20 ℃-60 ℃;
Gradient elution: the acetonitrile solution of 0min 40%-70%;
The acetonitrile solution of 40min 50%-100%;
Detect wavelength: 365nm or 380nm.
3. assay method according to claim 1 is characterized in that: described volatile carbonyl compound comprises formaldehyde, acetaldehyde, acetone, acryl aldehyde, propionic aldehyde, crotonaldehyde, 2-butanone or butyraldehyde.
4. according to claim 1 or 2 or 3 described assay methods, it is characterized in that: specifically comprise the steps:
1) preparation of solution:
2,4 dinitrophenyl hydrazine reagent preparation: take by weighing the 2,4 dinitrophenyl hydrazine solid and be dissolved in the acetonitrile solvent, add perchloric acid, use the acetonitrile constant volume;
The preparation of standard solution: the 2,4 dinitrophenyl hydrazine derivative compound standard items with volatile carbonyl compound to be measured are solute, are mixed with the standard solution of 3 above variable concentrations gradients;
2) cigarette mainstream flue gas sample collection: two glass fibre filter discs are stacked, soak into described filter disc with 2,4 dinitrophenyl hydrazine reagent, then cigarette mainstream flue gas is captured by above-mentioned filter disc, placement treats that volatile carbonyl compound fully reacts in 2,4 dinitrophenyl hydrazine and the main flume;
3) processing of sample: the filter disc after will collecting extracts with the acetonitrile solution of pyridine, and filter the extraction back;
4) detect: utilize high performance liquid chromatograph that the standard solution of various concentration is detected respectively, the chromatographic peak area of the volatile carbonyl compound that obtains and the concentration of respective standard solution are drawn the typical curve of various volatile carbonyl compounds respectively and obtained regression equation, under the same conditions sample is detected then, the chromatographic peak area of the volatile carbonyl compound to be measured that obtains is brought in the corresponding regression equation, obtained the content of corresponding volatile carbonyl compound in the sample.
5. assay method according to claim 4 is characterized in that: the mass concentration 0.01-0.05g/ml of described 2,4 dinitrophenyl hydrazine, the percent by volume of perchloric acid is 0.1-0.5%.
6. assay method according to claim 4 is characterized in that: described standard solution is 8 variable concentrations gradients.
7. assay method according to claim 4 is characterized in that: described standard solution is to be 0.14~39.44 μ g/ml in concentration.
8. assay method according to claim 4, it is characterized in that: the Step By Condition to the suction of cigarette when described cigarette mainstream flue gas is collected is: with cigarette balance 48 hours under 22 ± 1 ℃, relative humidity 60 ± 2% conditions, under this condition, use smoking machine that cigarette is aspirated then, the main flume of suction is collected by filter disc, every mouthful was aspirated 2 seconds, draw volume 35mL, every mouthful of interval 58 seconds, 2 cigarette of every group of suction.
9. assay method according to claim 4 is characterized in that: the percent by volume of the pyridine in the acetonitrile solution of described pyridine is 1-5%.
10. assay method according to claim 4 is characterized in that: the described filtration of step 3) is the membrane filtration that adopts 0.45 μ m.
CN200910066381A 2009-11-05 2009-11-05 Method fro determining content of volatile carbonyl compound in main stream smoke of cigarette CN101701941A (en)

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