CN111272921A - Quick constant-pressure back-blowing GC-FID method for detecting neophytic diene in tobacco leaves and tobacco shreds - Google Patents
Quick constant-pressure back-blowing GC-FID method for detecting neophytic diene in tobacco leaves and tobacco shreds Download PDFInfo
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Abstract
A rapid constant-pressure back-blowing GC-FID method for detecting new plant diene in tobacco leaves and cut tobacco is characterized in that: drying and crushing tobacco leaves, sieving the tobacco leaves with a 40-mesh sieve, extracting the neophytadiene in the tobacco powder by using a solvent vortex, centrifuging the tobacco leaves, taking supernatant, and finally analyzing the supernatant by using constant-pressure back-flushing GC-FID. The invention has the outstanding advantages that: firstly, the method comprises the following steps: the new phytodiene in the tobacco leaves is analyzed by adopting a back-blowing technology, and compounds with boiling points higher than that of the new phytodiene in the tobacco leaves are blown out quickly, so that the cleanness of the whole analysis system is ensured, and the stability of the analysis method is improved. II, secondly: the constant-pressure back flushing is adopted, so that the back flushing method is suitable for gas chromatographs of Agilent 6890, 7890 and 8890 in various models. Thirdly, the method comprises the following steps: the analysis method has simple pretreatment, short analysis time of the instrument, and only 11 minutes for analyzing each sample, thereby improving the working efficiency.
Description
Technical Field
The invention relates to a rapid constant-pressure back-blowing GC-FID method for detecting neophytadiene in tobacco leaves and tobacco shreds.
Background
The neophytadiene is a polyisoprenoid flavor substance with 20 carbon atoms, and is an important flavor substance in tobacco leaves. Research shows that the new phytodiene is mainly derived from chlorophyll in natural green plants through degradation and conversion, and the mass fraction of the new phytodiene in tobacco leaves is about 0.06% -0.1%. The neophytadiene is used as a carrier for collecting aroma substances in the smoke aerosol, has the capability of carrying volatile aroma substances and aroma components in the tobacco leaves into smoke, and is an important flavoring agent of the tobacco leaves[1]. The change of the content of the new phytodiene can approximately reflect the change of the total amount of the neutral aroma components in the tobacco leaves. Different tobacco varieties, different growing environments and different processing technologies all have great influence on the content of the new-planted diene in tobacco leaves and smoke, and further the quality of the tobacco is influenced. Therefore, the understanding of the content of the new plant diene in the tobacco leaves under different varieties, different growth environments and different processing technological conditions has great significance.
The determination of neophytadiene in tobacco is mostly carried out with the analysis of trace aroma components in other tobacco, and the adopted method is SDE-GC-MS method[2-4]、LC-GC-MS method[5-6]、SPME-GC-MS[7-8]And the like. The content of the new phytodiene is too different from the content of other flavor components by hundreds of times and is not in one order of magnitude, the new phytodiene is not suitable for being put together for mass spectrum detection, when the content of other target components reaches a stable and better detection peak, the new phytodiene is basically in an overload condition and is difficult to accurately quantify, and the accurate content of the new phytodiene is suitable for being separately treated with other trace components and being independently detected. Meanwhile, the distillation and extraction pretreatment method is complex to operate, time-consuming and labor-consuming, and is difficult to meet the requirements of rapid and efficient analysis of a large number of samples in a big data era. The new phytodiene is obtained by dehydrating a chlorophyll degradation product phytol, and the content of the new phytodiene is influenced by high-temperature long-time distillation, so that the real content of the new phytodiene in tobacco leaves is difficult to reflect. Although the liquid-phase gas-phase series method realizes the on-line purification of the sample, the analysis time is longer, and the requirement on the configuration of the instrument is overhigh; when the solid-phase micro-extraction method is adopted, in order to achieve the purpose of fully enriching the target components, the time consumption is long, and the static extraction time of one sample needs 40 minutes. Under the condition of analyzing a large number of samples in the big data era, the current analysis method is not suitable for rapidly obtaining the accurate content of the neophytadiene in a large number of tobacco leaves and tobacco products. There are also patents relating to the extraction and detection of neophytadiene, in the detection of neophytadiene, the GC-FID method is adopted, since the tobacco leaf extraction sample is complicated, in order to ensure the cleanliness of the system and the stability of the method, the high temperature baking of the chromatographic column is needed, the analysis time is longer, and about 45min is needed for one sample[9]。
Generally, a sample with a complex matrix needs to be purified before chromatographic analysis, such as solid phase extraction, gel purification, headspace analysis and other technologies, in order to remove most impurities, reduce interference of the matrix, reduce loss of a chromatographic column and maintenance times of an instrument, and increase quantitative accuracy and stability. However, these pretreatment methods require expensive equipment, complicated steps, and a lot of time and labor.
The back flushing of the chromatographic analysis sample by utilizing the microfluidic device provides a new idea for purifying the analysis sample[10-11]。
Disclosure of Invention
The invention aims to provide a rapid constant-pressure back-blowing GC-FID method for detecting neophytadiene in tobacco leaves, which is specially used for solving the technical problems in the prior art. The method can be used for measuring the content of the new plant diene in the tobacco leaves under different tobacco varieties, different growth environments and different processing technologies, and is a rapid, efficient and accurate measuring method. The carrier gas adopts the condition of constant pressure, so that the back flushing method can be applied to not only Agilent 7890 and 8890 gas chromatographs (PCM can be set to be constant pressure or constant flow), but also Agilent 6890 gas chromatographs (the corresponding PCM can be set to be constant pressure only).
The purpose of the invention is realized by the following technical scheme:
a constant-pressure back-blowing GC-FID method for detecting neophytadiene in tobacco leaves comprises the following steps: drying and crushing tobacco leaves, sieving the tobacco leaves with a 40-mesh sieve, performing vortex extraction on the neophytadiene in the tobacco powder by using an extraction solvent, centrifuging the tobacco leaves, taking supernate, and finally performing analysis by adopting constant-pressure back-flushing GC-FID.
The method comprises the following specific steps:
(1) crushing tobacco leaves: drying flue-cured tobacco leaves, crushing and sieving to 40-60 meshes, and storing at room temperature;
(2) extraction of neophytadiene from tobacco leaves: weighing 30-50mg of pulverized tobacco powder into a 50mL centrifuge tube, adding an internal standard solution and an extract, performing vortex extraction, centrifuging, and taking supernatant;
(3) and (3) detection: and (3) performing detection analysis by adopting constant-pressure back-blowing GC-FID, wherein the pressure of the sample inlet is greater than the PCM pressure at the beginning, the sample is separated by the chromatographic column 1, the freshly planted diene enters the chromatographic column for 2,4.5min, the pressure of the sample inlet is reduced to 5psi at the rate of 99psi/min, and at the moment, the pressure of the sample inlet and the pressure of the detector in the direction are both less than the PCM pressure. The carrier gas flows from the PCM to the direction of the sample inlet, and is blown out from the direction of the sample inlet by reverse purging to blow out components which do not enter the chromatographic column 2; secondly, the mixture flows from the PCM to the detector, so that the components such as the new phytodiene entering the chromatographic column 2 reach the FID detector for quantitative analysis.
The chromatographic conditions were as follows:
a chromatographic column 1: DB-5ms (5m 0.25mm 0.25 μm),
and (3) chromatographic column 2: DB-5ms (10m × 0.25mm × 0.25 μm);
carrier gas, He; sample inlet temperature: 280 ℃; sample introduction amount: 1 mu L of the solution; the split ratio is 20: 1;
injection port pressure 19psi (hold 4.5min) then reduced to 5psi at 99psi/min (hold 2.5min)
PCM pressure: 15psi.
Temperature rising procedure: the initial temperature is 100 ℃, then the temperature is raised to 200 ℃ at the temperature raising speed of 20 ℃/min, and then the temperature is raised to 290 ℃ at the temperature raising speed of 90 ℃/min, and the temperature is kept for 5 min.
FID parameters: the temperature is 300 ℃, the hydrogen flow is 40mL/min, the air flow is 400mL/min, and the tail blowing flow is 25 mL/min.
The internal standard is n-heptadecane solution prepared by using an extraction solvent.
The extraction solvent is dichloromethane.
The invention has the outstanding advantages that: firstly, the method comprises the following steps: the new phytodiene in the tobacco leaves is analyzed by adopting a back-blowing technology, and compounds with boiling points higher than that of the new phytodiene in the tobacco leaves are blown out quickly, so that the cleanness of the whole analysis system is ensured, and the stability of the analysis method is improved. II, secondly: constant-pressure back flushing (constant-current control cannot be realized by PCM configured in an Agilent 6890 instrument) is adopted, so that the back flushing method is suitable for gas chromatographs of Agilent 6890, 7890 and 8890 in various models. Thirdly, the method comprises the following steps: the analysis method has simple pretreatment, short analysis time of the instrument and improved working efficiency.
Drawings
FIG. 1 is a flow chart of the detection steps of the present invention.
FIG. 2 is a chromatogram of the GC-FID obtained according to the present invention.
FIG. 3 is a schematic view of an air path system.
Detailed Description
The invention is further described below with reference to examples (figures) without restricting the invention thereto.
Example of content measurement:
(1) preparation of tobacco leaf samples
The tobacco leaves are dried and crushed, and then are screened by a 40-mesh sieve and packed in a sealing bag for later use at room temperature.
(2) Sample pretreatment
Weighing 50mg of tobacco powder in a 50mL centrifuge tube, adding 50 mu l of heptadecane internal standard solution and 10mL of dichloromethane solution, performing vortex extraction for 15min under the condition of 2500r/min, centrifuging for 3min under the condition of 10000r/min, taking supernate, filtering the supernate with a 2 mu m organic phase filter membrane, and placing the supernate in a 1.5mL chromatographic bottle.
(3) Conditions of gas chromatograph
The HP6890 gas chromatograph is provided with a FID detector, and is provided with PCM (pneumatic control module), namely a pneumatic control module.
A chromatographic column 1: DB-5ms (5m 0.25mm 0.25 μm),
and (3) chromatographic column 2: DB-5ms (10m × 0.25mm × 0.25 μm);
carrier gas, He; sample inlet temperature: 280 ℃; sample introduction amount: 1 mu L of the solution; the split ratio is 20: 1;
injection port pressure 19psi (hold 4.5min) then reduced to 5psi at 99psi/min (hold 2.5min)
PCM pressure: 15psi.
Temperature rising procedure: the initial temperature is 100 ℃, then the temperature is raised to 200 ℃ at the temperature raising speed of 20 ℃/min, and then the temperature is raised to 290 ℃ at the temperature raising speed of 90 ℃/min, and the temperature is kept for 5 min.
FID parameters: the temperature is 300 ℃, the hydrogen flow is 40mL/min, the air flow is 400mL/min, and the tail blowing flow is 25 mL/min.
(4) Determination of working curve and detection limit
Adopting dichloromethane as a solvent to respectively prepare a series of standard solutions containing neophytadiene, wherein the concentration of an internal standard substance n-heptadecane is 50 mu g/mL, the concentration of a 5-grade marking line of the neophytadiene is respectively 10, 20, 50, 100 and 200 mu g/mL, and carrying out linear regression analysis by the ratio of the peak area of each target substance to the peak area of the internal standard substance and the ratio of the concentration of each target substance to the concentration of the internal standard substance to obtain a standard working curve. Within the linear concentration range, the working curve of neophytadiene is well linear and suitable for quantitative analysis, see table 1.
Table 1 Standard working curves for the Compounds
Injecting: y is the ratio of peak areas of the target compound to the internal standard; x-ratio of concentration of target Compound to concentration of internal Standard
(4) Recovery and precision
The same tobacco sample was subjected to 6 replicates (table 2), the precision of the process was examined, and the recovery of the spiked sample was measured at three levels, high, medium and low (table 3). The result shows that the coefficient of variation of the new phytodiene measurement result is 1.81%, and the method recovery rate is between 98% and 100%, so that the method has good precision and high recovery rate.
TABLE 2 precision of sample determination (n ═ 6) (unit: mg/g)
| Compound (I) | 1 st time | 2 nd time | 3 rd time | 4 th time | 5 th time | 6 th time | Mean value of | RSD(％) |
| Novel phytodienes | 0.99 | 0.99 | 0.98 | 0.97 | 1.01 | 1.02 | 0.99 | 1.82 |
TABLE 3 recovery (%)
| Compound (I) | Low concentration (%) | Middle concentration (%) | High concentration (%) | Average recovery (%) |
| Novel phytodienes | 99 | 100 | 98 | 99 |
(5) Sample assay
10 representative tobacco leaf samples were analyzed and the results are shown in Table 4.
TABLE 4 tobacco leaf sample measurement results (mg/g)
| Tobacco leaf sample | Novel phytodienes |
| Tobacco sample-1 | 0.85 |
| Tobacco sample-2 | 0.84 |
| Tobacco sample-3 | 0.73 |
| Tobacco sample-4 | 0.93 |
| Tobacco sample-5 | 0.86 |
| Tobacco sample 6 | 0.82 |
| Tobacco sample 7 | 0.88 |
| Tobacco sample-8 | 0.76 |
| Tobacco sample-9 | 0.65 |
| Tobacco sample-10 | 0.91 |
Reference documents:
[1] kangming' e. Synthesis of neophytadiene, essence and perfume cosmetics 2016,4,1-3.
[2] Zhang Shuangshuang, Yan iron army, Liu Guo shun, etc. The research on the difference of chemical components and aroma substances of flue-cured tobaccos with different genotypes, Jiangsu agricultural science 2012,4, 286-.
[3] Weipeng course, Zhang Xiao Li, Return to school faithfulness, etc. The influence of different altitude conditions on the neutral aroma component content of the middle-flavor flue-cured tobacco, Tianjin agricultural science, 2017,23(8),72-75.
[4] Song Xiao Hua, Liu Guo Shun, pay admirable Yi, etc. The influence of the lengthening yellowing and the color fixing time on the content of neutral aroma components of the flue-cured tobacco in the baking process is 2010,22(2),249-252 in Zhejiang agricultural science.
[5] Flue-cured tobacco aroma substance analysis in different ecological areas [ J ] flue-cured tobacco science, 2015, 36 (3): 1-5.
[6] Flue-cured tobacco leaf aroma substance analysis of Guizhou tobacco section [ J ] in tobacco science, 2016, 37 (1): 37-43.
[7] Fanwenpin, gajuan, wangyitang, etc. studies on chemical components and volatile aroma substances of different genotype flue-cured tobaccos in qinling smoke area [ J ] report on agrobiological science of mountain region, 2016, 35 (6): 18-25.
[8] Study of chemical composition and key aroma-causing substance characteristics of flue-cured tobacco of jujuan, xijianxin, fan wen yi etc. [ J ]. shanxi agricultural science, 2016, 62 (11): 30-32.
[9] Wei Song, Zhao Xiao Yan, Cao Jian Min, etc. A method for extracting, purifying and detecting neophytadiene in tobacco and its application are disclosed in patent application publication No. CN 106501420A.
[10] Yang Zhen, He Li Dong. The back-blowing-gas chromatography method for rapidly detecting the main flavor substances in the beer, brewing in China, 2019,38(10),171-174.
[11] Liliang, Wuchunmi, Chenjianghang, etc. And (3) detecting organophosphorus pesticide residues in the vegetables by back-blowing gas chromatography, wherein the chromatography is 2010,28(7), 724-728.
Claims (6)
1. A rapid constant-pressure back-blowing GC-FID method for detecting new plant diene in tobacco leaves and cut tobacco is characterized in that: drying and crushing tobacco leaves or tobacco shreds, sieving with a 40-mesh sieve, extracting the neophytadiene in the tobacco powder by using an extraction solvent in a vortex mode, centrifuging, taking supernate, and finally analyzing by adopting constant-pressure back-blowing GC-FID.
2. The method of claim 1, wherein: the method comprises the following specific steps:
(1) preparing a tobacco sample: drying flue-cured tobacco leaves, crushing and sieving to 40-60 meshes, and storing at room temperature;
(2) extraction of neophytadiene from tobacco leaves: weighing 30-50mg of pulverized tobacco powder into a 50mL centrifuge tube, adding an extraction solvent containing an internal standard, performing vortex extraction, centrifuging, and taking supernatant;
(3) and (3) detection: constant pressure back flushing GC-FID is adopted for detection and analysis, and the chromatographic conditions are as follows:
a chromatographic column 1: DB-5ms, specification 5m × 0.25mm × 0.25 μm;
and (3) chromatographic column 2: DB-5ms, specification 10m × 0.25mm × 0.25 μm;
carrier gas, He; sample inlet temperature: 280 ℃; sample introduction amount: 1 mu L of the solution; the split ratio is 20: 1;
the injection port pressure was 19psi (hold 4.5min), then reduced to 5psi at 99psi/min, hold 2.5 min;
temperature rising procedure: the initial temperature is 100 ℃, then the temperature is raised to 200 ℃ at the temperature raising speed of 20 ℃/min, then the temperature is raised to 290 ℃ at the temperature raising speed of 90 ℃/min, and the temperature is kept for 5 min;
PCM pressure: 15psi.
FID parameters: the temperature is 300 ℃, the hydrogen flow is 40mL/min, the air flow is 400mL/min, and the tail blowing flow is 25 mL/min.
3. The method of claim 2, wherein: the internal standard is n-heptadecane solution prepared by using an extraction solvent.
4. A method according to claim 1 or 2 or 3, characterized in that: the extraction solvent is dichloromethane.
5. A method according to claim 2 or 3, characterized in that: the concentration of n-heptadecane in the internal standard was 50. mu.g/mL.
6. The method of claim 2, wherein: the specific conditions of centrifugation after vortex extraction in the step (2) are that vortex extraction is carried out for 15min under the condition of 2500r/min, and centrifugation is carried out for 3min under the condition of 10000 r/min.
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