CN101762656A - Chromatography method for detecting tobacco flavors - Google Patents
Chromatography method for detecting tobacco flavors Download PDFInfo
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Abstract
The invention provides a chromatography method for detecting tobacco flavors, which comprises the steps: a, pre-treating; b, analyzing the organic phase after pretreating by GC-MS and GC-FID, using polar columns, and carrying out three-stage temperature rise that the initial furnace temperature is 30 DEG C to 60 DEG C and maintains 3 to 8 minutes, rises to 80 DEG C to 150 DEG C at a speed of 2 DEG C/min to 5 DEG C/min, and then rises to 180 DEG C to 250 DEG C at a speed of 3 DEG C/min to 8 DEG C/min, and rises to 200 DEG C to 300 DEG C at a speed of 5 DEG C/min to 15 DEG C/min again for 20 to 40 minutes; and c, adopting split/splitless injection, carrying out the splitless injection initially for 0.5 to 2 minutes, and then starting the split injection, with the split ratio of 40:1 to 60:1. The invention uses the polar columns to separate the tobacco flavors, and has good selectivity of fragrant substance, easy separation of similar components and sensitive detection, thereby effectively monitoring the quality of the flavors.
Description
Technical field
The present invention relates to the detection technique of flavouring essence for tobacco, be specifically related to a kind of red, orange, green, blue, yellow (ROGBY) of tobacco aromatics using.
Background technology
The flavouring essence for tobacco major part is liquid, and bag peak information is obvious, the mass content of propylene glycol, glycerine and carbohydrate≤1%, and other fragrance matter peak quantity of information is bigger, and most critical is the evaluation of aroma quality in the detection of the various indexs of tobacco aromatics using.If the evaluation of aroma quality is by people's subjective appreciation, and then to have the diversity ratio that subjectivity exists uncertain factor that the result is existed bigger owing to people's sensory evaluation.
Adopt efficient sensitive modern analysis isolation technics such as mass spectrum, chromatogram, make people can separate complicated potpourri, and obtain the bulk information of relevant component organic chemistry configuration aspects, therefore, generally use GC-MS (gas chromatography-mass spectrography), GC-FID (gas chromatography-flame ionization ditector) that flavouring essence for tobacco is detected in the tobacco business.When sample entered GC and separates, because most of component all belongs to volatilization or half volatile material in the flavouring essence for tobacco, and the peak sequence of non-polar column was just to go out the peak according to the boiling point that goes out the peak material, so capillary column is generally selected non-polar column for use.Therefore but lower boiling aroma constituent content is more in the flavouring essence for tobacco, goes out the peak and may have overlappingly, and sometimes the separating effect of non-polar column is relatively poor.
Summary of the invention
The problem that the present invention solves is to provide a kind of chromatogram check and analysis method of flavouring essence for tobacco, uses polar column that flavouring essence for tobacco is separated, and is good to the polar material selectivity in the flavouring essence for tobacco, and similar component is easy to separate.
In order to solve the problems of the technologies described above, technical scheme of the present invention is:
A kind of chromatography method for detecting tobacco flavors may further comprise the steps:
A, tobacco aromatics using to be measured is carried out pre-treatment;
B, the liquid that contains fragrance matter that obtains after the pre-treatment is analyzed with GC-MS, GC-FID, GC uses polar column, heating schedule is three rank heating schedules, furnace temperature is initially 30 ℃～60 ℃, keep 3min～8min, heat up with the heating rate of 2 ℃/min～5 ℃/min, the heating rate that is raised to after 80 ℃～150 ℃ with 3 ℃/min～8 ℃/min is warming up to 180 ℃～250 ℃, heating rate with 5 ℃/min～15 ℃/min is warming up to 200 ℃～300 ℃ again, keeps 20min～40min;
C, employing are shunted/are regardless of and flow to sample loading mode, and the sample introduction starting stage is split sampling not, begin shunting after sample introduction 0.5min～2min, and split ratio is 40: 1～60: 1.
As preferably, three rank heating schedules among the described step b are that furnace temperature is initially 40 ℃, keep 5min, heating rate with 3 ℃/min heats up, be raised to that the heating rate with 5 ℃/min is warming up to 200 ℃ after 100 ℃, the heating rate with 8 ℃/min is warming up to 245 ℃ again, keeps 30min.
As preferably, the input mode of the shunting among the described step c/do not shunt is that sample introduction begins not shunt to sample introduction 1min, begins shunting after the sample introduction 1min.
As preferably, the split ratio that begins to shunt after the described sample introduction 1min is 50: 1.
As preferably, described polar column is the FFAP polar column.
As preferably, the model of described FFAP polar column is 60m * 0.25 μ m * 0.25mm.
As preferably, the temperature of the injection port of GC is 200 ℃～300 ℃ among the described step b.
As preferably, the detected temperatures of FID is 200 ℃～300 ℃ among the described step b.
As preferably, the operating conditions of MS is among the described step b: the MS interface temperature is 200 ℃～300 ℃; EI ion gun, electron energy 60eV～80eV, ion source temperature are 200 ℃～300 ℃; Sweep limit 30u～500u.
The fragrance matter component of flavouring essence for tobacco is a polar material, and the fragrance matter component is more, the chromatographic peak quantity of information is bigger, characteristics at tobacco flavor components, the present invention uses polar column that flavouring essence for tobacco is separated, and is good to the fragrance matter selectivity in the flavouring essence for tobacco, and similar component is easy to separate, detect sensitive, thereby quality situation that can effective monitoring essence.
Description of drawings
Fig. 1 is the GC-MS figure of flavouring essence for tobacco under the operating conditions of embodiment 1;
Fig. 2 is the GC-FID figure of flavouring essence for tobacco under the operating conditions of embodiment 2;
Fig. 3 is the GC-FID figure of flavouring essence for tobacco under the operating conditions of embodiment 3;
Fig. 4 is the GC-FID figure of flavouring essence for tobacco under the operating conditions of Comparative Examples 1;
Fig. 5 is the GC-FID figure of flavouring essence for tobacco under the operating conditions of Comparative Examples 2.
Embodiment
In order further to understand the present invention, below in conjunction with embodiment the preferred embodiment of the invention is described, but should be appreciated that these describe just to further specifying the features and advantages of the present invention, rather than to the restriction of claim of the present invention.
Chromatography method for detecting tobacco flavors provided by the invention may further comprise the steps:
A, flavouring essence for tobacco to be measured is carried out pre-treatment, flavouring essence for tobacco is carried out pre-treatment can prevent a large amount of Bao Feng, influence testing result, and if do not carry out pre-treatment, sample stops up sample introduction needle easily, also can make internal lining pipe, the capillary column of chromatogram very fast contaminated, the present invention uses, and to be methylene chloride carry out pre-treatment as the liquid-liquid extraction method of extractant to flavouring essence for tobacco.
B, the liquid that contains fragrance matter that obtains after the pre-treatment is analyzed with GC-MS, GC-FID.GC-MS is the gas chromatography-mass spectrography technology, is the gas chromatography instrument is combined by suitable interface with mass spectrometer, by computer technology, can carry out qualitative analysis to the material with complex component.GC-FID is gas chromatography-flame ionization ditector coupling technique, can carry out quantitative test to material composition.
GC-MS is identical with the chromatographic condition of GC-FID among the present invention, and GC uses polar column, is the FFAP polar column, and preferred model is 60m * 0.25 μ m * 0.25mm.
Heating schedule is three rank heating schedules, furnace temperature is initially 30 ℃～60 ℃, keep 3min～8min, heating rate with 2 ℃/min～5 ℃/min heats up, the heating rate that is raised to after 80 ℃～150 ℃ with 3 ℃/min～8 ℃/min is warming up to 180 ℃～250 ℃, heating rate with 5 ℃/min～15 ℃/min is warming up to 200 ℃～300 ℃ again, keeps 20min～40min.As preferably, furnace temperature is initially 40 ℃, keeps 5min, heats up with the heating rate of 3 ℃/min, is raised to that the heating rate with 5 ℃/min is warming up to 200 ℃ after 100 ℃, and the heating rate with 8 ℃/min is warming up to 245 ℃ again, keeps 30min.
The preferred input mode sample introduction in GC shunt/do not shunted that adopts, sample introduction begins not shunt between sample introduction 0.5min～2min, begins shunting after sample introduction 0.5min～2min.As preferably, sample introduction begins not shunt between sample introduction 1min, begins shunting after the sample introduction 1min, and split ratio is 40: 1～60: 1, is preferably 50: 1.
The temperature of the injection port of GC is 200 ℃～300 ℃, is preferably 280 ℃.The detected temperatures of FID is 200 ℃～300 ℃, is preferably 280 ℃.
The operating conditions of MS is preferably 280 ℃ for the MS interface temperature is 200 ℃～300 ℃; The EI ion gun, electron energy 60eV～80eV is preferably 70eV, and ion source temperature is 200 ℃～300 ℃, is preferably 250 ℃; Sweep limit 30u～500u.
Embodiment 1:
Get flavouring essence for tobacco 1mL, this tobacco aromatics using is the product of Huafang Tobacco Flavors Co., Ltd., wherein the mass content of propylene glycol, glycerine and carbohydrate≤1%.In this flavouring essence for tobacco, add the 2mL methylene chloride, leave standstill after the vibration evenly, the mixing material layering, wherein organic layer presents light yellowly, gets light yellow organic layer liquid sample introduction, utilizes GC-MS to carry out qualitative analysis.
Use the GC of Agilent 6890, the MS of Finnigan, GC uses the FFAP polar column, and model is 60m * 0.25 μ m * 0.25mm.Flow rate of carrier gas 1.2mL/min.Three rank heating schedules are: initial 40 ℃ of furnace temperature, keep 5min, and heat up with the heating rate of 3 ℃/min, be raised to that the heating rate with 5 ℃/min is warming up to 200 ℃ after 100 ℃, the heating rate with 8 ℃/min is warming up to 245 ℃ again, keeps 30min.
Adopt input mode sample introduction in GC of shunt/not shunting, sample introduction begins not shunt between sample introduction 1min, begins shunting after the sample introduction 1min, and split ratio is 50: 1.
The temperature of the injection port of GC is 280 ℃.
The operating conditions of MS is 280 ℃ for the MS interface temperature; EI ion gun, electron energy are 70eV, and ion source temperature is 250 ℃; Sweep limit 30u～500u.
The GC-MS figure that detect to obtain please refer to Fig. 1, and Fig. 1 be that the GC-MS of flavouring essence for tobacco schemes under the operating conditions of embodiment 1.
Embodiment 2:
Get with embodiment 1 in identical tobacco aromatics using, identical among pre-treatment and the embodiment 1, get organic layer liquid sample introduction, utilize GC-FID to carry out detection by quantitative.
Flow rate of carrier gas 0.8mL/min.The detected temperatures of FID is 280 ℃, and the throughput ratio of hydrogen and air is 1: 10, and is identical among other GC conditions and the embodiment 1.
The GC-FID figure that detect to obtain please refer to Fig. 2, and Fig. 2 be that the GC-FID of flavouring essence for tobacco schemes under the operating conditions of embodiment 2.
Embodiment 3:
Get with embodiment 1 in identical tobacco aromatics using, identical among pre-treatment and the embodiment 1, get pale yellow chromatograph liquid sample introduction, utilize GC-FID to carry out detection by quantitative.
The three rank heating schedules of GC are: initial 40 ℃ of furnace temperature, keep 5min, and heat up with the heating rate of 4 ℃/min, be raised to that the heating rate with 3 ℃/min is warming up to 200 ℃ after 120 ℃, the heating rate with 6 ℃/min is warming up to 245 ℃ again, keeps 30min.
Identical among other operating conditions of GC and the embodiment 2.
The GC-FID figure that detect to obtain please refer to Fig. 3, and Fig. 3 be that the GC-FID of flavouring essence for tobacco schemes under the operating conditions of embodiment 3.
Comparative Examples 1:
Get with embodiment 1 in identical tobacco aromatics using, identical among pre-treatment and the embodiment 1, get organic layer liquid sample introduction, utilize GC-FID to carry out detection by quantitative.
Adopt input mode sample introduction in GC of shunting, promptly begin just shunting from sample introduction, split ratio adopts 50: 1.
Identical among other operating conditions of GC and the embodiment 2.
The GC-FID figure that detect to obtain please refer to Fig. 4, and Fig. 4 be that the GC-FID of flavouring essence for tobacco schemes under the operating conditions of Comparative Examples 1.
Comparative Examples 2:
Get with embodiment 1 in identical tobacco aromatics using, identical among pre-treatment and the embodiment 1, get organic layer liquid sample introduction, utilize GC-FID to carry out detection by quantitative.
GC heat up to adopt second order to heat up, and heating schedule is: initial 40 ℃ of furnace temperature, keep 5min, and heat up with the heating rate of 3 ℃/min, be raised to that the heating rate with 5 ℃/min is warming up to 245 ℃ after 180 ℃, keep 30min.
Identical among other operating conditions of GC and the embodiment 2.
The GC-FID figure that detect to obtain please refer to Fig. 5, and Fig. 5 be that the GC-FID of flavouring essence for tobacco schemes under the operating conditions of Comparative Examples 2.
At first carry out embodiment 1, use liquid-liquid extraction method known in the field to carry out pre-treatment, and utilize GC-MS to carry out qualitative analysis flavouring essence for tobacco to be measured.Embodiment 2 and embodiment 3 utilize GC-FID to carry out quantitative test flavouring essence for tobacco to be measured, adopt the input mode of shunt/not shunting, and use three rank heating schedules.Comparative Examples 1 is to utilize GC-FID to carry out quantitative test flavouring essence for tobacco to be measured, adopts the input mode of shunting.Comparative Examples 2 is to utilize GC-FID to carry out quantitative test flavouring essence for tobacco to be measured, uses the second order heating schedule.
Comparison diagram 2 is to Fig. 4, can see that Fig. 2 and Fig. 3 are obviously many than the peak that goes out among Fig. 4, particularly the peak of high boiling substance is more, can obtain more material information, increased the detection sensitivity of high boiling substance, as seen for polar column, the input mode of shunt/not shunting is better to the separating effect of flavouring essence for tobacco.
Can see among Fig. 5 that the material overlap of peaks that has together, not not separately, heating schedule is a second order, and use three rank heating schedules among Fig. 2 and Fig. 3, overlap peak is less, especially as the scheme of the three rank heating schedules of the preferred pairing embodiment 2 of Fig. 2, material peak good separating effect, detection sensitivity height.
More than chromatography method for detecting tobacco flavors provided by the present invention is described in detail.Used specific case herein principle of the present invention and embodiment are set forth, the explanation of above embodiment just is used for helping to understand method of the present invention and core concept thereof.Should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention, can also carry out some improvement and modification to the present invention, these improvement and modification also fall in the protection domain of claim of the present invention.
Claims (9)
1. a chromatography method for detecting tobacco flavors is characterized in that, may further comprise the steps:
A, tobacco aromatics using to be measured is carried out pre-treatment;
B, the liquid that contains fragrance matter that obtains after the pre-treatment is analyzed with GC-MS, GC-FID, GC uses polar column, heating schedule is three rank heating schedules, furnace temperature is initially 30 ℃～60 ℃, keep 3min～8min, heat up with the heating rate of 2 ℃/min～5 ℃/min, the heating rate that is raised to after 80 ℃～150 ℃ with 3 ℃/min～8 ℃/min is warming up to 180 ℃～250 ℃, heating rate with 5 ℃/min～15 ℃/min is warming up to 200 ℃～300 ℃ again, keeps 20min～40min;
C, employing are shunted/are regardless of and flow to sample loading mode, and the starting stage is split sampling not, begin shunting after sample introduction 0.5min～2min, and split ratio is 40: 1～60: 1.
2. red, orange, green, blue, yellow (ROGBY) according to claim 1, it is characterized in that, three rank heating schedules among the described step b are that furnace temperature is initially 40 ℃, keep 5min, heating rate with 3 ℃/min heats up, be raised to that the heating rate with 5 ℃/min is warming up to 200 ℃ after 100 ℃, the heating rate with 8 ℃/min is warming up to 245 ℃ again, keeps 30min.
3. red, orange, green, blue, yellow (ROGBY) according to claim 1 and 2 is characterized in that, the input mode of the shunting among the described step c/do not shunt is that sample introduction begins not shunt to sample introduction 1min, begins shunting after the sample introduction 1min.
4. red, orange, green, blue, yellow (ROGBY) according to claim 3 is characterized in that, the split ratio that begins to shunt after the described sample introduction 1min is 50: 1.
5. red, orange, green, blue, yellow (ROGBY) according to claim 1 and 2 is characterized in that, described polar column is the FFAP polar column.
6. red, orange, green, blue, yellow (ROGBY) according to claim 5 is characterized in that, the model of described FFAP polar column is 60m * 0.25 μ m * 0.25mm.
7. red, orange, green, blue, yellow (ROGBY) according to claim 1 and 2 is characterized in that, the temperature of the injection port of GC is 200 ℃～300 ℃ among the described step b.
8. red, orange, green, blue, yellow (ROGBY) according to claim 1 and 2 is characterized in that, the detected temperatures of FID is 200 ℃～300 ℃ among the described step b.
9. red, orange, green, blue, yellow (ROGBY) according to claim 1 and 2 is characterized in that, the operating conditions of MS is among the described step b: the MS interface temperature is 200 ℃～300 ℃; EI ion gun, electron energy 60eV～80eV, ion source temperature are 200 ℃～300 ℃; Sweep limit 30u～500u.
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| CN102721776A (en) * | 2012-05-29 | 2012-10-10 | 广东中烟工业有限责任公司 | Detection method for extract type spice |
| CN102830196A (en) * | 2012-09-25 | 2012-12-19 | 广东中烟工业有限责任公司 | Method for detecting quality of tobacco flavor |
| CN103436361A (en) * | 2013-08-05 | 2013-12-11 | 湖南中烟工业有限责任公司 | Intelligent fragrance blending and simulating method of cigarette flavor |
| CN104792898A (en) * | 2015-04-23 | 2015-07-22 | 红云红河烟草(集团)有限责任公司 | Quality analysis method for tobacco essence and spice |
| CN105891367A (en) * | 2016-04-27 | 2016-08-24 | 中国烟草总公司郑州烟草研究院 | Gas chromatography-quadrupole time-of-flight mass spectrometry/flame ionization detection method for tobacco essence perfume |
| CN105929070A (en) * | 2016-04-27 | 2016-09-07 | 中国烟草总公司郑州烟草研究院 | Gas chromatography-quadrupole time-of-flight mass spectrometry/flame ionization detection method of flavor components in cigarette mainstream smoke |
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| CN102721776A (en) * | 2012-05-29 | 2012-10-10 | 广东中烟工业有限责任公司 | Detection method for extract type spice |
| CN102830196A (en) * | 2012-09-25 | 2012-12-19 | 广东中烟工业有限责任公司 | Method for detecting quality of tobacco flavor |
| CN102830196B (en) * | 2012-09-25 | 2014-10-22 | 广东中烟工业有限责任公司 | Method for detecting quality of tobacco flavor |
| CN103436361A (en) * | 2013-08-05 | 2013-12-11 | 湖南中烟工业有限责任公司 | Intelligent fragrance blending and simulating method of cigarette flavor |
| CN103436361B (en) * | 2013-08-05 | 2015-08-05 | 湖南中烟工业有限责任公司 | The blending of a kind of flavouring essence for tobacco intelligence, imitative fragrant method |
| CN104792898A (en) * | 2015-04-23 | 2015-07-22 | 红云红河烟草(集团)有限责任公司 | Quality analysis method for tobacco essence and spice |
| CN105891367A (en) * | 2016-04-27 | 2016-08-24 | 中国烟草总公司郑州烟草研究院 | Gas chromatography-quadrupole time-of-flight mass spectrometry/flame ionization detection method for tobacco essence perfume |
| CN105929070A (en) * | 2016-04-27 | 2016-09-07 | 中国烟草总公司郑州烟草研究院 | Gas chromatography-quadrupole time-of-flight mass spectrometry/flame ionization detection method of flavor components in cigarette mainstream smoke |
| CN105891367B (en) * | 2016-04-27 | 2018-06-15 | 中国烟草总公司郑州烟草研究院 | A kind of gas-chromatography of essence spice for cigarette-quadrupole rod flight time mass spectrum/flame ion detection method |
| CN105929070B (en) * | 2016-04-27 | 2018-06-15 | 中国烟草总公司郑州烟草研究院 | The gas-chromatography of flavor component-quadrupole rod flight time mass spectrum/flame ion detection method in a kind of cigarette mainstream flue gas |
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