CN104931633B - The measuring method of a kind of tobacco Dry distillated flavor chemical composition - Google Patents
The measuring method of a kind of tobacco Dry distillated flavor chemical composition Download PDFInfo
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- CN104931633B CN104931633B CN201510306157.1A CN201510306157A CN104931633B CN 104931633 B CN104931633 B CN 104931633B CN 201510306157 A CN201510306157 A CN 201510306157A CN 104931633 B CN104931633 B CN 104931633B
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Abstract
The present invention discloses the measuring method of a kind of tobacco Dry distillated flavor chemical composition, comprises the steps: that (1) take ethanol as solvent, prepares menthol standardized solution and propyl benzoate standardized solution respectively; (2) tobacco Dry distillated flavor is mixed with menthol standardized solution and propyl benzoate standardized solution, obtain testing sample solution; (3) testing sample solution is carried out gas chromatography combined with mass spectrometry analysis, obtain the chemical constituents determination result of tobacco Dry distillated flavor. The measuring method of a kind of tobacco Dry distillated flavor chemical composition of the present invention, it is possible to simply, measure the chemical composition of tobacco Dry distillated flavor quickly and accurately, and then instruct process modification prepared by tobacco Dry distillated flavor.
Description
Technical field
The present invention relates to tobacco analysis field, it is specifically related to the measuring method of a kind of tobacco Dry distillated flavor chemical composition.
Background technology
In tobacco, the flavour content added in tobacco product is considerable, except cigarette only has the spices of trace mostly, the flavour content of other several tobacco products is all higher, and the spices addition in the cigarette that wherein struggles against, cigar, hand scroll cigarette, chewing tobacco, snuff and shredded tobacco for water pipes is usually all higher than cigarette. In these products, spices plays a part decisive for the taste of whole product.
A kind of novel fragrance that Dry distillated flavor is the shortcoming for tradition fume smoking method acquisition spices and develops, the be harmful wood cigarette pollution to food and environment and the infringement to HUMAN HEALTH that tradition fume smoking method obtains the main drawback of spices, particularly some strong carcinogens, such as 3,4-benzopyrene etc.
Not containing 3, the Dry distillated flavor of 4-benzopyrene is that people dream of, it is easy to use, a small amount of interpolation can obtain smoking color fragrance more better than traditional method, the more important thing is pollution-free, safety and sanitation, modern free-radical theory shows, the spices adopting method for destructive distillation to obtain also has nourishing function, possesses the advantage advocated energetically and promote the use of.
So-called destructive distillation refers to a kind of chemical engineering unit operation of " isolated air heating ", the outstanding advantage of method for destructive distillation is real " isolated air ", destructive distillation process does not generate objectionable impurities, and convenient operation and control, product yield height, quality are good, this technology just marches to cigarette industry at present, for the preparation of pipe tobacco Dry distillated flavor.
For traditional cigarette, because it burns under about 800 DEG C of conditions, creating a large amount of tar and multiple aroma component, the health of smoker is harmful by the part composition produced that simultaneously burns. Therefore, exploitation can discharge the similar tobacco material normally burning and sucking cigarette smoke by retorting technique at a lower temperature, and the development for cigarette has important practical significance.
Tobacco Dry distillated flavor, as a kind of novel tobacco spices, not yet has report at tobacco industry at present. How its chemical composition to be carried out qualitative and quantitative analysis accurately, carry out the analysis appraisal to pipe tobacco Dry distillated flavor, have very important significance for promoting the preparation technology of Dry distillated flavor and quality stability and follow-up perfumed applications, produce huge pushing effect by the analysis appraisal of new cigarette spices simultaneously.
Owing in tobacco Dry distillated flavor, nicotine content is very high, and other chemical composition contents are very low, adopt single interior mark to carry out quantitative assay error bigger. Therefore in order to ensure the accuracy of quantitative assay, it is necessary to adopt two interior calibration method to carry out assay.
In order to realize the analysis to tobacco Dry distillated flavor chemical composition, except selecting suitable internal standard substance, in addition it is also necessary to various analysis testing conditions is optimized, to obtain best analysis detected result.
Summary of the invention
The present invention provides the measuring method of a kind of tobacco Dry distillated flavor chemical composition, it is possible to simply, measures the chemical composition of tobacco Dry distillated flavor quickly and accurately, and then instructs process modification prepared by tobacco Dry distillated flavor.
A measuring method for tobacco Dry distillated flavor chemical composition, comprises the steps:
(1) take ethanol as solvent, prepare menthol standardized solution and propyl benzoate standardized solution respectively;
(2) tobacco Dry distillated flavor is mixed with menthol standardized solution and propyl benzoate standardized solution, obtain testing sample solution;
(3) testing sample solution is carried out gas chromatography combined with mass spectrometry analysis, obtain the chemical constituents determination result of tobacco Dry distillated flavor.
Tobacco Dry distillated flavor is carried out composition detection by the present invention, the preparation technology of tobacco Dry distillated flavor to be improved, the preparation method of described tobacco Dry distillated flavor comprises the following steps:
(1) tobacco being carried out destructive distillation, the temperature of destructive distillation is 400��800 DEG C;
(2) utilize propylene glycol to be absorbed by destructive distillation product, and absorbing liquid is carried out condensation, obtain described tobacco Dry distillated flavor.
Preferably, the time of destructive distillation is 2��5h. After being heated to predetermined cracking temperature, constant temperature 2��5 hours, constant temperature time is the destructive distillation time, in the process, utilizes solvent to be absorbed by the product of destructive distillation.
In the preparation process of tobacco Dry distillated flavor, relatively crucial technique is the temperature of control destructive distillation, the time of destructive distillation, the solvent of Selective absorber split product, the temperature etc. of condensation, paper examines of the present invention under different pyrolysis temperature, the difference of the chemical composition of the tobacco Dry distillated flavor of acquisition.
If analyze the difference evaluating chemical composition under different pyrolysis temperature with area normalization method, the chemical composition of tobacco Dry distillated flavor is under different pyrolysis temperature, regularity is not very obvious, it is difficult to judge the impact of pyrolysis temperature for Dry distillated flavor chemical composition, in order to better evaluate pyrolysis temperature to the impact of chemical composition, introduce two interior mark and analyze.
Chromatogram internal standard substance should be close with the relative molecular mass of tested component, boiling point and retention time, and structure is similar, can with tested Component seperation, the present invention selects menthol and propyl benzoate to do interior mark, and chemical composition and internal standard substance in tobacco Dry distillated flavor can achieve good separation on color atlas.
Owing to propyl benzoate goes out peak position and intensity and nicotine relatively, it is possible to be used for calculating the content of nicotine, and menthol is used for calculating the content of other trace ingredientss in tobacco Dry distillated flavor.
Tobacco Dry distillated flavor chemical composition under adopting method provided by the invention to measure differing temps, the result obtained shows, the Dry distillated flavor that retorting technique is prepared under cryogenic can reach the effect of traditional cigarette.
The concentration of the standardized solution of internal standard substance needs to be optimized, to guarantee that the add-on of internal standard substance can either present the peak value of proper strength in chromatogram, good being separated can be realized on color atlas again with tobacco Dry distillated flavor chemical composition, preferably, the concentration of described menthol standardized solution is 1000ppm, and the concentration of described propyl benzoate standardized solution is 2000ppm.
In order to present good separation on color atlas, and there is the peak value of suitable intensity, it may be preferred that the volume ratio of described tobacco Dry distillated flavor, menthol standardized solution, propyl benzoate standardized solution is 2��4:1:7. Further preferably, the volume ratio of described tobacco Dry distillated flavor, menthol standardized solution, propyl benzoate standardized solution is 3:1:7. The cumulative volume of testing sample solution is 500 �� L.
As preferably, when carrying out gas chromatography combined with mass spectrometry analysis, gas-chromatography temperature programming process is as follows:
Initial column oven temperature is 40 �� 5 DEG C;
Then it is warming up to 160 �� 10 DEG C with the speed of 2 �� 1 DEG C/min;
Finally it is warming up to 260 �� 10 DEG C with the speed of 3 �� 1 DEG C/min, constant temperature 8��12min at this temperature (namely 260 �� 10 DEG C).
Gas-chromatography temperature programming process has material impact for the detected result of the tobacco Dry distillated flavor composition obtained, the temperature of chromatographic column, according to the change of program of setting, makes low boiling component and high boiling component that suitable reservation, chromatographic peak can both be had in the chromatography column to be evenly distributed and peak shape symmetry.
When carrying out gas chromatography combined with mass spectrometry analysis, mass spectrum is as follows:
Ion source: electron bombardment formula ion source; Ionization energy: 70eV; Ion trap temperature: 200 �� 10 DEG C; Manifold temperature: 50 �� 5 DEG C; Transmission line temperature: 230 �� 10 DEG C.
The present invention compared with prior art, has the following advantages:
(1) the present invention is simple, it is possible to realize accurately quantitative while extremely high in tobacco Dry distillated flavor and pole low levels chemical composition.
(2) in the present invention, tobacco Dry distillated flavor sample directly adds internal standard substance sample detection, and measuring method is simple and efficient, and can eliminate due to sample size, instrument instability etc. the interference that causes of the systematic error brought, measurement result is accurately and reliably.
(3) utilize two marker method that the chemical composition of tobacco Dry distillated flavor is carried out semi-quantitative analysis, it is possible to the difference of Dry distillated flavor chemical composition under remarkable differentiation differing temps, and then instruct the preparation technology of tobacco Dry distillated flavor better.
Accompanying drawing explanation
Fig. 1 is the total ion current figure under different pyrolysis temperature;
Fig. 2 inserts target total ion current figure in menthol and propyl benzoate under 400 DEG C of pyrolysis temperatures;
Fig. 3 is the different classes of compound number under different pyrolysis temperature;
Fig. 4 is the percentage composition of the different classes of compound under different pyrolysis temperature;
Fig. 5 is the chemical composition absolute content under different pyrolysis temperature;
Fig. 6 is the nicotine absolute content under different pyrolysis temperature.
Embodiment
Embodiment 1
Take 4g pipe tobacco and put into tube furnace, it is heated to 400 DEG C, and constant temperature 2.5h, flue gas utilization nitrogen destructive distillation produced brings the absorption bottle being placed in cold-trap into, 25mL propylene glycol is housed in absorption bottle in advance, and condenser temperature is-15 DEG C, washes out the smoke condensate in pipeline with 40mL propylene glycol, absorbing liquid in absorption bottle is merged with the smoke condensate washed out in pipeline, obtains tobacco Dry distillated flavor.
Embodiment 2
Take 4g pipe tobacco and put into tube furnace, it is heated to 500 DEG C, and constant temperature 2.5h, flue gas utilization nitrogen destructive distillation produced brings the absorption bottle being placed in cold-trap into, 25mL propylene glycol is housed in absorption bottle in advance, and condenser temperature is-15 DEG C, washes out the smoke condensate in pipeline with 40mL propylene glycol, absorbing liquid in absorption bottle is merged with the smoke condensate washed out in pipeline, obtains tobacco Dry distillated flavor.
Embodiment 3
Take 4g pipe tobacco and put into tube furnace, it is heated to 600 DEG C, and constant temperature 2.5h, flue gas utilization nitrogen destructive distillation produced brings the absorption bottle being placed in cold-trap into, 25mL propylene glycol is housed in absorption bottle in advance, and condenser temperature is-15 DEG C, washes out the smoke condensate in pipeline with 40mL propylene glycol, absorbing liquid in absorption bottle is merged with the smoke condensate washed out in pipeline, obtains tobacco Dry distillated flavor.
Embodiment 4
Take 4g pipe tobacco and put into tube furnace, it is heated to 800 DEG C, and constant temperature 2.5h, flue gas utilization nitrogen destructive distillation produced brings the absorption bottle being placed in cold-trap into, 25mL propylene glycol is housed in absorption bottle in advance, and condenser temperature is-15 DEG C, washes out the smoke condensate in pipeline with 40mL propylene glycol, absorbing liquid in absorption bottle is merged with the smoke condensate washed out in pipeline, obtains tobacco Dry distillated flavor.
The preparation of inner mark solution:
Adopt AE163 electronic balance (sense amount: 0.0001g, Mettler company of Switzerland) accurately take 0.050g (being accurate to 0.1mg) (-)-Menthol standard specimen (menthol standard specimen, Fluka company), it is placed in 50mL volumetric flask, with ethanol (chromatographically pure, MERCK Merck company) dissolve and determine to hold, it is mixed with the menthol standardized solution that concentration is 1000ppm.
Adopt AE163 electronic balance accurately take 0.100g (being accurate to 0.1mg) propyl benzoate standard specimen (purity > 99.0%, ladder is uncommon likes chemical conversion industrial development company limited), it is placed in 50mL volumetric flask, hold with dissolve with ethanol is also fixed, it is mixed with the propyl benzoate standardized solution that concentration is 2000ppm.
Embodiment 5
Pipette the tobacco Dry distillated flavor supernatant liquor of 150 �� L embodiments 1,50 �� L menthol standardized solution and 350 �� L propyl benzoate standardized solution (cumulative volume is 500 �� L) respectively, mixed even, it is testing sample solution.
Chromatographic condition is as follows:
Capillary chromatographic column DB-624, specification: 60mx320 ��m x1.8 ��m; Injector temperature: 270 DEG C; Sample size: 1 �� L, split stream sampling (splitting ratio: 10:1); Carrier gas: helium (purity >=99.999%), constant current mode, flow velocity: 1.0mL/min; Heating schedule: initial temperature 40 DEG C, keeps 0min, with the speed to 160 DEG C of 2 DEG C/min, keeps 0min, then the speed to 260 DEG C with 3 DEG C/min, keeps 10min.
Mass Spectrometry Conditions is as follows:
Ionization mode: electron bombardment ionization source (EI source); Ionization energy: 70eV; Transmission line temperature: 230 DEG C; Ion source temperature: 200 DEG C; Solvent delay: 3.5min; Sweep limit 50��450amu; Mensuration mode: full scan.
The testing sample solution prepared is introduced gas chromatograph-mass spectrometer (U.S.'s Agilent7890A-5975C type), the principle being greater than 80% with matching degree by standard spectrum library searching carries out qualitative, by qualitative go out compound carry out semi-quantitative analysis with marker method, the default response factor is 1, by qualitative go out compound and the peak area ratio of interior mark compound calculate the content of each chemical composition in testing sample solution.
Concrete calculation formula is as follows:
In tobacco Dry distillated flavor, the mass concentration of target component is: X1=f �� A1 �� I/A2
Relative correction factor: f=�� �� d2/d1
In formula: X1 is the mass concentration of target component in tobacco Dry distillated flavor, ppm;
F is relative correction factor;
�� is response factor, is defaulted as 1;
A1 is the peak area (or peak height) of target compound in testing sample solution;
A2 is the peak area (or peak height) of internal standard substance in testing sample solution;
D1 is the add-on of target compound in testing sample solution;
D2 is the add-on of internal standard substance in testing sample solution;
I is the mass concentration of the internal standard substance added, ppm.
The total ion current figure that the present embodiment obtains is as shown in Figure 2, the chemical composition can found out in menthol and propyl benzoate and tobacco Dry distillated flavor achieves good separation, owing to propyl benzoate goes out peak position and intensity and nicotine relatively, therefore the content of nicotine it is used for calculating, and menthol is used for calculating the content of other trace ingredientss of Dry distillated flavor, the chemical composition of the tobacco Dry distillated flavor that the present embodiment obtains is as listed in table 1.
Table 1
Embodiment 6��8
Adopting method as described in Example 5, tobacco Dry distillated flavor embodiment 2��4 prepared respectively carries out chemical composition detection.
The total ion current figure of the tobacco Dry distillated flavor of embodiment 5��8 as shown in Figure 1, by the chemical composition appearance time in the tobacco Dry distillated flavor under the differing temps that can visually see in figure and peak area all relatively. Undertaken qualitative by standard spectrum library searching, altogether qualitative go out 50 kinds of chemical compositions, mainly comprise the compound of alcohol class, arene, phenols, aldoketones, acid class, carbohydrate, heterocyclic, the big classification of ester class eight.
The chemical composition of the tobacco Dry distillated flavor that embodiment 6, embodiment 7, embodiment 8 obtain is respectively as listed by table 2, table 3, table 4.
Table 2
Table 3
Table 4
By Fig. 3 and Fig. 4 it may be seen that chemical composition under different pyrolysis temperature be number or percentage composition all comparing class seemingly, based on heterocyclic compound, this compounds accounts for about the 80% of total amount, secondly mainly phenols and group compounds of aldehydes and ketones. Wherein heterocyclic compound is again based on nicotine content, has accounted for more than the 80% of heterocycle total amount.
At each retention time place in Fig. 5, under being followed successively by 400 DEG C, 500 DEG C, 600 DEG C, 800 DEG C pyrolysis temperatures from left to right, the content of each chemical composition in the tobacco Dry distillated flavor obtained, as seen from Figure 5 along with temperature rise each chemical composition content roughly on a declining curve, the particularly main flavor such as heterocyclic and aldoketones material in Dry distillated flavor, such as pyridine, 3-methyl pyrrole, 3,5-lutidine, 3-methyl-2-cyclopentenes-1-ketone, 2-hydroxy-3-methyl-2-cyclopentenes-1-ketone, 2,3-bis-hydrogen-3,5-dihydroxyl-6-methyl-4H-pyrans-4-ketone etc. In tobacco Dry distillated flavor, the objectionable constituent such as arene do not occur under 400 DEG C, 500 DEG C conditions, are improve the main flavor substances content such as heterocyclic and aldoketones, enrich flavour ingredient kind, and reduce Harmful ingredient content, and 400 DEG C is the best pyrolysis temperature.
The nicotine composition occupied an leading position in tobacco Dry distillated flavor as seen from Figure 6, its content is also along with the regular decline that rises of pyrolysis temperature.
Adopt method provided by the invention that tobacco Dry distillated flavor is carried out chemical constituents determination, it is possible to obviously to find out that temperature is on the impact of Dry distillated flavor chemical composition, for selecting suitable pyrolysis temperature to provide good foundation. Simultaneously, two interior demarcation amount result shows, no matter the Dry distillated flavor that retorting technique is prepared at cold condition is that chemically composition kind or content can reach even beyond tradition cigarette effect, provides good theory support for retorting technique is applied to novel tobacco goods further.
Claims (2)
1. the measuring method of a tobacco Dry distillated flavor chemical composition, it is characterised in that, comprise the steps:
(1) take ethanol as solvent, prepare menthol standardized solution and propyl benzoate standardized solution respectively;
The concentration of described menthol standardized solution is 1000ppm, and the concentration of described propyl benzoate standardized solution is 2000ppm;
(2) tobacco Dry distillated flavor is mixed with menthol standardized solution and propyl benzoate standardized solution, obtain testing sample solution;
The preparation method of described tobacco Dry distillated flavor comprises the following steps:
(1) tobacco being carried out destructive distillation, the temperature of destructive distillation is 400��800 DEG C, and the time of destructive distillation is 2��5h;
(2) utilize propylene glycol to be absorbed by destructive distillation product, and absorbing liquid is carried out condensation, obtain described tobacco Dry distillated flavor;
The volume ratio of described tobacco Dry distillated flavor, menthol standardized solution, propyl benzoate standardized solution is 2��4:1:7;
(3) testing sample solution is carried out gas chromatography combined with mass spectrometry analysis, obtain the chemical constituents determination result of tobacco Dry distillated flavor;
When carrying out gas chromatography combined with mass spectrometry analysis, gas-chromatography temperature programming process is as follows:
Initial column oven temperature is 40 �� 5 DEG C;
Then it is warming up to 160 �� 10 DEG C with the speed of 2 �� 1 DEG C/min;
Finally it is warming up to 260 �� 10 DEG C with the speed of 3 �� 1 DEG C/min, constant temperature 8��12min at such a temperature;
Mass spectrum is as follows:
Ion source: electron bombardment formula ion source; Ionization energy: 70eV; Ion trap temperature: 200 �� 10 DEG C; Manifold temperature: 50 �� 5 DEG C; Transmission line temperature: 230 �� 10 DEG C.
2. the measuring method of tobacco Dry distillated flavor chemical composition as claimed in claim 1, it is characterised in that, the cumulative volume of testing sample solution is 500 �� L.
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| CN114200032B (en) * | 2020-09-18 | 2024-02-23 | 湖南中烟工业有限责任公司 | Method for detecting nicotine form in tobacco material and method for judging type of acid added in tobacco material |
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| CN101816790A (en) * | 2010-05-06 | 2010-09-01 | 桂林莱茵生物科技股份有限公司 | Spray for treating radioactive xerostomia and preparation method thereof |
| CN103472149A (en) * | 2013-09-12 | 2013-12-25 | 上海烟草集团有限责任公司 | Method for analyzing influence of mentholated cigarette processing process on production environment |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101816790A (en) * | 2010-05-06 | 2010-09-01 | 桂林莱茵生物科技股份有限公司 | Spray for treating radioactive xerostomia and preparation method thereof |
| CN103472149A (en) * | 2013-09-12 | 2013-12-25 | 上海烟草集团有限责任公司 | Method for analyzing influence of mentholated cigarette processing process on production environment |
Non-Patent Citations (4)
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| Application of headspace solid phase microextraction to qualitative and quantitative analysis of tobacco additives in cigarettes;Careen Merckel et al;《Journal of Chromatography A》;20060331;第1116卷;10-19 * |
| Characterization of rum using solid-phase microextraction with gas chromatography-mass spectrometry;Jorge A.Pino;《Food Chemistry》;20071231;第104卷;421-428 * |
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| 卷烟及烟气中薄荷醇含量的测定;宫梅等;《烟草科技/烟草检验》;20021231(第7期);29-31 * |
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