CN108548881A - Chromatographic detection method that is a kind of while analyzing 39 kinds of phenol in cigarette mainstream flue gas - Google Patents
Chromatographic detection method that is a kind of while analyzing 39 kinds of phenol in cigarette mainstream flue gas Download PDFInfo
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Abstract
The invention discloses a kind of while analyzing the chromatographic detection method of 39 kinds of phenol in cigarette mainstream flue gas, include the following steps：(1) trapping of cigarette mainstream flue gas；(2) in cigarette mainstream flue gas sample phenol extraction；(3) derivatization of phenol；(4) extraction and enrichment of phenol；(5) analysis detection is carried out to phenol with gaschromatographic mass spectrometry detector；The present invention establishes ultrasonic extraction, acetylpyridine derivativeization combines micro-extraction extractive technique, the method of 39 kinds of phenol in gaschromatographic mass spectrometry while qualitative and quantitative main flume, have the characteristics that simple, quick, highly sensitive, separating capacity is strong and stability is good, can effectively improve the data accuracy of sample detection.
Description
Technical field
Cigarette master is analyzed while the present invention relates to one kind simply, quick, highly sensitive, separating capacity is strong and stability is good
The chromatographic detection method for flowing 39 kinds of phenol in flue gas, belongs to the assay method technical field of tobacco components.
Background technology
When cigarette burning is made through processing in tobacco, polyphenol substance in tobacco is low because of volatility so that seldom straight when burning and sucking
Switch through in flue gas, but enter flue gas by being thermally decomposed into phenol, therefore the aldehydes matter in cigarette smoke is mostly monohydroxy
Phenol, dihydroxy phenol and trihydroxy phenol etc..Main phenols component has 7 kinds in cigarette mainstream and flow measurement flue gas, respectively
Phenol, o- benzenediol, m- benzenediol, p- benzenediol, o-cresol, m-cresol, p-Cresol.Since most of phenol are to skin
And respiratory mucosa has strong impulse effect, and the mouthfeel of cigarette is influenced, such as cause astringent taste, pungent, pleasant impression unclean, it is special
Not being catechol (o- benzenediol) in smoke condensate has stronger auxiliary tumor promotion, and therefore, the phenols in flue gas has arranged
Enter one of main harmful components of 7 classes in flue gas, but existing document report includes only main 7 to the detection of phenols in flue gas
Kind, it can not reflect the composition and content of phenols in cigarette smoke completely, therefore, the phenol as much as possible in flue gas is qualitative simultaneously
It is particularly important with quantitative analysis.
Phenolic compound contains hydroxy functional group, and belongs to the stronger half volatile substance of polarity, therefore current liquid phase
Chromatography is to analyze the common method of phenolic compounds in cigarette smoke, but be kept completely separate m-cresol and p-Cresol and other phenol
Isomers is always the bottleneck of this method.Direct injected gas chromatography also studies have reported that, but non-derivative method sample introduction point
When analysis, due to there are highly polar group-hydroxyl, phenomena such as when analysis is also easy to produce matrix effect, and peak hangover is with interference, so as to cause
Quantitative analysis is inaccurate.In addition, the extraction efficiency that water-soluble stronger polarity phenol easily leads to method reduces.In order to overcome above-mentioned lack
It falls into, converts hydroxyl to the smaller derivatization product of polarity frequently with derivatization method and analyze.Common derivatization method
There are silanization, alkylation and acylation, most commonly seen derivatization reagent to have bis- (trimethylsilyl) trifluoroacetamides, N- first
Base-N- (trimethylsilyl) trifluoroacetamide, 2,3,4,5,6- five fluorine bromobenzyls, Alkyl chloroformates etc., but these derive examination
There are the derivatization reaction time is long, derivative products stability is poor for agent, and price is costly and some reagents are that strong dacryagogue etc. lacks
Point.
In conclusion in the determination techniques field of tobacco components, there is presently no establish it is a set of it is simple, quickly,
The analysis method of 39 kinds of phenol while qualitative and quantitative in highly sensitive and good stability cigarette mainstream flue gas.
Invention content
The technical problem to be solved by the present invention is to：Chromatography inspection that is a kind of while analyzing 39 kinds of phenol in cigarette mainstream flue gas is provided
Survey method, this method have the characteristics that simple, quick, highly sensitive, separating capacity is strong and stability is good, can effectively improve sample
The data accuracy that product examine is surveyed, with overcome the deficiencies in the prior art.
The technical scheme is that：Chromatographic detection method that is a kind of while analyzing 39 kinds of phenol in cigarette mainstream flue gas, packet
Include following steps：
(1) trapping of cigarette mainstream flue gas：Cigarette mainstream flue gas is trapped using cambridge filter；
(2) in cigarette mainstream flue gas sample phenol extraction：The inner mark solution of phenol and extraction solution are added to and are placed with sword
In the container of bridge filter disc, after ultrasonic extraction, the supernatant liquor after extraction is obtained into filtrate by filter membrane；
(3) derivatization of phenol：It takes filtrate in centrifuge tube, acetic acid aqueous solution and derivatization reagent mixing is added, slowly adds
Enter sodium bicarbonate, stands after the dissolving of vortex mixing, stood after adding solution of potassium carbonate and derivatization reagent vortex mixing；
(4) extraction and enrichment of phenol：Sodium chloride is added into the solution after derivatization, dispersion solvent is added after the dissolving that is vortexed
With extractant, vortex oscillation mixing forms fine droplet, extracts the acetylation derivative products of phenol, centrifuges, and draws in centrifuge tube
Precipitated phase and transfer them in chromatography column feed materials bottle；
(5) analysis detection：Analysis detection is carried out to the phenol in sample injection bottle with gas chromatography-mass spectrum detector.
When analyzing detection, to there is the phenol of standard items to carry out absolute quantitation, to not there is the phenol of standard items to carry out relative quantification.
Extraction solution is 1% acetic acid aqueous solution in step (2), and inner mark solution is 2- metoxyphenols-D3.
Step (3) derivedization reagent is acetic anhydride.
Dispersion solvent is acetone in step (4), and extractant is carbon tetrachloride, and wherein acetone is with carbon tetrachloride volume ratio
4:1。
Gas chromatography-mass spectrum condition is in step (5)：Gas chromatographic column is DB-1701,30m × 0.25mm i.d ×
0.25 μm of d.f, sampling volume：1 μ L, 280 DEG C of injector temperature, split sampling, split ratio 20:1, carrier gas is helium, constant current
Pattern, flow velocity 1.0mL/min, column oven are temperature programming, and 50 DEG C of holding 3min rise to 160 DEG C with 18 DEG C/min, keep
4min rises to 260 DEG C with 20 DEG C/min, keeps 5min, run 23.11min altogether；Ion source temperature is 230 DEG C, level four bars temperature
Degree is 150 DEG C, ionization energy 70eV, and transmission line temperature is 280 DEG C, solvent delay 8.3min, and scan pattern is full scan and selection
Ion scan acquires simultaneously, 45~400amu of full scan mass range.
The beneficial effects of the invention are as follows：The present invention establishes a kind of 1% acetic acid aqueous solution ultrasonic extraction-acetic anhydride derivative
Change-dispersive liquid-liquid microextraction extraction measures the side of 39 kinds of aldehydes matters in main flume with enrichment-gas chromatography-mass spectrum simultaneously
Method.Compared with the prior art, the advantages of the present invention are as follows：1) substance classes of method qualitative and quantitative are increased, it can the same time-division
Analyse 39 kinds of phenol；2) acetic anhydride derivative reagent has the reaction time short, and derivatization product is stablized, cheap and easy acquisition, toxicity
Also the advantages that smaller；3) separating capacity improves, and can efficiently separate m-cresol and p-Cresol；4) have simple, quick, highly sensitive
Degree and the good feature of stability, can effectively improve the data accuracy of sample detection.
Description of the drawings
Fig. 1 is the flow chart of the method for the present invention；
Fig. 2 is the acetylate gas chromatography-mass spectrum chromatogram of common 7 kinds of phenol standard items；
Fig. 3 is the acetylate gas chromatography-mass spectrum chromatogram of 39 kinds of phenol in cigarette mainstream flue gas.
Specific implementation mode
Below in conjunction with the accompanying drawings and invention is described further in specific embodiment：
Embodiment 1：
With reference to 1 flow chart of figure, according to present invention chromatography detection side that is a kind of while analyzing 39 kinds of phenol in cigarette mainstream flue gas
Method includes the following steps：
(1) select Cigarette by the method for GB/T 5606.1-2004,22 ± 1 DEG C of temperature, relative humidity 60% ±
48h is balanced under the conditions of 2%, is aspirated using ISO according to the method for GB/T 19609-2004 using SM450 linear type smoking machines
Pattern collects the main flume of 4 cigarette on 44mm cambridge filters, leaves and takes filter disc.
(2) cambridge filter is placed in 50mL conical flasks, the accurate Isotopic Internal Standard that 15 a concentration of 1.04mg/mL of μ L are added
With 20mL extraction solution (1% acetic acid aqueous solution) after solution (2- metoxyphenols-D3), ultrasound under room temperature after oscillation mixing 1min
30min is extracted, after vibrating mixing 1min again, takes supernatant liquor to cross 0.45 μm of water system filter membrane to be measured.
(3) it takes 1mL filtered fluids in 10mL glass centrifuge tubes, 3mL1% acetic acid aqueous solutions and 60 μ L derivatization reagents is added
(acetic anhydride) mixing afterwards is slowly added to 0.2g sodium bicarbonates, stands 2min after the dissolving of vortex mixing, add 0.1mL mass point
2min is stood after several 50% solution of potassium carbonate and 60 μ L acetic anhydride vortex mixings.
(4) it is slowly added to 0.5g sodium chloride into the solution after derivatization, dispersion solvent and extraction is added after the dissolving that is vortexed
330 μ L of solvent (dispersion solvent acetone and extractant carbon tetrachloride volume ratio 4:1), vortex oscillation mixing 2min extracts the second of phenol
Acylated derivative products (attention, which is uncapped, puts primary gas, there is a small amount of carbon dioxide gas in solution), 3500rpm centrifuge 5min, use
100 μ L micro-sampling pins draw the precipitated phase (25~28 μ L) in centrifuge tube, transfer them in 150 μ L micro-sampling bottles and use gas
Phase chromatography-mass spectroscopy detector carries out analysis detection.
(5) carried out qualitative and quantitative analysis with gas chromatography-mass spectrum detector, respectively with retention time, NIST08,
Wiley08, retention index or standard substance carry out qualitative analysis, and internal standard method carries out quantitative analysis.It quantifies with 2- metoxyphenols-
D3 is that internal standard carries out absolute quantitation and relative quantification respectively.Utilize standard curve absolute quantitation phenol, catechol, isophthalic two
Phenol, hydroquinone, ortho-methyl phenol, m-methyl phenol, p-methyl phenol；Using internal standard 2- metoxyphenol-D3 according to correction
The other 32 kinds of phenol of factor F=1 relative quantifications.
GC conditions are as follows：
Gas chromatographic column is DB-1701, i.d × 0.25 μm 30m × 0.25mm d.f, sampling volume：1 μ L, injection port temperature
280 DEG C of degree, split sampling, split ratio 20:1, carrier gas is helium, and constant current mode, flow velocity 1.0mL/min, column oven is journey
Sequence heats up, and 50 DEG C of holding 3min rise to 160 DEG C with 18 DEG C/min, keep 4min, rise to 260 DEG C with 20 DEG C/min, keep
5min runs altogether 23.11min；Ion source temperature is 230 DEG C, and level four bars temperature is 150 DEG C, ionization energy 70eV, transmission line temperature
Degree is 280 DEG C, solvent delay 8.3min.Scan pattern is that full scan acquires simultaneously with selection ion scan, full scan quality model
Enclose 45-400amu；The retention time of 39 kinds of phenol and index, it is quantitative with qualitative ion, qualitative fashion, split time, residence time,
Sample method repeatability and acetylation derivative products stability are as shown in table 1 below：
The mass spectrum and stability analysis result of 39 kinds of phenol and Isotopic Internal Standard in 1 main flume of table
The mother liquor that respective concentration is prepared with 1% acetic acid aqueous solution, mother liquor is mixed and is diluted to 5 with 1% acetic acid aqueous solution
The mixed sample of a concentration gradient takes a certain amount of mixed sample and 15 μ L Isotopic Internal Standards (2- metoxyphenols-D3), uses
1% acetic acid aqueous solution is diluted to 4mL, is performed the derivatization and chromatography (standard specimen and sample according to the condition of (3), (4) and (5)
Chromatogram is as shown in Fig. 2 and 3), using the ratio of target compound peak area and internal standard compound peak area as ordinate (y), target chemical combination
The ratio of the amount of object and interior scalar (15.6 μ g) is that abscissa (x) carries out regression analysis, obtains regression equation and related coefficient, will
The standard solution of minimum concentration is according to the minimum detection limit (LOD) that signal-to-noise ratio is 3 (S/N=3) computational methods, to the Kentucky 3R4F
It is extracted after adding the standard solution of two concentration gradients in the main flume cambridge filter of standard sample, derivatization and chromatography point
Analysis, calculates its rate of recovery.The rate of recovery is that the phenols content of sample after adding subtracts content divided by the addition of blank sample phenols
Phenols content, addition concentration are about that 1/2 and 1 times of content in blank sample is added to row respectively, and the precision of method is will
Low concentration is added with high concentration and is repeated 5 times interior on the same day, calculates the relative standard deviation of its measurement result.As a result such as table 2 and 3
It is shown.Method is that interior be repeated 5 times analyzes detection on the same day to the repeatability of other aldehydes matters in sample, calculates its relative standard
Deviation；Peak area variation of the acetylation phenol derivative products stability test under 4 DEG C of preservation conditions after 1d, 3d, 5d and 7d, calculates
Corresponding relative standard deviation.Method is shown in the repeatability of other aldehydes matters in sample with acetylation phenol derivative products stability
Table 1.
The range of linearity of 2 common 7 kinds of phenol standard specimens of table, standard curve, related coefficient are limited with detection
The TIANZHU XINGNAO Capsul and precision of 3 common 7 kinds of phenol standard specimens of table
The result shows that：The method of the present invention linearly dependent coefficient is both greater than 0.9990, shows the linear preferable of method.Method
Concentration Testing limits and cigarette detection limits respectively between 0.053~0.087ng/mL and 1.06~1.74ng/, and the rate of recovery of phenol exists
Between 95.2%~102.0%, the rate of recovery is good, and precision range meets stringent quantitative want between 1.1%~4.8%
It asks.Method in sample other aldehydes matters repeatability with acetylation phenol derivative products stability be both less than 6.99% with
2.89%, only scopoletin repeatability and stability is slightly worse, and respectively 10.5% and 3.78%.
Embodiment 2：
For the phenol content composition between more different tar content cigarette, take the method for embodiment 1 to low tar
(3mg), middle tar (11mg) are analyzed with the phenol in the main flume of high tar (15mg) cigarette, measurement result such as the following table 4
It is shown：From testing result it is found that phenol composition differs greatly in the cigarette mainstream flue gas of different tar contents, tar content is higher,
Phenol content is higher.7 kinds of common phenol in the cigarette mainstream flue gas of same tar content is (phenol, o- benzenediol, m- benzenediol, p-
Benzenediol, o-cresol, m-cresol, p-Cresol) content occupy 60% or so, show 7 kinds of common phenol wherein occupancy volume compared with
Height preferably explains the above-mentioned 7 kinds of substances of Main Analysis in conventional detection.Phenol is divided into mono-hydroxy phenol, dihydric phenol, trihydroxy
Phenol, wherein dihydric phenol account for 85~87% or so, and mono-hydroxy phenol accounts for 12~13%, and trihydroxy phenol accounts for 1~2%, shows tobacco leaf master
Flow in flue gas is mainly dihydric phenol.Since dihydric phenol has higher toxicity, need to pay close attention to its content composition.
The composition of phenol in the main flume of the different tar content cigarette of table 4
aPhenol separation not yet in effect, and quota ion is also identical, it is final result to calculate its total amount
The result shows that：Detection method using the present invention can fast and accurately obtain in cigarette mainstream flue gas 39 kinds of phenol
Composition.
The above content is a further detailed description of the present invention in conjunction with specific preferred embodiments, and it cannot be said that
The specific implementation of the present invention is confined to these explanations.For those of ordinary skill in the art to which the present invention belongs, exist
Under the premise of not departing from present inventive concept, a number of simple deductions or replacements can also be made, all shall be regarded as belonging to the present invention's
Protection domain.
Claims (6)
1. chromatographic detection method that is a kind of while analyzing 39 kinds of phenol in cigarette mainstream flue gas, it is characterised in that：Include the following steps：
(1) trapping of cigarette mainstream flue gas：Cigarette mainstream flue gas is trapped using cambridge filter；
(2) in cigarette mainstream flue gas sample phenol extraction：The inner mark solution of phenol and extraction solution are added to and are placed with Cambridge filter
In the container of piece, after ultrasonic extraction, the supernatant liquor after extraction is obtained into filtrate by filter membrane；
(3) derivatization of phenol：It takes filtrate in centrifuge tube, acetic acid aqueous solution and derivatization reagent mixing is added, is slowly added to carbon
Sour hydrogen sodium stands after the dissolving of vortex mixing, is stood after adding solution of potassium carbonate and derivatization reagent vortex mixing；
(4) extraction and enrichment of phenol：Sodium chloride is added into the solution after derivatization, dispersion solvent and extraction is added after the dissolving that is vortexed
It takes solvent, vortex oscillation mixing to form fine droplet, extract the acetylation derivative products of phenol, centrifuges, it is heavy in centrifuge tube to draw
It forms sediment mutually and transfers them in chromatography column feed materials bottle；
(5) analysis detection：Analysis detection is carried out to the phenol in sample injection bottle with gas chromatography-mass spectrum detector.
2. chromatographic detection method that is according to claim 1 while analyzing 39 kinds of phenol in cigarette mainstream flue gas, feature exist
In：When analyzing detection, to there is the phenol of standard items to carry out absolute quantitation, to not there is the phenol of standard items to carry out relative quantification.
3. chromatographic detection method that is according to claim 1 while analyzing 39 kinds of phenol in cigarette mainstream flue gas, feature exist
In：Extraction solution is 1% acetic acid aqueous solution in step (2), and inner mark solution is 2- metoxyphenols-D3.
4. chromatographic detection method that is according to claim 1 while analyzing 39 kinds of phenol in cigarette mainstream flue gas, feature exist
In：Step (3) derivedization reagent is acetic anhydride.
5. chromatographic detection method that is according to claim 1 while analyzing 39 kinds of phenol in cigarette mainstream flue gas, feature exist
In：Dispersion solvent is acetone in step (4), and extractant is carbon tetrachloride, and wherein acetone and carbon tetrachloride volume ratio are 4:1.
6. chromatographic detection method that is according to claim 1 while analyzing 39 kinds of phenol in cigarette mainstream flue gas, feature exist
In：Gas chromatography-mass spectrum condition is in step (5)：Gas chromatographic column is DB-1701, the μ of 30m × 0.25mm i.d × 0.25
Md.f, sampling volume：1 μ L, 280 DEG C of injector temperature, split sampling, split ratio 20:1, carrier gas is helium, constant current mode,
Flow velocity is 1.0mL/min, and column oven is temperature programming, and 50 DEG C of holding 3min rise to 160 DEG C with 18 DEG C/min, keep 4min, with
20 DEG C/min rises to 260 DEG C, keeps 5min, runs 23.11min altogether；Ion source temperature is 230 DEG C, and level four bars temperature is 150
DEG C, ionization energy 70eV, transmission line temperature is 280 DEG C, solvent delay 8.3min, and scan pattern is full scan and selection ion scan
It acquires simultaneously, 45~400amu of full scan mass range.
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| CN111208263A (en) * | 2020-01-16 | 2020-05-29 | 贵州省烟草科学研究院 | Method for evaluating ecotoxicity of organic additive in full-biodegradable mulching film by applying seeds |
| CN111257489A (en) * | 2020-01-21 | 2020-06-09 | 浙江工业大学 | Method for analyzing volatile phenolic compounds in water based on ultrasonic-assisted in-situ bubbling and simultaneous derivatization-dispersion liquid-liquid microextraction |
| CN113310866A (en) * | 2021-05-14 | 2021-08-27 | 河北中烟工业有限责任公司 | Method for measuring retention rate of cigarette filter stick on hydroxypyridine |
| CN114034787A (en) * | 2021-10-29 | 2022-02-11 | 中国烟草总公司郑州烟草研究院 | Method for determining sensory related amide compounds in cigarette mainstream smoke |
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| CN109557215A (en) * | 2019-01-16 | 2019-04-02 | 黑龙江八农垦大学 | The method that PDMS micro-pipe extracts phenolic substances in root exudates after derivative |
| CN110907235A (en) * | 2019-10-21 | 2020-03-24 | 河南中烟工业有限责任公司 | Method for collecting and detecting phenol flavor components in cigarette mainstream smoke |
| CN111208263A (en) * | 2020-01-16 | 2020-05-29 | 贵州省烟草科学研究院 | Method for evaluating ecotoxicity of organic additive in full-biodegradable mulching film by applying seeds |
| CN111257489A (en) * | 2020-01-21 | 2020-06-09 | 浙江工业大学 | Method for analyzing volatile phenolic compounds in water based on ultrasonic-assisted in-situ bubbling and simultaneous derivatization-dispersion liquid-liquid microextraction |
| CN113310866A (en) * | 2021-05-14 | 2021-08-27 | 河北中烟工业有限责任公司 | Method for measuring retention rate of cigarette filter stick on hydroxypyridine |
| CN115728398A (en) * | 2021-08-26 | 2023-03-03 | 贵州中烟工业有限责任公司 | Method for measuring nicotine and volatile phenol in smoke intercepted by cigarette filter |
| CN114034787A (en) * | 2021-10-29 | 2022-02-11 | 中国烟草总公司郑州烟草研究院 | Method for determining sensory related amide compounds in cigarette mainstream smoke |
| CN114034787B (en) * | 2021-10-29 | 2024-05-03 | 中国烟草总公司郑州烟草研究院 | Method for measuring sensory related amide compounds in main stream smoke of cigarettes |
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