CN109781879A - A method of fragrance component in tobacco aromaticss is extracted using the Soxhlet extraction device with Solid Phase Extraction function - Google Patents
A method of fragrance component in tobacco aromaticss is extracted using the Soxhlet extraction device with Solid Phase Extraction function Download PDFInfo
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- CN109781879A CN109781879A CN201910028005.8A CN201910028005A CN109781879A CN 109781879 A CN109781879 A CN 109781879A CN 201910028005 A CN201910028005 A CN 201910028005A CN 109781879 A CN109781879 A CN 109781879A
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Abstract
The present invention discloses a kind of method for extracting fragrance component in tobacco aromaticss using the Soxhlet extraction device with Solid Phase Extraction function, includes the following steps: that (1) tobacco aromaticss sample extraction flows back；(2) tobacco aromaticss sample concentration；(3) sample to be tested after step (2) concentration is analyzed using LC-MS.The present invention makes a kind of Soxhlet extraction device with Solid Phase Extraction function by oneself, the device can carry out separating-purifying, concentration to sample in confined conditions, the present invention is not necessarily to need the operating procedure of repeatedly transfer, concentration as traditional separating-purifying, concentration, substantially increases extraction efficiency.
Description
Technical field
The invention belongs to tobacco aromaticss chemical analysis technology fields, in particular to a kind of to utilize the rope with Solid Phase Extraction function
The method that family name's extraction element extracts fragrance component in tobacco aromaticss.
Background technique
Flavors and fragrances is the important source material of production, plays special effect in terms of keeping selling point and flavor,
And has great importance also for interior qualities such as the style of product stabilizations, therefore keep the stability of flavors and fragrances especially
It is important.For most flavors and fragrances, the loss of its fragrant ingredient is to influence quality in storage and use process
One key factor of stability.
Flavors and fragrances plays its special effect on keeping product feature style and product quality, in order to keep product
Stable style and quality keeps the stability of flavors and fragrances particularly important in production process.Therefore it establishes accurate and reliable
Flavors and fragrances in the analysis method whether lost of fragrance component, and pass through the accurate analysis of fragrance component, determine that its quality is steady
It is qualitative, have great importance to the quality holding of product.
About fragrance ingredient volatilization loss, fragrance component is accurately analyzed by modern chromatographic techniques, utilizes the modern times
Fingerprint chromatogram technology can identify its self-consistent property, in addition also have electronic nose, NIR transmittance spectroscopy, ultraviolet spectra with
The report of the methods of Fourier transformation.Wherein, gas chromatography-mass spectrography is most common method.But flavors and fragrances
Fragrance component content is different, complicated composition, to analyze these ingredients it may first have to volatile component in sample into
A series of pre-treatments such as row extraction, purification, concentration.Currently, common pre-treating method mainly has steam distillation, molecule to steam
It evaporates, the extraction of Simultaneous distillation-extraction, ultrasonic solvent, Soxhlet extraction, solid phase microextraction, supercritical extract etc.；These methods respectively have spy
Point, but it is all insufficient there is be easy to causeing fragrance component to extract, the shortcomings that losing is easy in purification process.
Since the quality stability and style maintenance of flavors and fragrances and product are of close concern to each other, urgently by more wide
The invention of the sample-pretreating method of spectrality improves the measurement defect of flavors and fragrances fragrance component, and can be with by these methods
The fragrance loss situation of flavors and fragrances low to component content, complicated composition is effectively monitored.
Summary of the invention
It is extracted in tobacco aromaticss the object of the present invention is to provide a kind of using the Soxhlet extraction device with Solid Phase Extraction function
The method of fragrance component, efficiently solving interference when extracting fragrance component in tobacco aromaticss, greatly, the fragrance component rate of recovery is low
Problem, and without processes such as repeatedly extraction, transfer, concentrations, entire sample pretreatment process high-efficient simple has ensured detection knot
The accuracy and precision of fruit.
Unless otherwise indicated, percentage of the present invention is weight percent.
First aspect present invention is related to a kind of using in the Soxhlet extraction device extraction tobacco aromaticss with Solid Phase Extraction function
The method of fragrance component, includes the following steps:
(1) tobacco aromaticss sample extraction flows back: silica gel particle and silico-tungstic acid particle are successively added in solid-phase extraction column 9,
2~10g tobacco aromaticss sample is weighed in sample cylinder 8, sample cylinder 8 and solid-phase extraction column 9 are tightly connected, by chromatography column feed materials
The hickey 2 of bottle and round-bottomed flask 1 is tightly connected, and the solvent of 50~100mL is added in round-bottomed flask 1, and solid phase is extracted
It takes column 9 to be tightly connected by solvent refluxing pipe 6 and second interface 4, heat-insulated gas-guide tube 5 is tightly connected with first interface 3, by three
Three interfaces of logical transfer tube 7 are tightly connected with sample cylinder 8, sealed condensating pipe 10 and heat-insulated gas-guide tube 5 respectively, sealed condensating pipe
10 connect condensed water, and finally flask is placed in water-bath, and 60~80 DEG C of heating are condensed back 0.25~4h；
(2) tobacco aromaticss sample concentration: to step (1) back flow of sample extract after, switching three-way valve 13, make its with
Outside air conducting, the solvent constantly to volatilize are flowed out and are recycled by triple valve 13, and the solution in flask 1 is constantly concentrated into
Solvent volatilization finishes；
(3) sample to be tested after step (2) concentration is analyzed using LC-MS.
In the preferred embodiment of the invention, the solvent that step (1) is added in flask 1 is methyl acetate or methylene chloride.
In the preferred embodiment of the invention, step (1) further includes covering anhydrous sodium sulfate on silico-tungstic acid particle.
In the preferred embodiment of the invention, the analysis condition of step (3) are as follows:
Chromatographic condition: DB-5MS (60m × 0.25mm × 0.32 μm or equivalent specifications chromatographic column；Carrier gas is He, and flow velocity is
1mL/min；Sample volume is 1 μ L, and injector temperature is 250 DEG C, input mode are as follows: split sampling, split ratio: 25:1；Gradient liter
Warm program are as follows: 50 DEG C of initial temperature lasting 5min are warming up to 240 DEG C with the heating rate of 3 DEG C/min, continue 5min, with 2 DEG C/
The heating rate of min is warming up to 250 DEG C, continues 30min；Mass Spectrometry Conditions: ionization mode is EI, and ion source temperature is 180 DEG C, electricity
From that can be 70eV, using (full scan) mode is swept entirely, scanning range be 45~450amu.
Second aspect of the present invention is related to a kind of Soxhlet extraction device with Solid Phase Extraction function, including such as lower component:
Flask 1, flask 1 be equipped with first interface 3, second interface 4 and hickey 2, flask 1 by first interface 3 with
Connection, threeway switching are connected with 7 air-flow of threeway transfer tube for heat-insulated 5 air-flow of gas-guide tube conducting connection, heat-insulated 5 other end of gas-guide tube
Connection is connected with closed condenser pipe 10 and 8 air-flow of sample cylinder respectively in other two interface of pipe 7, and closed condenser pipe 10 is equipped with
Relief valve 11, sample cylinder 8 are equipped with sieve plate 12 far from one end of threeway transfer tube 7 and connection are connected with 9 air-flow of solid-phase extraction column, Gu
Connection is connected with 4 air-flow of second interface by solvent refluxing pipe 6 for the other end of phase extraction column 9, is equipped with threeway in solvent refluxing pipe 6
Valve 13.
In the preferred embodiment of the invention, silico-tungstic acid particle and silica gel particle are accommodated in solid-phase extraction column 9.
In the preferred embodiment of the invention, hickey 2 is detachably connected with chromatography column feed materials bottle 15.
In the preferred embodiment of the invention, heat-insulated gas-guide tube 5 and solvent refluxing pipe 6 use soft material, such as PES；Tool
There is certain retractility, facilitates the assembly and connection in operating process.
In the preferred embodiment of the invention, sample cylinder 8 and solid-phase extraction column 9 are the plastics material of organic solvent-resistant corrosion
Matter, sieve plate 12 are that plastics sieve plate or metal sieve plate, remaining part, such as flask 1, triple valve 13 and closed condenser pipe 10 are glass
Glass material.
In the preferred embodiment of the invention, closed condenser pipe 10 is equipped with relief valve 11, and dress is extracted when being heated to reflux
When setting middle hypertonia can releasing pressure automatically, prevent hypertonia from damaging to device.
In the preferred embodiment of the invention, solid-phase extraction column 9 has loaded silico-tungstic acid particle and silica gel particle, is carrying out sample
Product pre-treatment fills in solid-phase extraction column 9 using preceding prepackage, directly uses in sample pretreatment process.
In the preferred embodiment of the invention, triple valve 13 is set, changeable solvent flows back to flask 1 in solvent refluxing pipe 6
Or flow out to outside flask 1, realize the switching that back flow of sample is extracted and is concentrated.
In the preferred embodiment of the invention, total interface junction is all made of gripping means grips in extraction element, connects
Mouth has sealing ring, guarantees the leakproofness of extraction element in use, while guaranteeing the pressure limit in relief valve pressure release
Interior each interface will not gas leakage.
The course of work of Soxhlet extraction device with Solid Phase Extraction function in the present invention is as follows:
When sample analysis, silico-tungstic acid particle and silica gel particle are added in solid-phase extraction column 9, is packed into and claims in sample cylinder 8
Measured sample covers one layer of anhydrous sodium sulfate (for removing the moisture in solvent and pipeline), by sample cylinder 8 above sample
It is tightly connected with solid-phase extraction column 9, the solvent (methylene chloride and internal standard compound) of refluxing extraction is added in flask 1, solid phase is extracted
It takes column 9 to be tightly connected by solvent refluxing pipe 6 and second interface 4, heat-insulated gas-guide tube 5 is tightly connected with first interface 3, by three
Three interfaces of logical transfer tube 7 are tightly connected with sample cylinder 8, sealed condensating pipe 10 and heat-insulated gas-guide tube 5 respectively, sealed condensating pipe
10 connect condensed water, and finally flask is placed in water-bath or oil bath pan and heats condensing reflux.In sample extraction process, solvent is returned
The triple valve 13 of flow tube 6 is connected with 4 air-flow of second interface, and the solvent of volatilization is by sample to be tested extracted in solid-phase extraction column 9
It is back in flask 1, after sample extraction, triple valve 13 is adjusted to the state be connected with outside air, constantly volatilize
Solvent flow out and recycle by triple valve 13, the solution in flask 1 is constantly concentrated until solvent is evaporated at this time, Ji Kejin
The detection of row chromatography.
The invention has the advantages that:
1, the present invention makes a kind of Soxhlet extraction device with Solid Phase Extraction function by oneself, which can be right in confined conditions
Sample carries out separating-purifying, is concentrated, and the present invention is not necessarily to need the operation of repeatedly transfer, concentration as traditional separating-purifying, concentration
Step substantially increases extraction efficiency.
2, the homemade extraction element of the present invention uses totally enclosed condenser pipe, effectively prevents the volatilization damage of Extraction solvent
It loses, greatly reduces sample pretreatment process pollution caused by laboratory environment；Also, closed condenser has relief valve,
When hypertonia can releasing pressure automatically, effectively preventing may be because hypertonia is damage caused by extraction element.
3, triple valve is set in solvent refluxing pipe in the homemade extraction element of the present invention, can be directly cut by switch valve
Product refluxing extraction and concentration are varied, entire operation process does not need transfer sample；Connection chromatography column feed materials have also been devised in the present apparatus
The round-bottomed flask of bottle interface, after the completion of sample concentration, screwing off chromatography column feed materials bottle can directly be analyzed, and conventional sample is avoided
After tail pipe concentration flask has been concentrated, the step of solution in tail pipe need to being taken out and washed tail pipe and suction pipe with suction pipe.Further letter
Sample pre-treatments operation is changed.
4, the GCMS analysis method high by easy to operate pre-treatment and accuracy, can effectively differentiate in flavors and fragrances
The damaed cordition of fragrance component has the advantages that accurate, reliable.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of present invention self-control extraction and cleaning device；
Fig. 2 is operation schematic diagram of the invention；
Fig. 3 is the analysis of aroma components chromatogram of Yunnan tobacco alcohol extracting thing；
Appended drawing reference meaning is as follows in figure:
1- flask, 2- hickey, 3- first interface, 4- second interface, the heat-insulated gas-guide tube of 5-, 6- solvent refluxing pipe, 7-
Threeway transfer tube, 8- sample cylinder, 9- solid-phase extraction column, the closed condenser pipe of 10-, 11- relief valve, 12- sieve plate, 13- triple valve,
14- silico-tungstic acid particle and silica gel particle, 15- chromatography column feed materials bottle.
Specific embodiment
Below in conjunction with specific example, the present invention will be described in detail, but is not intended to limit the present invention.
Embodiment 1
The present embodiment using tobacco extract sample as investigation object, investigate respectively the method for the present invention and Simultaneous distillation,
The method precision of headspace analysis.
Analytic process is as follows:
(1) sample extraction, concentration: successively filling 10g silica gel particle and 2.5g anhydrous sodium sulfate in solid-phase extraction column 9,
Then it is added in sample cylinder 8 after the silica gel of sample to be tested 2.5g and 5.0g being fully ground uniformly；After installing sample, with folder
Tight device sealing, and 60mL methyl acetate solvent is added in flask 1, then above-mentioned apparatus is put into water-bath at 68 DEG C
It is heated to reflux 45min.After sample extraction is complete, triple valve 13 is opened, solvent is allowed to flow out recycling design from solvent recovery mouth, until burning
Sample solution in 1 tail pipe of bottle is evaporated to dryness, and the sample being concentrated dissolves residue using 1mL ethyl alcohol, and carries out GC-MS detection
Analyze related fragrance component.
(2) chromatographic condition: DB-5MS (60m × 0.25mm (internal diameter) × 0.32 μm (film thickness) or equivalent specifications chromatographic column；
Carrier gas is He, flow velocity 1mL/min；Sample volume is 1 μ L, and injector temperature is 250 DEG C, input mode are as follows: split sampling, point
Flow ratio: 25:1；Gradient increased temperature program are as follows: 50 DEG C of initial temperature lasting 5min are warming up to 240 DEG C with the heating rate of 3 DEG C/min,
Continue 5min, be warming up to 250 DEG C with the heating rate of 2 DEG C/min, continues 30min；Mass Spectrometry Conditions: ionization mode is EI, ion
Source temperature is 180 DEG C, ionization energy 70eV, and using (full scan) mode is swept entirely, scanning range is 45~450amu； MS
Retrieval spectrum library is the library NIST.
The precision of fragrance component compares (n=9) in 1 three kinds of method measurement tobacco extracts of table
From table 1 it follows that method precision of the invention is more preferably, for the collimation effect of the measurement of same sample
More excellent, the fragrance loss situation for monitoring flavors and fragrances has better stability monitoring ability.
Embodiment 2
It is investigation object that the present embodiment, which selects 11 flavors and fragrances samples, and wherein 1-5 is medicinal extract class sample, 6,8,10 samples
Product be essence sample, wherein 7,9,11 be 6,8,10 samples place one section when after sample (place condition: production of cigarettes workshop
It is interior, at room temperature, be not protected from light directly, spiral cover bottle is placed, and is not done other sealings, is carried out corkage sampling daily).
Analytic process is as follows:
(1) sample extraction, concentration: 10g silica gel particle and 2.5g anhydrous sodium sulfate are filled in solid-phase extraction column 9, then
It is added in sample cylinder 8 after sample to be tested 2.5g and 5.0g silica gel is fully ground uniformly；It is close with clamping device after installing sample
Envelope, and 60mL methyl acetate solvent is added in flask 1, then above-mentioned apparatus is put into water-bath and is heated to reflux at 75 DEG C
2h.After sample extraction is complete, triple valve 13 is opened, solvent is allowed to flow out recycling design from solvent recovery mouth, until in 1 tail pipe of flask
Sample solution is evaporated to dryness, the accurate constant volume of the sample being concentrated to 5.0mL, dissolves residue with 1mL ethyl alcohol, and carry out GC-MS
Test and analyze related fragrance component.
(2) chromatographic condition: chromatographic column: DB-5MS (60m × 0.25mm (internal diameter) × 0.32 μm of (film thickness) or equivalent specifications
Chromatographic column；Carrier gas is He, flow velocity 1mL/min；Sample volume is 1 μ L, and injector temperature is 250 DEG C, input mode are as follows: be diverted into
Sample, split ratio: 25:1；Gradient increased temperature program are as follows: 50 DEG C of initial temperature lasting 5min are warming up to the heating rate of 3 DEG C/min
240 DEG C, continue 5min, be warming up to 250 DEG C with the heating rate of 2 DEG C/min, continues 30min；Mass Spectrometry Conditions: ionization mode is
EI, ion source temperature are 180 DEG C, ionization energy 70eV, and using (full scan) mode is swept entirely, scanning range is 45~450
amu；MS retrieval spectrum library is the library NIST.
The analytical table of the representative volatile compound of table 2
It is found from table 2, which can not only carry out effectively to the fragrance component situation of flavors and fragrances
It detects (No. 1-5), but also can be to the fragrance for the flavors and fragrances sample for placing a period of time and (sampling and produce in simulated production)
Damaed cordition is monitored, and as a result using well, can provide good technology hand for the quality judging of flavors and fragrances and monitoring
Section.
Claims (5)
1. a kind of method for extracting fragrance component in tobacco aromaticss using the Soxhlet extraction device with Solid Phase Extraction function, feature
It is, includes the following steps:
(1) tobacco aromaticss sample extraction flows back: silica gel particle and silico-tungstic acid particle being successively added in solid-phase extraction column (9), claims
Take 2~10g tobacco aromaticss sample in sample cylinder (8), sample cylinder (8) and solid-phase extraction column (9) be tightly connected, by chromatography into
The hickey (2) of sample bottle and round-bottomed flask (1) is tightly connected, and the solvent of 50~100mL is added in round-bottomed flask (1),
Solid-phase extraction column (9) are tightly connected by solvent refluxing pipe (6) and second interface (4), heat-insulated gas-guide tube (5) is connect with first
Mouthful (3) are tightly connected, by three interfaces of threeway transfer tube (7) respectively with sample cylinder (8), sealed condensating pipe (10) and heat-insulated lead
Tracheae (5) is tightly connected, and sealed condensating pipe (10) connects condensed water, and finally flask is placed in water-bath, 60~80 DEG C of heating,
It is condensed back 0.25~4h；
(2) tobacco aromaticss sample concentration: after extracting to step (1) back flow of sample, switching three-way valve (13) makes itself and the external world
Air conducting, the solvent constantly to volatilize are flowed out and are recycled by triple valve (13), and the solution in flask (1) is constantly concentrated into molten
Agent volatilization finishes；
(3) sample to be tested after step (2) concentration is analyzed using LC-MS.
2. the Soxhlet extraction device according to claim 1 using with Solid Phase Extraction function extract in tobacco aromaticss fragrance at
The method divided, which is characterized in that the solvent that step (1) is added in flask (1) is methyl acetate or methylene chloride.
3. the Soxhlet extraction device according to claim 2 using with Solid Phase Extraction function extract in tobacco aromaticss fragrance at
The method divided, which is characterized in that step (1) further includes covering anhydrous sodium sulfate on silico-tungstic acid particle.
4. the Soxhlet extraction device according to claim 3 using with Solid Phase Extraction function extract in tobacco aromaticss fragrance at
The method divided, which is characterized in that the analysis condition of step (3) are as follows:
Chromatographic condition: DB-5MS (60m × 0.25mm × 0.32 μm or equivalent specifications chromatographic column；Carrier gas is He, flow velocity 1mL/
min；Sample volume is 1 μ L, and injector temperature is 250 DEG C, input mode are as follows: split sampling, split ratio: 25:1；Gradient increased temperature journey
Sequence are as follows: 50 DEG C of initial temperature lasting 5min are warming up to 240 DEG C with the heating rate of 3 DEG C/min, continue 5min, with 2 DEG C/min's
Heating rate is warming up to 250 DEG C, continues 30min；Mass Spectrometry Conditions: ionization mode is EI, and ion source temperature is 180 DEG C, ionization energy
For 70eV, using (full scan) mode is swept entirely, scanning range is 45~450amu.
5. the Soxhlet extraction device according to claim 1 using with Solid Phase Extraction function extract in tobacco aromaticss fragrance at
The method divided, which is characterized in that the Soxhlet extraction device with Solid Phase Extraction function includes such as lower component:
Flask (1), flask (1) are equipped with first interface (3), second interface (4) and hickey (2), and flask (1) passes through first
Connection is connected with heat-insulated gas-guide tube (5) air-flow for interface (3), and heat-insulated gas-guide tube (5) other end is connected with threeway transfer tube (7) air-flow
Connection is connected with closed condenser pipe (10) and sample cylinder (8) air-flow respectively in connection, other two interface of threeway transfer tube (7),
Sample cylinder (8) is equipped with sieve plate (12) far from the one end of threeway transfer tube (7) and connection is connected with solid-phase extraction column (9) air-flow, Gu
Connection is connected with second interface (4) air-flow by solvent refluxing pipe (6) for the other end of phase extraction column (9), and solvent refluxing pipe (6) is interior
Equipped with triple valve (13).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910028005.8A CN109781879A (en) | 2019-01-11 | 2019-01-11 | A method of fragrance component in tobacco aromaticss is extracted using the Soxhlet extraction device with Solid Phase Extraction function |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910028005.8A CN109781879A (en) | 2019-01-11 | 2019-01-11 | A method of fragrance component in tobacco aromaticss is extracted using the Soxhlet extraction device with Solid Phase Extraction function |
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| Publication Number | Publication Date |
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| CN109781879A true CN109781879A (en) | 2019-05-21 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910028005.8A Withdrawn CN109781879A (en) | 2019-01-11 | 2019-01-11 | A method of fragrance component in tobacco aromaticss is extracted using the Soxhlet extraction device with Solid Phase Extraction function |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113671089A (en) * | 2021-09-18 | 2021-11-19 | 云南中烟工业有限责任公司 | Tobacco essence extraction, separation and concentration device with sample feeding bottle and method |
| CN113834894A (en) * | 2021-08-30 | 2021-12-24 | 云南中烟工业有限责任公司 | Tobacco essence extraction and separation device with sampler and method |
-
2019
- 2019-01-11 CN CN201910028005.8A patent/CN109781879A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113834894A (en) * | 2021-08-30 | 2021-12-24 | 云南中烟工业有限责任公司 | Tobacco essence extraction and separation device with sampler and method |
| CN113671089A (en) * | 2021-09-18 | 2021-11-19 | 云南中烟工业有限责任公司 | Tobacco essence extraction, separation and concentration device with sample feeding bottle and method |
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Application publication date: 20190521 |