CN110554113A - method for detecting volatile components in tobacco shreds based on SBSE-HS-GC-MS - Google Patents
method for detecting volatile components in tobacco shreds based on SBSE-HS-GC-MS Download PDFInfo
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- CN110554113A CN110554113A CN201910867341.1A CN201910867341A CN110554113A CN 110554113 A CN110554113 A CN 110554113A CN 201910867341 A CN201910867341 A CN 201910867341A CN 110554113 A CN110554113 A CN 110554113A
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Abstract
The invention relates to a method for detecting volatile components in tobacco shreds based on SBSE-HS-GC-MS, belonging to the technical field of tobacco chemistry. The method comprises three steps of sample pretreatment, HS-GC-MS detection and internal standard method quantification. The method for detecting the volatile components in the tobacco shreds by adopting the SBSE-HS-GC-MS method has the advantages of simple sample pretreatment, simple and convenient operation, accurate quantification and the like; the invention can adopt SBSE to accurately detect without adopting thermal desorption equipment, so the method is an ideal detection method for replacing SBSE-TD-GC-MS, has the advantages of high efficiency, concentration and enrichment and high sensitivity, is particularly suitable for extracting and separating trace volatile components in the tobacco shreds, and is favorable for comprehensively analyzing the volatile components in the tobacco shreds.
Description
Technical Field
The invention belongs to the technical field of tobacco chemistry, and particularly relates to a method for detecting volatile components in tobacco shreds based on SBSE-HS-GC-MS.
Background
With the development of the detection technology, compared with the detection technology which is 5 years ago, the detection technology has great progress in the aspects of accurate qualitative and quantitative determination, and has some new ideas and methods for the detection means of a complex substance system. These methods include: chromatographic and spectroscopic fingerprinting (HPLC-DAD, GC-FID, IR, UV) techniques, full two-dimensional chromatographic techniques, Multiple Reaction Monitoring (MRM) mass spectrometric techniques, etc. The technologies promote the progress of the detection technology of chemical components in tobacco and smoke, and play an important promoting role in controlling the quality of cigarette products and reducing harm and tar.
however, from the chemical components of tobacco shreds and smoke, the quality evaluation of cigarette products is a difficult problem which is troubling tobacco chemists. The method has the technical problems of three aspects, namely, too many factors are involved in the processing process of the cigarette product, internal and external substances are staggered, and the material basis related to the quality of the cigarette product cannot be determined; in the second aspect, because the components of tobacco and smoke are very complex and synergistic effects exist in a large quantity, the target substances related to the overall quality are not clear, and the quality of the cigarette product is difficult to judge by using basic detection data of one or more substances; in the third aspect, the chemical components of tobacco and smoke have trace (nanogram) and trace (microgram) concentration levels, which are difficult to be accurately determined by the current detection technology. The existence of these technical problems determines that the quality evaluation of cigarette products is difficult from the material basis.
Stirring magneton adsorption extraction (SBSE) is a new solid phase microextraction pretreatment technology, and is a sample pretreatment technology which has no solvent or less solvent and integrates extraction, purification and enrichment. SBSE has the advantages of large stationary phase volume, high extraction capacity and no need of additional stirring components. After being stirred by the technology, the stirrer is directly put into a thermal desorption unit TDU or a thermal desorption instrument TDS for thermal analysis, and then sent to a chromatograph for separation and detection, such as an SBSE-TD-GC-MS method. However, at present, due to the limitation of various reasons, thermal desorption equipment is not available for many times, so that the search for a detection method capable of replacing SBSE-TD-GC-MS is particularly important.
in addition, when the sample is processed by the existing SBSE-TD-GC-MS method, the sample can be damaged, so that the cell structure is damaged, the cell wall is broken, and cytoplasm and cell sap are dissolved out, so that the base peak is higher during detection, and the detection result is influenced. The problem to be solved in the art is urgent if the shortcomings of the prior art are overcome.
disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a method for detecting volatile components in tobacco shreds based on SBSE-HS-GC-MS, which has the advantages of simple sample pretreatment, simple and convenient operation, accurate quantification and the like.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a detection method for volatile components in tobacco shreds based on SBSE-HS-GC-MS comprises the following steps:
Step (1), sample pretreatment:
Adding an acetone solution of internal standard naphthalene into the cigarette tobacco shreds by taking naphthalene as an internal standard, sealing for a period of time, and adsorbing volatile components in the tobacco shreds by adopting an SBSE stirring rod;
Step (2), HS-GC-MS detection:
placing the SBSE stirring rod into a headspace sample injector for HS-GC-MS detection;
step (3), quantifying by an internal standard method:
The quantitative calculation formula is as follows:
；
In the formula:
Xn represents the content of the nth volatile component,. mu.g/g;
Mi represents the mass of internal standard added, μ g;
An denotes the chromatographic peak area of the nth volatile component;
Ai denotes the chromatographic peak area of the internal standard;
m denotes the mass, g, of the cut tobacco of cigarettes.
further, it is preferable that the concentration of the acetone solution of the internal standard naphthalene is 6. mu.g/mL.
further, it is preferable that 40. mu.L of internal standard naphthalene is added to cut tobacco of 10 cigarettes.
Further, it is preferable that the sealing time is 3 to 5 min.
Further, it is preferable that the adsorption time is 1.5 to 2.5 hours.
further, it is preferable that the specific method of step (1) is: putting 10 cigarettes into a small beaker, adding 40 mu L of acetone solution of internal standard naphthalene of 6 mu g/mL, reversely covering another large beaker on the small beaker, sealing for 3-5min, taking the large beaker, putting an SBSE stirring rod on the small beaker for adsorption, and taking down the large beaker after 2h for sample injection.
Further, it is preferable that the headspace condition is: temperature of the sampling needle: 120 ℃; transmission line temperature: 190 ℃; furnace temperature: 180 ℃; GC cycle time: 57 min; sample equilibration time: 30 min; pressurizing time: 0.20 min; sample introduction time: 0.1 min.
further, it is preferable that the GC conditions are: DB-5MS gas chromatographic column with specification of 30m × 0.25 mm × 0.25 μm and helium as carrier gas; the temperature of a sample inlet is 180 ℃; in a constant flow mode, the column flow is 1.0mL/min, and the split ratio is 20: 1; the temperature program was 50 ℃ for 1 minute, then 5 ℃/min to 200 ℃ for 10 minutes.
Further, it is preferable that the MS condition is: the auxiliary interface temperature, 220 ℃; ionization mode, electron bombardment source; ion source temperature, 180 ℃; ionization energy, 70 eV; the temperature of the quadrupole rods is 150 ℃; a full-scanning monitoring mode, wherein the scanning range is 50-300 amu; an ion monitoring mode is selected.
compared with the prior art, the invention has the beneficial effects that:
according to the invention, the SBSE-HS-GC-MS method is adopted to detect the volatile component samples in the tobacco shreds without pretreatment and balance, so that the operation is simple, convenient and rapid, and the quantification is accurate;
According to the invention, thermal desorption equipment is not adopted, and SBSE can be adopted for accurate detection, so that the method is an ideal detection method for replacing SBSE-TD-GC-MS;
the method has the advantages of high efficiency, concentration and enrichment, high sensitivity and relative standard deviation of less than 5%, is particularly suitable for extracting and separating trace volatile components in the tobacco shreds, and is favorable for comprehensively analyzing the volatile components in the tobacco shreds.
the invention overcomes the defects of the prior SBSE-TD-GC-MS method, and the SBSE stirring rod is not directly contacted with the tobacco shreds, thereby avoiding the influence of impurities and matrix effect and greatly improving the accuracy of the result. When TD is adopted for thermal desorption, the influence on thermosensitive substances is large, HS is directly adopted, the temperature is low and easy to control, the influence is greatly reduced, and the accuracy is improved.
Drawings
FIG. 1 is a total particle flow diagram of a gas chromatography mass spectrum of cigarette tobacco shreds.
Detailed Description
the present invention will be described in further detail with reference to examples.
it will be appreciated by those skilled in the art that the following examples are illustrative of the invention only and should not be taken as limiting the scope of the invention. The examples do not specify particular techniques or conditions, and are performed according to the techniques or conditions described in the literature in the art or according to the product specifications. The materials or equipment used are not indicated by manufacturers, and all are conventional products available by purchase.
example 1
a detection method for volatile components in tobacco shreds based on SBSE-HS-GC-MS comprises the following steps:
step (1), sample pretreatment:
Adding an acetone solution of internal standard naphthalene into the cigarette tobacco shreds by taking naphthalene as an internal standard, sealing for a period of time, and adsorbing volatile components in the tobacco shreds by adopting an SBSE stirring rod;
Step (2), HS-GC-MS detection:
Placing the SBSE stirring rod into a headspace sample injector for HS-GC-MS detection;
step (3), quantifying by an internal standard method:
the quantitative calculation formula is as follows:
；
In the formula:
Xn represents the content of the nth volatile component,. mu.g/g;
Mi represents the mass of internal standard added, μ g;
An denotes the chromatographic peak area of the nth volatile component;
Ai denotes the chromatographic peak area of the internal standard;
m denotes the mass, g, of the cut tobacco of cigarettes.
example 2
A detection method for volatile components in tobacco shreds based on SBSE-HS-GC-MS comprises the following steps:
step (1), sample pretreatment:
Adding an acetone solution of internal standard naphthalene into the cigarette tobacco shreds by taking naphthalene as an internal standard, sealing for a period of time, and adsorbing volatile components in the tobacco shreds by adopting an SBSE stirring rod;
the method specifically comprises the following steps:
Putting 10 cigarettes into a small beaker, adding 40 mu L of acetone solution of internal standard naphthalene at 6 mu g/mL, reversely covering another large beaker on the small beaker, sealing for 3min, taking the large beaker, putting an SBSE stirring rod on the small beaker for adsorption, and taking down the large beaker after 1.5h for sample injection;
step (2), HS-GC-MS detection:
Placing the SBSE stirring rod into a headspace sample injector for HS-GC-MS detection;
step (3), quantifying by an internal standard method:
The quantitative calculation formula is as follows:
；
In the formula:
Xn represents the content of the nth volatile component,. mu.g/g;
Mi represents the mass of internal standard added, μ g;
An denotes the chromatographic peak area of the nth volatile component;
Ai denotes the chromatographic peak area of the internal standard;
m denotes the mass, g, of the cut tobacco of cigarettes.
the headspace conditions were: temperature of the sampling needle: 120 ℃; transmission line temperature: 190 ℃; furnace temperature: 180 ℃; GC cycle time: 57 min; sample equilibration time: 30 min; pressurizing time: 0.20 min; sample introduction time: 0.1 min.
the GC conditions were: DB-5MS gas chromatographic column with specification of 30m × 0.25 mm × 0.25 μm and helium as carrier gas; the temperature of a sample inlet is 180 ℃; in a constant flow mode, the column flow is 1.0mL/min, and the split ratio is 20: 1; the temperature program was 50 ℃ for 1 minute, then 5 ℃/min to 200 ℃ for 10 minutes.
the MS conditions are as follows: the auxiliary interface temperature, 220 ℃; ionization mode, electron bombardment source; ion source temperature, 180 ℃; ionization energy, 70 eV; the temperature of the quadrupole rods is 150 ℃; a full-scanning monitoring mode, wherein the scanning range is 50-300 amu; an ion monitoring mode is selected.
example 3
a detection method for volatile components in tobacco shreds based on SBSE-HS-GC-MS comprises the following steps:
Step (1), sample pretreatment:
Adding an acetone solution of internal standard naphthalene into the cigarette tobacco shreds by taking naphthalene as an internal standard, sealing for a period of time, and adsorbing volatile components in the tobacco shreds by adopting an SBSE stirring rod;
the method specifically comprises the following steps:
Putting 10 cigarettes into a small beaker, adding 40 mu L of acetone solution of internal standard naphthalene at 6 mu g/mL, reversely covering another large beaker on the small beaker, sealing for 5min, taking the large beaker, putting an SBSE stirring rod on the small beaker for adsorption, and taking down the large beaker after 2.5h for sample injection;
step (2), HS-GC-MS detection:
Placing the SBSE stirring rod into a headspace sample injector for HS-GC-MS detection;
Step (3), quantifying by an internal standard method:
the quantitative calculation formula is as follows:
；
In the formula:
Xn represents the content of the nth volatile component,. mu.g/g;
Mi represents the mass of internal standard added, μ g;
An denotes the chromatographic peak area of the nth volatile component;
Ai denotes the chromatographic peak area of the internal standard;
m denotes the mass, g, of the cut tobacco of cigarettes.
the headspace conditions were: temperature of the sampling needle: 120 ℃; transmission line temperature: 190 ℃; furnace temperature: 180 ℃; GC cycle time: 57 min; sample equilibration time: 30 min; pressurizing time: 0.20 min; sample introduction time: 0.1 min.
the GC conditions were: DB-5MS gas chromatographic column with specification of 30m × 0.25 mm × 0.25 μm and helium as carrier gas; the temperature of a sample inlet is 180 ℃; in a constant flow mode, the column flow is 1.0mL/min, and the split ratio is 20: 1; the temperature program was 50 ℃ for 1 minute, then 5 ℃/min to 200 ℃ for 10 minutes.
the MS conditions are as follows: the auxiliary interface temperature, 220 ℃; ionization mode, electron bombardment source; ion source temperature, 180 ℃; ionization energy, 70 eV; the temperature of the quadrupole rods is 150 ℃; a full-scanning monitoring mode, wherein the scanning range is 50-300 amu; an ion monitoring mode is selected.
example 4
a detection method for volatile components in tobacco shreds based on SBSE-HS-GC-MS comprises the following steps:
Step (1), sample pretreatment:
adding an acetone solution of internal standard naphthalene into the cigarette tobacco shreds by taking naphthalene as an internal standard, sealing for a period of time, and adsorbing volatile components in the tobacco shreds by adopting an SBSE stirring rod;
The method specifically comprises the following steps:
putting 10 cigarettes into a small beaker, adding 40 mu L of acetone solution of internal standard naphthalene at 6 mu g/mL, reversely covering another large beaker on the small beaker, sealing for 4min, taking the large beaker, putting an SBSE stirring rod on the small beaker for adsorption, and taking down the large beaker after 2h for sample injection;
Step (2), HS-GC-MS detection:
placing the SBSE stirring rod into a headspace sample injector for HS-GC-MS detection;
step (3), quantifying by an internal standard method:
The quantitative calculation formula is as follows:
；
in the formula:
Xn represents the content of the nth volatile component,. mu.g/g;
Mi represents the mass of internal standard added, μ g;
An denotes the chromatographic peak area of the nth volatile component;
Ai denotes the chromatographic peak area of the internal standard;
m denotes the mass, g, of the cut tobacco of cigarettes.
the headspace conditions were: temperature of the sampling needle: 120 ℃; transmission line temperature: 190 ℃; furnace temperature: 180 ℃; GC cycle time: 57 min; sample equilibration time: 30 min; pressurizing time: 0.20 min; sample introduction time: 0.1 min.
the GC conditions were: DB-5MS gas chromatographic column with specification of 30m × 0.25 mm × 0.25 μm and helium as carrier gas; the temperature of a sample inlet is 180 ℃; in a constant flow mode, the column flow is 1.0mL/min, and the split ratio is 20: 1; the temperature program was 50 ℃ for 1 minute, then 5 ℃/min to 200 ℃ for 10 minutes.
the MS conditions are as follows: the auxiliary interface temperature, 220 ℃; ionization mode, electron bombardment source; ion source temperature, 180 ℃; ionization energy, 70 eV; the temperature of the quadrupole rods is 150 ℃; a full-scanning monitoring mode, wherein the scanning range is 50-300 amu; an ion monitoring mode is selected.
examples of the applications
The invention measures the cut tobacco of certain commercially available cigarette by adopting the method of example 4, the result is shown in table 1, and the total particle flow diagram of the gas chromatography mass spectrum is shown in figure 1.
TABLE 1
The measurement method of the present example can be accurate to 0.0001. mu.g/10 counts, and has very high sensitivity.
the foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (9)
1. a detection method for volatile components in tobacco shreds based on SBSE-HS-GC-MS is characterized by comprising the following steps:
Step (1), sample pretreatment:
Adding an acetone solution of internal standard naphthalene into the cigarette tobacco shreds by taking naphthalene as an internal standard, sealing for a period of time, and adsorbing volatile components in the tobacco shreds by adopting an SBSE stirring rod;
Step (2), HS-GC-MS detection:
Placing the SBSE stirring rod into a headspace sample injector for HS-GC-MS detection;
Step (3), quantifying by an internal standard method:
The quantitative calculation formula is as follows:
；
In the formula:
Xn represents the content of the nth volatile component,. mu.g/g;
Mi represents the mass of internal standard added, μ g;
An denotes the chromatographic peak area of the nth volatile component;
Ai denotes the chromatographic peak area of the internal standard;
m denotes the mass, g, of the cut tobacco of cigarettes.
2. the SBSE-HS-GC-MS-based detection method of volatile components in tobacco shreds according to claim 1, wherein the concentration of acetone solution of internal standard naphthalene is 6 μ g/mL.
3. the SBSE-HS-GC-MS-based detection method for volatile components in tobacco shreds according to claim 1, wherein 40 μ L of internal standard naphthalene is added into tobacco shreds of 10 cigarettes.
4. The SBSE-HS-GC-MS-based detection method for volatile components in tobacco shreds according to claim 1, wherein the sealing time is 3-5 min.
5. the SBSE-HS-GC-MS-based detection method of volatile components in tobacco shreds according to claim 1, wherein the adsorption time is 1.5-2.5 h.
6. the SBSE-HS-GC-MS-based detection method for volatile components in tobacco shreds according to claim 1, wherein the specific method in step (1) is as follows: putting 10 cigarettes into a small beaker, adding 40 mu L of acetone solution of internal standard naphthalene of 6 mu g/mL, reversely covering another large beaker on the small beaker, sealing for 3-5min, taking the large beaker, putting an SBSE stirring rod on the small beaker for adsorption, and taking down the large beaker after 2h for sample injection.
7. The SBSE-HS-GC-MS-based detection method for volatile components in tobacco shreds according to claim 1, wherein the headspace conditions are as follows: temperature of the sampling needle: 120 ℃; transmission line temperature: 190 ℃; furnace temperature: 180 ℃; GC cycle time: 57 min; sample equilibration time: 30 min; pressurizing time: 0.20 min; sample introduction time: 0.1 min.
8. the SBSE-HS-GC-MS-based detection method for volatile components in tobacco shreds according to claim 1, wherein GC conditions are as follows: DB-5MS gas chromatographic column with specification of 30m × 0.25 mm × 0.25 μm and helium as carrier gas; the temperature of a sample inlet is 180 ℃; in a constant flow mode, the column flow is 1.0mL/min, and the split ratio is 20: 1; the temperature program was 50 ℃ for 1 minute, then 5 ℃/min to 200 ℃ for 10 minutes.
9. the SBSE-HS-GC-MS-based detection method for volatile components in tobacco shreds according to claim 1, wherein MS conditions are as follows: the auxiliary interface temperature, 220 ℃; ionization mode, electron bombardment source; ion source temperature, 180 ℃; ionization energy, 70 eV; the temperature of the quadrupole rods is 150 ℃; a full-scanning monitoring mode, wherein the scanning range is 50-300 amu; an ion monitoring mode is selected.
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