CN111272921B - Rapid constant-pressure back-blowing GC-FID method for detecting neophytadiene in tobacco leaves and tobacco shreds - Google Patents
Rapid constant-pressure back-blowing GC-FID method for detecting neophytadiene in tobacco leaves and tobacco shreds Download PDFInfo
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Abstract
A rapid constant-pressure back-blowing GC-FID method for detecting neophytadiene in tobacco leaves and tobacco shreds is characterized by comprising the following steps: drying and crushing tobacco leaves, sieving with a 40-mesh sieve, extracting neophytadiene in the tobacco powder by using a solvent vortex, centrifuging, taking supernatant, and finally analyzing by adopting constant-pressure blowback GC-FID. The invention has the outstanding advantages that: and (3) a step of: the neophytadiene in the tobacco leaves is analyzed by adopting the back blowing technology, and the compounds with boiling point higher than that of the neophytadiene in the tobacco leaves are blown out rapidly, so that the cleanness of the whole analysis system is ensured, and the stability of the analysis method is improved. And II: the constant pressure back blowing is adopted, so that the back blowing method is suitable for gas chromatographs of various models of Agilent 6890, 7890 and 8890. Thirdly,: the analysis method has simple pretreatment and short instrument analysis time, and each sample is analyzed for only 11 minutes, so that the working efficiency is improved.
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, which can be used for determining the neophytadiene in various tobacco leaves and tobacco shreds and is a rapid, efficient and accurate neophytadiene analysis method.
Background
Neophytadiene is a polyisoprenoid aromatic substance with 20 carbon atoms, and is an important aroma substance in tobacco leaves. Research shows that the neophytadiene is mainly derived from chlorophyll in natural green plants through degradation and conversion, and the mass fraction of the neophytadiene in tobacco leaves is about 0.06% -0.1%. The neophytadiene is used as a carrier for trapping aroma substances in the smoke aerosol, has the capability of carrying volatile aroma substances and aroma components in tobacco leaves into the smoke, and is an important flavoring agent for the tobacco leaves [1] . The change of the content of the neophytadiene can reflect the change of the total amount of the neutral aroma components of the tobacco leaves. Different tobacco varieties, different growth environments and different processing technologies have great influence on the content of neophytadiene in tobacco leaves and smoke, and further influence the quality of the tobacco. Therefore, the method has great significance in knowing the content of the neophytadiene in the tobacco leaves under different varieties, different growth environments and different processing technology conditions.
The measurement of neophytadiene in tobacco is mostly analyzed together with trace aroma components in other tobacco by SDE-GC-MS method [2-4] LC-GC-MS method [5-6] 、SPME-GC-MS [7-8] Etc. The difference between the content of the neophytadiene and the content of other aroma components is too large and is hundreds of times, the content of the neophytadiene and the content of other aroma components are not in one order of magnitude, mass spectrum detection is unsuitable, when the content of other target components reaches a stable and better detection peak, the neophytadiene is basically in an overload condition, and is difficult to accurately quantify, so that the accurate content of the neophytadiene is obtained, and the neophytadiene is suitable for being treated separately from other trace componentsIt was detected separately. Meanwhile, the distillation and extraction pretreatment method is complex in operation, 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 large data age. The neophytadiene is dehydrated by phytol which is a chlorophyll degradation product, and is distilled at high temperature for a long time, so that the content of the neophytadiene is influenced, and the real content of the neophytadiene 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 instrument configuration is too high; when the solid-phase micro extraction method is adopted, the time for achieving the full enrichment of the target components is long, and the static extraction time of one sample is 40 minutes. Under the condition of analyzing a large number of samples in a big data era, the accurate content of neophytadiene in a large number of tobacco leaves and tobacco products is required to be obtained quickly, and the existing analysis method is unsuitable. There are also patents related to the extraction and detection of neophytadiene, in which GC-FID method is adopted, because the tobacco leaf extraction sample is complex, high temperature baking chromatographic column is required for ensuring the cleanliness of the system and the stability of the method, analysis time is long, and a sample is about 45min [9] 。
Generally, a sample with complex matrix needs purification treatment before chromatographic analysis, such as solid phase extraction, gel purification, headspace analysis and other technologies, so as to remove most of impurities, reduce interference of the matrix, reduce chromatographic column loss and instrument maintenance times, and increase quantitative accuracy and stability. However, these pretreatment methods require expensive equipment, complicated procedures, and are time-consuming and labor-consuming.
The microfluidic device is utilized to carry out back flushing on chromatographic analysis samples, thus providing a new thought for purifying the analysis samples [10-11] 。
Disclosure of Invention
The invention aims at providing a rapid constant-pressure blowback GC-FID method for detecting neophytadiene in tobacco leaves. The method can be used for measuring the content of the neophytadiene in the tobacco leaves under different tobacco varieties, different growing environments and different processing technologies, and is a quick, efficient and accurate measuring method. The carrier gas adopts the condition of constant pressure, so that the back blowing method can be applied to not only Yu Anjie-DEG 7890 and 8890 gas chromatographs (the PCM can be set to be constant pressure or constant current), but also Agilent 6890 gas chromatographs (the corresponding PCM can only be set to be constant pressure).
The aim 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 crushed tobacco leaves with a 40-mesh sieve, vortex extracting neophytadiene in the tobacco powder by using an extraction solvent, centrifuging, taking supernatant, and finally analyzing by adopting constant-pressure blowback GC-FID.
The method comprises the following specific steps:
(1) Crushing tobacco leaves: airing the flue-cured tobacco leaves, crushing and sieving the flue-cured tobacco leaves to 40-60 meshes, and preserving the flue-cured tobacco leaves at room temperature;
(2) Extraction of neophytadiene in tobacco leaves: weighing 30-50mg of crushed tobacco powder in 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) detecting and analyzing by adopting constant-pressure back-blowing GC-FID, wherein the pressure of the sample inlet is larger than the PCM pressure at the beginning, the sample is separated by the chromatographic column 1, the pressure of the sample inlet is reduced to 5psi at the speed of 99psi/min after the neophytadiene enters the chromatographic column 2 for 4.5min, and at the moment, the pressure of the sample inlet and the pressure of the detector direction are smaller than the PCM pressure. The carrier gas is divided into two directions, namely, flows from the PCM to the direction of the sample inlet, and is reversely purged to blow out the components which do not enter the chromatographic column 2 from the direction of the sample inlet; secondly, the component such as neophytadiene which enters the chromatographic column 2 is allowed to flow from the PCM to the detector to reach the FID detector for quantitative analysis.
The chromatographic conditions were as follows:
chromatographic column 1: DB-5ms (5 m.times.0.25 mm.times.0.25 μm),
chromatographic column 2: DB-5ms (10 m. Times.0.25 mm. Times.0.25 μm);
a carrier gas, he; sample inlet temperature: 280 ℃; sample injection amount: 1 μl; the split ratio is 20:1;
sample inlet pressure 19psi (hold 4.5 min) and then drop to 5psi (hold 2.5 min) at a rate of 99psi/min
PCM pressure: 15psi.
Heating program: the initial temperature is 100 ℃, then the temperature is increased to 200 ℃ at the heating rate of 20 ℃/min, and then the temperature is increased to 290 ℃ at the heating rate of 90 ℃/min, and the temperature is kept for 5min.
FID parameters: the temperature is 300 ℃, the hydrogen flow is 40mL/min, the air flow is 400 mL/min, and the tail blowing flow is 25 mL/min.
The internal standard is n-heptadecane solution prepared by extraction solvent.
The extraction solvent is dichloromethane.
The invention has the outstanding advantages that: and (3) a step of: the neophytadiene in the tobacco leaves is analyzed by adopting the back blowing technology, and the compounds with boiling point higher than that of the neophytadiene in the tobacco leaves are blown out rapidly, so that the cleanness of the whole analysis system is ensured, and the stability of the analysis method is improved. And II: constant-pressure back blowing (constant-current control cannot be realized by PCM configured by Agilent 6890 instruments) is adopted, so that the back blowing method is suitable for various types of Agilent 6890, 7890 and 8890 gas chromatographs. Thirdly,: the analysis method has simple pretreatment and short instrument analysis time, and improves the 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 in the present invention.
FIG. 3 is a schematic diagram of an air circuit system.
Detailed Description
The invention is further described below in connection with the examples (figures), but the invention is not limited thereto.
Content measurement example:
(1) Preparation of tobacco leaf samples
The tobacco leaves are crushed after being dried, and are put into a sealing bag for standby after passing through a 40-mesh sieve chamber.
(2) Sample pretreatment
Weighing 50mg of tobacco powder in a 50mL centrifuge tube, adding 50 μl of heptadecane internal standard solution and 10mL of dichloromethane solution, performing vortex extraction for 15min at 2500r/min, performing centrifugation for 3min at 10000r/min, and taking supernatant, and filtering the supernatant with a 2 [ mu ] m organic phase filter membrane in a 1.5mL chromatographic bottle.
(3) Gas chromatograph conditions
The HP6890 gas chromatograph is equipped with a FID detector and a PCM (pneumatic control module) pneumatic control module.
Chromatographic column 1: DB-5ms (5 m.times.0.25 mm.times.0.25 μm),
chromatographic column 2: DB-5ms (10 m. Times.0.25 mm. Times.0.25 μm);
a carrier gas, he; sample inlet temperature: 280 ℃; sample injection amount: 1 μl; the split ratio is 20:1;
sample inlet pressure 19psi (hold 4.5 min) and then drop to 5psi (hold 2.5 min) at a rate of 99psi/min
PCM pressure: 15psi.
Heating program: the initial temperature is 100 ℃, then the temperature is increased to 200 ℃ at the heating rate of 20 ℃/min, and then the temperature is increased to 290 ℃ at the heating rate of 90 ℃/min, and the temperature is kept for 5min.
FID parameters: the temperature is 300 ℃, the hydrogen flow is 40mL/min, the air flow is 400 mL/min, and the tail blowing flow is 25 mL/min.
(4) Determination of working curve and detection limit
And (3) respectively preparing a series of standard solutions containing neophytadiene by using methylene dichloride as a solvent, wherein the concentration of n-heptadecane as an internal standard substance is 50 mug/mL, the concentration of 5-grade marked lines of neophytadiene is 10 mug/mL, 20 mug/mL, 50 mug/mL, 100 mug/mL and 200 mug/mL, and performing linear regression analysis according to 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. In the linear concentration range, the working curve of the neophytadiene has good linearity and is suitable for quantitative analysis, as shown in Table 1。
* And (3) injection: y-ratio of peak area of target compound to internal standard; ratio of X-target compound concentration to internal standard concentration
(4) Recovery rate and precision
The same tobacco samples were subjected to 6 replicates (Table 2), the precision of the method was examined, and the sample addition recovery was determined at three levels, high, medium and low (Table 3). The result shows that the variation coefficient of the measured result of the neophytadiene is 1.81%, and the result of the recovery rate of the method is 98% -100%, so that the method has better precision and higher recovery rate.
Table 2 sample measurement precision (n=6) (unit: mg/g)
| Compounds of formula (I) | 1 st time | 2 nd time | 3 rd time | Fourth time | 5 th time | Last time (6) | Average value of | RSD（%） |
| New phytadienes | 0.99 | 0.99 | 0.98 | 0.97 | 1.01 | 1.02 | 0.99 | 1.82 |
TABLE 3 recovery (%)
| Compounds of formula (I) | Low concentration (%) | Middle concentration (%) | High concentration (%) | Average recovery (%) |
| New phytadienes | 99 | 100 | 98 | 99 |
(5) Sample measurement
10 representative tobacco samples were analyzed and the measurement results are shown in Table 4.
TABLE 4 tobacco sample measurement results (mg/g)
| Tobacco sample | New phytadienes |
| Smoke sample-1 | 0.85 |
| Smoke sample-2 | 0.84 |
| Smoke sample-3 | 0.73 |
| Smoke sample-4 | 0.93 |
| Smoke sample-5 | 0.86 |
| Smoke sample-6 | 0.82 |
| Smoke sample-7 | 0.88 |
| Smoke sample-8 | 0.76 |
| Smoke sample-9 | 0.65 |
| Smoke sample-10 | 0.91 |
Reference is made to:
[1] kang Minge. Synthesis studies of neophytadiene, perfume cosmetics, 2016, 4, 1-3.
[2] Zhang Shuangshuang, tiejun, liu Guoshun, etc. Chemical composition and aroma substances of flue-cured tobacco of different genotypes are studied differently, and Jiangsu agricultural science, 2012,4, 286-289.
[3] Wei Pengcheng, zhang Xiaoli, reiteration, etc. The influence of different altitude conditions on the content of neutral aroma components of the intermediate aroma type flue-cured tobacco is 2017,23 (8), 72-75.
[4] Song Xiaohua, liu Guoshun, pair encourage, etc. The influence of the elongation yellowing and the fixation time on the content of neutral aroma components of flue-cured tobacco in the baking process is 2010,22 (2), 249-252 of Zhejiang agricultural science.
[5] Li Lingyan, xu Yimin, liu Baizhan, etc. flue-cured tobacco aroma analysis in different ecological areas [ J ]. Chinese tobacco science, 2015, 36 (3): 1-5.
[6] Li Lingyan, xu Yimin, wang Chengdong, etc. flue-cured tobacco aroma analysis in Guizhou tobacco district [ J ]. China tobacco science, 2016, 37 (1): 37-43.
[7] Fan Wenju, gao Juanjuan, wang Yutang. Qinling mountain tobacco district chemical components of flue-cured tobacco of different genotypes and volatile aroma substance research [ J ]. Mountain agricultural biology journal, 2016, 35 (6): 18-25.
[8] Gao Juanjuan, zhang Jianxin, fan Wenju, etc. research on chemical composition of flue-cured tobacco in Qinling mountain and characteristics of key aroma-generating substances [ J ]. Agricultural science in shanxi, 2016, 62 (11): 30-32.
[9] Wei Song, zhao Xiaoyan, cao Jianmin, etc. A method for extracting, purifying and detecting neophytadiene in tobacco and application thereof, and the patent application publication number CN 106501420A.
[10] Yang Zhen, he Lidong. The back-flushing gas chromatography method is used for rapidly detecting main flavor substances in beer, and Chinese brewing is 2019,38 (10), 171-174.
[11] Bright plum, wu Chunmei, chen Jianhang, etc. Reverse-blowing gas chromatography to detect organophosphorus pesticide residues in vegetables, chromatography, 2010, 28 (7), 724-728.
Claims (4)
1. A rapid constant-pressure back-blowing GC-FID method for detecting neophytadiene in tobacco leaves is characterized by comprising the following steps of: drying and crushing tobacco leaves, sieving the crushed tobacco leaves with a 40-mesh sieve, vortex extracting neophytadiene in the tobacco powder by using an extraction solvent, centrifuging, taking supernatant, and finally analyzing by adopting constant-pressure blowback GC-FID, wherein the specific steps are as follows:
(1) Preparation of smoke samples: drying tobacco leaves, pulverizing, sieving to 40-60 mesh, and preserving at room temperature;
(2) Extraction of neophytadiene in tobacco leaves: weighing 30-50mg of crushed tobacco powder in a 50mL centrifuge tube, adding an extraction solvent containing an internal standard, performing vortex extraction, centrifuging, and taking supernatant; the internal standard is n-heptadecane solution prepared by an extraction solvent;
(3) And (3) detection: adopting constant-pressure back-blowing GC-FID for detection and analysis, adopting constant-pressure back-blowing, and enabling a back-blowing method to be suitable for gas chromatographs of Agilent 6890, 7890 and 8890 in various types;
the chromatographic conditions were as follows:
chromatographic column 1: DB-5ms, specification 5m 0.25mm 0.25 μm;
chromatographic column 2: DB-5ms, specification 10 m.times.0.25 mm.times.0.25 μm;
a carrier gas, he; sample inlet temperature: 280 ℃; sample injection amount: 1 μl; the split ratio is 20:1;
the sample inlet pressure is 19psi, kept for 4.5min, then reduced to 5psi at a rate of 99psi/min, and kept for 2.5min;
heating program: the initial temperature is 100 ℃, then the temperature is increased to 200 ℃ at the heating rate of 20 ℃/min, and then the temperature is increased to 290 ℃ at the heating rate of 90 ℃/min, and the temperature is kept for 5min;
PCM pressure: 15psi of the total pressure of the air,
FID parameters: the temperature is 300 ℃, the hydrogen flow is 40mL/min, the air flow is 400 mL/min, and the tail blowing flow is 25 mL/min.
2. The method according to claim 1, characterized in that: the extraction solvent is dichloromethane.
3. The method according to claim 1, characterized in that: the concentration of n-heptadecane in the internal standard was 50. Mu.g/mL.
4. The method according to claim 1, characterized in that: the specific conditions of the centrifugation after the vortex extraction in the step (2) are that the vortex extraction is carried out for 15min under the condition of 2500r/min, and the centrifugation is carried out for 3min under the condition of 10000 r/min.
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