CN102818871B - Interface device and method for on-line coupling of liquid chromatography-gas chromatography/mass spectrum (LC-GC/MS) - Google Patents
Interface device and method for on-line coupling of liquid chromatography-gas chromatography/mass spectrum (LC-GC/MS) Download PDFInfo
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Abstract
The invention provides an interface device for on-line coupling of LC-GC/MS and a method for analyzing fragrant components in tobaccos by utilizing the device. According to the method, reverse blowing gas can be provided through switch of a gas switch valve, during sample injection, the reverse blowing gas is discharged form a GC flow-splitting port against the GC carrier gas direction through a tee coupling, therefore solvents can be transferred out completely, solutes are reserved in a TenaxTA absorbent in a PTV liner tube, thermal desorption is performed on a PTV injection port after the solvents are transferred completely, the GC carrier gas shifts cut fractions to be tested into a GC column for separation, effects on an MS vacuum system due to the fact the solvents enter the GC column are effectively avoided, and large volume injection can be achieved.
Description
Technical field
The present invention relates to a kind of interfacing, particularly relate to a kind of liquid chromatography-gas chromatography/mass spectrometry on-line coupling interface arrangement and adopt the method for aroma component in this device analysis tobacco.
Background technology
In tobacco and spices research, conventional LC(liquid chromatography) pre-separation of fragrance thing is become to multiple cuts, for interesting fragrance cut, adopt GC/MS(gas chromatography/mass spectrometry) further analyze.But, this traditional offline mode, complicated operation, sensitivity is low, poor repeatability, and easily cause the pollution of sample, mainly for separating of identification research, be rarely used in conventional quantitative test, especially trace constituent analysis.LC-GC on-line coupling is highly sensitive, reproducible, pollutes less, and robotization, saves manpower, and efficiency and effect are significantly better than traditional off-line mode.Therefore, LC-GC coupling technique has vital role to the analysis and research of tobacco, the important fragrance matter of flue gas, and interfacing is the key of LC-GC/MS on-line coupling technology, can its effect be interested LC to be flowed out to component proceed to GC, the accuracy of interface to the cutting of LC effluent selectivity and it free of losses is proceeded to GC and determined the quality of its performance.
Propose so far from LC-GC/MS on-line coupling, people have designed various interface, sum up and are divided three classes: interface on the post of employing retention gap technology, the quantity tube interface of employing solvent coevaporation technology, programmed temperature sampling (PTV).On post, interface is in fact a four-way valve, and this interface structure is simple, easy to operate, owing to not being coated with the finite volume of pre-column liquid hold-up of stain, can only shift low dose of cut; Quantitatively cast interface, conventional is six-way valve and ten-way valve, but this Interface design complexity has sample loss, and quantitative result is unreliable; Hot injection port generally adopt temperature programme vaporizer (PTV) or in have the hot vaporizer of packing material, to shift large volume solvent, can successfully be applied to the transfer of bulk sample.But the interfacing of LC-GC/MS coupling is comparatively complicated, the LC mobile phase used from GC is different, gas chromatographic sample introduction amount generally only has 1-2 microlitre, and the flow of LC mobile phase is generally higher than 100 μ l/min, how to remove desolventizing, component to be measured is introduced to GC, carry out the conversion of mobile phase, also there is no ripe interfacing at present.
Summary of the invention
The shortcoming of prior art in view of the above, the object of the present invention is to provide a kind of liquid chromatography-gas chromatography/mass spectrometry on-line coupling interface arrangement and adopt the method for aroma component in this device analysis tobacco, for solve prior art medium sensitivity low, to proceeding to the problem that the quantity of solvent of gas chromatographic sample introduction mouth is restricted, cannot realize large volume sample injection.
For achieving the above object and other relevant objects, liquid chromatography-gas chromatography/mass spectrometry on-line coupling interface arrangement provided by the invention, wherein, liquid chromatographic system comprises LC sampling valve, liquid-phase chromatographic column and UV-detector, gas chromatography system comprises PTV bushing pipe, GC retains pre-column and gas chromatographic column, the upper end of described PTV bushing pipe is provided with PTV injection port, one side of described PTV bushing pipe upper end is provided with GC carrier gas inlet, the lower end of described PTV bushing pipe is connected with the entrance that GC retains pre-column, also comprise LC backwash valve, LC cut cutting valve, three-way connection and the gas transfer valve that can control purge gas break-make,
Described LC sampling valve is a six-way valve, 1. the position of described LC sampling valve is LC injection port, 2. the position of described LC sampling valve and 5. being connected with the two ends of quantitative ring respectively, 4. the position of described LC sampling valve is connected with described solvent bottle by pipeline, pipeline between described LC sampling valve and described solvent bottle is provided with high-pressure pump, and the 6. position of described LC sampling valve is connected with the first waste liquid bottle by pipeline;
Described LC backwash valve is a four-way valve, described LC cut cutting valve is a four-way valve, 3. the position of described LC sampling valve is connected with the 1. position of LC backwash valve by pipeline, 2. the position of described LC backwash valve is connected with the entrance of liquid-phase chromatographic column by pipeline, the outlet of described liquid-phase chromatographic column is connected with the 4. position of LC backwash valve by pipeline, 3. the position of described LC backwash valve is connected with one end of UV-detector by pipeline, the other end of described UV-detector is connected with the 2. position of LC cut cutting valve by pipeline, 3. the position of described LC cut cutting valve is connected with the second waste liquid bottle by pipeline, 4. the position of described LC cut cutting valve is connected with a damper tube by pipeline, 1. the position of described LC cut cutting valve is connected with PTV injection port by kapillary,
One side of described PTV liner at its lower end is provided with GC diffluence pass, first interface of described three-way connection is connected with the outlet that GC retains pre-column, second interface of described three-way connection is connected with the entrance of gas chromatographic column, and the 3rd interface of described three-way connection communicates with purge gas by gas transfer valve.
Preferably, described gas transfer valve is a T-valve, and the 3rd interface of described three-way connection is connected with the 3. position of gas transfer valve, the logical purge gas in 1. position of described gas transfer valve, and the 2. position of described gas transfer valve is blocked.
Preferably, described gas transfer valve is two transfer valves or multiport valve or stop valve.
Preferably, described PTV bushing pipe is filled by glass wool or beaded glass or Tenax TA.
Preferably, described three-way connection material is glass or quartz or metal.
Preferably, described GC reservation pre-column is quartz capillary.
The present invention also provides a kind of method of utilizing above-mentioned liquid chromatography-gas chromatography/mass spectrometry on-line coupling interface arrangement to analyze aroma component in tobacco, and it comprises the following steps:
A. sample carries out pre-treatment by liquid chromatographic system: sample is from LC sampling valve hand sampling, with quantitative ring constant volume, the now 1. position of LC sampling valve and 2. being connected, 3. position and 4. being connected, 5. position and 6. being connected, after sample introduction, rotate LC sampling valve, make the 2. position of LC sampling valve and 3. be connected, 4. position and 5. being connected, 6. position and 1. being connected, now, 1. the position of LC backwash valve and 2. being connected, 3. position and 4. being connected, then the solvent in solvent bottle is sent into the sample in quantitative ring liquid-phase chromatographic column by LC sampling valve through LC backwash valve and is separated through high-pressure pump, after UV-detector detects the cut to be measured in sample, rotate LC cut cutting valve, the 1. position that makes LC cut cutting valve be 2. connected, 3. position and 4. being connected, solvent enters PTV injection port, then enter PTV bushing pipe,
B. shift solvent, retain cut to be measured in PTV bushing pipe: PTV injection port pressure decreased, GC diffluence pass and gas transfer valve are all opened, making pressure retain pre-column higher than the purge gas of PTV injection port pressure through gas transfer valve, three-way connection, GC discharges from GC diffluence pass, purge gas shifts away the solvent vapo(u)r in PTV bushing pipe, and cut to be measured is carried in the adsorbent in PTV bushing pipe;
C. liquid-phase chromatographic column is carried out to backwash, process unnecessary solvent: judge that cut to be measured is transferred to after PTV bushing pipe completely simultaneously, rotate LC backwash valve and LC cut cutting valve, make the 1. position of LC backwash valve and 4. be connected, 2. position and 3. being connected, 1. the position of LC cut cutting valve and 4. being connected, 2. position and 3. being connected, solvent enters from the outlet of liquid-phase chromatographic column, from entrance out, enter LC cut cutting valve through UV-detector again, then enter the second waste liquid bottle, the kapillary of the GC carrier gas entering from GC carrier gas inlet through connecting between PTV injection port and LC cut cutting valve, residual solvent in kapillary is discharged from damper tube,
D. detect cut to be measured: after judging that purge gas shifts solvent completely, gas transfer valve cuts out, described GC diffluence pass is closed, the pressure of PTV injection port raises, and PTV injection port temperature programme, the GC carrier gas entering from GC carrier gas inlet retains pre-column the cut to be measured adsorbing in PTV bushing pipe through GC and proceeds to gas chromatographic column, separates, and then enters mass detector and detects.
Preferably, described gas transfer valve is by the Valve control module control on PerkinElmer Clarus 600T gas chromatography system.
As mentioned above, liquid chromatography-gas chromatography/mass spectrometry on-line coupling interface arrangement of the present invention and utilize the analytical approach of this device, from tobacco sample, can detect several important aroma component, and there are reasonable degree of separation and higher sensitivity, and the quantity of solvent that proceeds to gas chromatographic sample introduction mouth is not limited, can realize large volume sample injection, shorten loaded down with trivial details tediously long sample pretreatment step in early stage, analytical effect and efficiency can be greatly improved.
Brief description of the drawings
Fig. 1 is shown as the schematic diagram of liquid chromatography-gas chromatography/mass spectrometry on-line coupling interface arrangement of the present invention.
Fig. 2 is shown as the schematic diagram of the LC-GC/MS chromatogram of tobacco sample aroma component in the present invention.
Number in the figure explanation
1 LC sampling valve 2 LC backwash valve
3 LC cut cutting valve 4 gas transfer valves
5 solvent bottles 6 quantitatively encircle
7 liquid-phase chromatographic column 8 UV-detector
9 high-pressure pump 10 first waste liquid bottles
11 second waste liquid bottle 12 damper tubes
13 PTV injection port 14 GC carrier gas inlets
15 GC diffluence pass 16 three-way connections
17 GC retain pre-column 18 gas chromatographic columns
19 purge gas
Embodiment
By particular specific embodiment explanation embodiments of the present invention, person skilled in the art scholar can understand other advantages of the present invention and effect easily by the disclosed content of this instructions below.
Refer to Fig. 1 to Fig. 2.Notice, appended graphic the illustrated structure of this instructions, ratio, size etc., all contents in order to coordinate instructions to disclose only, understand and read for person skilled in the art scholar, not in order to limit the enforceable qualifications of the present invention, therefore the not technical essential meaning of tool, the adjustment of the modification of any structure, the change of proportionate relationship or size, not affecting under effect that the present invention can produce and the object that can reach, all should still drop on disclosed technology contents and obtain in the scope that can contain.Simultaneously, in this instructions, quote as " on ", the term of D score, " left side ", " right side ", " centre " and " " etc., also only for ease of understanding of narrating, but not in order to limit the enforceable scope of the present invention, the change of its relativeness or adjustment, changing under technology contents, when being also considered as the enforceable category of the present invention without essence.
As shown in Figure 1, liquid chromatography-gas chromatography/mass spectrometry on-line coupling interface arrangement provided by the invention, wherein, liquid chromatographic system comprises LC sampling valve 1, liquid-phase chromatographic column 7 and UV-detector 8, gas chromatography system comprises PTV bushing pipe, GC retains pre-column 17 and gas chromatographic column 18, the upper end of PTV bushing pipe is provided with PTV injection port 13, one side of PTV bushing pipe upper end is provided with GC carrier gas inlet 14, the lower end of PTV bushing pipe is connected with the entrance that GC retains pre-column 17, also comprise LC backwash valve 2, LC cut cutting valve 3, three-way connection 16 and the gas transfer valve 4 that can control purge gas 19 break-makes,
LC sampling valve 1 is a six-way valve, 1. the position of LC sampling valve 1 is LC injection port, 2. the position of LC sampling valve 1 and 5. being connected with the two ends of quantitative ring 6 respectively, 4. the position of LC sampling valve 1 is connected with solvent bottle 5 by pipeline, pipeline between LC sampling valve 1 and solvent bottle 5 is provided with high-pressure pump 9, and the 6. position of LC sampling valve 1 is connected with the first waste liquid bottle 10 by pipeline;
LC backwash valve 2 is a four-way valve, LC cut cutting valve 3 is a four-way valve, 3. the position of LC sampling valve 1 is connected with the 1. position of LC backwash valve 2 by pipeline, 2. the position of LC backwash valve 2 is connected with the entrance of liquid-phase chromatographic column 7 by pipeline, the outlet of liquid-phase chromatographic column 7 is connected with the 4. position of LC backwash valve 2 by pipeline, 3. the position of LC backwash valve 2 is connected with one end of UV-detector 8 by pipeline, the other end of UV-detector 8 is connected with the 2. position of LC cut cutting valve 3 by pipeline, 3. the position of LC cut cutting valve 3 is connected with the second waste liquid bottle 11 by pipeline, 4. the position of LC cut cutting valve 3 is connected with a damper tube 12 by pipeline, 1. the position of LC cut cutting valve 3 is connected with PTV injection port 13 by kapillary,
One side of PTV liner at its lower end is provided with GC diffluence pass 15, first interface of three-way connection 16 is connected with the outlet that GC retains pre-column 17, second interface of three-way connection 16 is connected with the entrance of gas chromatographic column 18, the 3rd interface of three-way connection 16 communicates with purge gas 19 by gas transfer valve 4, gas transfer valve 4 is a T-valve as shown in Figure 1, the 3rd interface of three-way connection 16 is connected with the 3. position of gas transfer valve 4,1. the logical purge gas 19 in position of gas transfer valve 4, the 2. position of gas transfer valve 4 is blocked.And gas transfer valve 4 also can be two transfer valves or multiport valve or stop valve, as long as can realize the break-make of purge gas.
PTV bushing pipe is filled by glass wool or beaded glass or Tenax TA, or other form bushing pipes also can, three-way connection 16 materials are glass or quartz or metal, it is quartz capillary that GC retains pre-column 17.
The present invention also provides the analytical approach of utilizing said apparatus to analyze aroma component in tobacco, and it comprises the following steps:
A. tobacco sample carries out pre-treatment by liquid chromatographic system: hand sampling, sample enters from the 1. position of LC sampling valve 1, with quantitatively ring 6 constant volumes of 20 μ l, the now 1. position of LC sampling valve and 2. being connected, 3. position and 4. being connected, 5. position and 6. being connected, after sample introduction, rotate LC sampling valve 1, make the 2. position of LC sampling valve 1 and 3. be connected, 4. position and 5. being connected, 6. position and 1. being connected, now, 1. the position of LC backwash valve 2 and 2. being connected, 3. position and 4. being connected, then in solvent bottle 5, the mixed solvent of ether and pentane is sent into liquid-phase chromatographic column 7 by LC sampling valve 1 through LC backwash valve 2 and is separated quantitatively encircling sample in 6 through high-pressure pump 9, after UV-detector 8 detects the cut to be measured in sample, rotate LC cut cutting valve 3, the 1. position that makes LC cut cutting valve 3 be 2. connected, 3. position and 4. being connected, solvent enters PTV injection port 13, then enter PTV bushing pipe,
B. shift solvent, retain cut to be measured in PTV bushing pipe: in the time that solvent enters PTV injection port, PTV injection port 13 pressure decreaseds, reduce to 0.5psi by 15psi, GC diffluence pass 15 is all opened (the 1. position of gas transfer valve 4 and 3. be connected) with gas transfer valve 4, purge gas 19 is provided, purge gas 19 pressure are 15-50psi, flow is 3-10ml/min, , purge gas 19 is through gas transfer valve 4, three-way connection 16, GC retains pre-column 17 and discharges from GC diffluence pass 15 against carrier gas direction, (temperature of PTV injection port is higher than solvent boiling point by the solvent vapo(u)r in PTV bushing pipe for purge gas 19, make liquid solvent vaporization) shift away, and cut to be measured is carried in the adsorbent Tenax TA in PTV bushing pipe, in addition, the GC nebulizer gas pressure pressure lower and purge gas 19 entering from GC carrier gas inlet 14 is higher, has avoided solvent enter mass detector (MS) and vacuum system is impacted so completely,
C. liquid-phase chromatographic column 7 is carried out to backwash, process unnecessary solvent: judge that cut to be measured is transferred to after PTV bushing pipe completely simultaneously, rotate LC backwash valve 2 and LC cut cutting valve 3, make the 1. position of LC backwash valve 2 and 4. position be connected, 2. with 3. be connected, 1. the position of LC cut cutting valve and 4. position be connected, 2. with 3. be connected, thereby solvent enters, from entrance out from the outlet of liquid-phase chromatographic column 7, reach the recoil object of wash-out of liquid-phase chromatographic column 7, to the composition that adsorptive power is stronger is more easily eluted, reduces the pollution to liquid-phase chromatographic column 7; Then solvent enters LC cut cutting valve 3 through UV-detector 8 again, then enter the second waste liquid bottle 11, the kapillary of the GC carrier gas entering from GC carrier gas inlet 14 through connecting between PTV injection port 13 and LC cut cutting valve 3, residual solvent in kapillary is discharged from damper tube 12, to avoid residual and memory effect;
D. detect cut to be measured: after judging that purge gas 19 shifts solvent completely, gas transfer valve 4 cuts out, make its 1. position and 3. position disconnection, close purge gas 19, and GC diffluence pass 15 is closed, the pressure of PTV injection port 13 is increased to 15psi, and the temperature programme of PTV injection port, the GC carrier gas that GC carrier gas inlet 14 enters proceeds to gas chromatographic column 18 the cut to be measured adsorbing in PTV bushing pipe through GC reservation pre-column 17 and separates, and then enters mass detector (MS) and detects.
From above analytical approach of the present invention, due to before cut to be measured enters gas chromatographic column, solvent is transferred away, so use the analytical approach of the present invention's design, the quantity of solvent that proceeds to gas chromatographic sample introduction mouth is not limited, can realize large volume sample injection, shorten loaded down with trivial details tediously long sample pretreatment step in early stage, analytical effect and efficiency can be greatly improved.
In above analytical approach, gas transfer valve 4, by the Valve control module control in PerkinElmer Clarus 600T gas chromatography, only has two patterns of ON/OFF.In tobacco sample, the LC-GC/MS testing result of aroma component as shown in Figure 2 and Table 1, therefrom can find out, through simple sample pre-treatments, use liquid chromatography-gas chromatography/mass spectrometry on-line coupling interface arrangement and the analytical approach of the present invention's design, from tobacco sample, can detect several important aroma component, and there are reasonable degree of separation and higher sensitivity, what illustrate that liquid chromatography-gas chromatography/mass spectrometry on-line coupling interface arrangement of design and installation of the present invention can be accurately and in Fast Measurement tobacco importantly causes fragrant composition, also can be used for the analyzing and testing of trace constituent in other complex system.
Aroma component LC-GC/MS testing result in table 1 tobacco leaf
| Retention time | Title | Molecular weight |
| 26.33 | Phenethyl acetate | 164 |
| 29.27 | Solanone | 194 |
| 29.83 | Damascenone | 190 |
| 30.62 | Damascone | 192 |
| 31.64 | Geranyl acetone | 194 |
| 32.45 | Irisone | 192 |
| 32.53 | Jonone by oxidizing | 208 |
| 33.69 | Dihydroactinidiolide | 180 |
| 34.44 | Megastigmatrienone A | 190 |
| 34.90 | Megastigmatrienone B | 190 |
| 35.67 | Megastigmatrienone C | 190 |
| 36.00 | Megastigmatrienone D | 190 |
| 40.89 | Six hydrogen method ketone | 268 |
| 42.31 | Method ketone | 262 |
The result of Fig. 2 and table 1 is gain of parameter based on following:
Sample pre-treatments: 0.2g offal (Hunan Flue-cured Tobacco), add 5ml normal hexane to extract solvent and 100 μ l acetic acid benzene ester inner mark solution (0.024mg/ml), ultrasonic extraction 2-3min, 3000 leave heart 10min, get 1-2 milliliter supernatant to chromatographic sample bottle.
Liquid phase chromatogram condition
Liquid-phase chromatographic column: silicagel column (5 μ m particle diameters, 2.2x 150mm); Liquid chromatography pump (LC-20AD, SHIMADZU); UV-detector wavelength 252nm; Mobile phase: ether and pentane mixed liquor (1:1), flow velocity 0.15ml/min, clipping time 6min, hand sampling valve, sample size 50 μ l, quantitatively encircle 20 μ l.
Gas chromatography-mass spectrum condition
PTV injection port: Tenax TA bushing pipe, solvent emptying pattern, 50 ° of C of initial temperature, keep 6.5min, purge time 3min, 300 ° of C of desorption temperature, purge flow velocity 50ml/min; Chromatographic column: DB-5MS (30m × 0.25mmI.D, thickness 0.25 μ is m); Carrier gas: helium, column head pressure 15psi; Furnace temperature case: 40 ° of C keep 11 minutes, is warming up to 230 ° of C with 8 ° of C/min and keeps 20min; Mass spectrometer ionization pattern: EI, electron energy 70eV, 180 ° of C of ion source temperature, sweep limit 33-350amu.
In sum, liquid chromatography-gas chromatography/mass spectrometry on-line coupling interface arrangement of the present invention design and utilize the analytical approach of this device, from tobacco sample, can detect several important aroma component, and there are reasonable degree of separation and higher sensitivity, and the quantity of solvent that proceeds to gas chromatographic sample introduction mouth is not limited, can realize large volume sample injection, shorten loaded down with trivial details tediously long sample pretreatment step in early stage, analytical effect and efficiency can be greatly improved.So the present invention has effectively overcome various shortcoming of the prior art and tool high industrial utilization.
Above-described embodiment is illustrative principle of the present invention and effect thereof only, but not for limiting the present invention.Any person skilled in the art scholar all can, under spirit of the present invention and category, modify or change above-described embodiment.Therefore, such as in affiliated technical field, have and conventionally know that the knowledgeable, not departing from all equivalence modifications that complete under disclosed spirit and technological thought or changing, must be contained by claim of the present invention.
Claims (7)
1. liquid chromatography-gas chromatography/mass spectrometry on-line coupling interface arrangement, wherein, liquid chromatographic system comprises LC sampling valve (1), liquid-phase chromatographic column (7) and UV-detector (8), gas chromatography system comprises PTV bushing pipe, GC retains pre-column (17) and gas chromatographic column (18), the upper end of described PTV bushing pipe is provided with PTV injection port (13), one side of described PTV bushing pipe upper end is provided with GC carrier gas inlet (14), the lower end of described PTV bushing pipe is connected with the entrance that GC retains pre-column (17), it is characterized in that, also comprise LC backwash valve (2), LC cut cutting valve (3), three-way connection (16) and can control the gas transfer valve (4) of purge gas (19) break-make,
Described LC sampling valve (1) is a six-way valve, 1. the position of described LC sampling valve (1) is LC injection port, 2. the position of described LC sampling valve (1) and 5. being connected with the two ends of quantitative ring (6) respectively, 4. the position of described LC sampling valve (1) is connected with solvent bottle (5) by pipeline, pipeline between described LC sampling valve (1) and described solvent bottle (5) is provided with high-pressure pump (9), and the 6. position of described LC sampling valve (1) is connected with the first waste liquid bottle (10) by pipeline;
Described LC backwash valve (2) is a four-way valve, described LC cut cutting valve (3) is a four-way valve, 3. the position of described LC sampling valve (1) is connected with the 1. position of LC backwash valve (2) by pipeline, 2. the position of described LC backwash valve (2) is connected with the entrance of liquid-phase chromatographic column (7) by pipeline, the outlet of described liquid-phase chromatographic column (7) is connected with the 4. position of LC backwash valve (2) by pipeline, 3. the position of described LC backwash valve (2) is connected with one end of UV-detector (8) by pipeline, the other end of described UV-detector (8) is connected with the 2. position of LC cut cutting valve (3) by pipeline, 3. the position of described LC cut cutting valve (3) is connected with the second waste liquid bottle (11) by pipeline, 4. the position of described LC cut cutting valve (3) is connected with a damper tube (12) by pipeline, 1. the position of described LC cut cutting valve (3) is connected with PTV injection port (13) by kapillary,
One side of described PTV liner at its lower end is provided with GC diffluence pass (15), first interface of described three-way connection (16) is connected with the outlet that GC retains pre-column (17), second interface of described three-way connection (16) is connected with the entrance of gas chromatographic column (18), and the 3rd interface of described three-way connection (16) communicates with purge gas (19) by gas transfer valve (4); Described PTV bushing pipe is filled by glass wool or beaded glass or Tenax TA.
2. liquid chromatography-gas chromatography/mass spectrometry on-line coupling interface arrangement according to claim 1, it is characterized in that, described gas transfer valve (4) is a T-valve, the 3rd interface of described three-way connection (16) is connected with the 3. position of gas transfer valve (4), 1. the logical purge gas in position (19) of described gas transfer valve (4), the 2. position of described gas transfer valve is blocked.
3. liquid chromatography-gas chromatography/mass spectrometry on-line coupling interface arrangement according to claim 1, is characterized in that, described gas transfer valve (4) is two transfer valves or multiport valve or stop valve.
4. liquid chromatography-gas chromatography/mass spectrometry on-line coupling interface arrangement according to claim 1, is characterized in that, the material of described three-way connection (16) is glass or quartz or metal.
5. liquid chromatography-gas chromatography/mass spectrometry on-line coupling interface arrangement according to claim 1, is characterized in that, it is quartz capillary that described GC retains pre-column (17).
6. utilize liquid chromatography-gas chromatography/mass spectrometry on-line coupling interface arrangement described in claim 1 to analyze a method for aroma component in tobacco, it is characterized in that, comprise the following steps:
A. sample carries out pre-treatment by liquid chromatographic system: sample is from LC sampling valve (1) hand sampling, with quantitative ring (6) constant volume, the now 1. position of LC sampling valve and 2. being connected, 3. position and 4. being connected, 5. position and 6. being connected, after sample introduction, rotate LC sampling valve (1), make the 2. position of LC sampling valve (1) and 3. be connected, 4. position and 5. being connected, 6. position and 1. being connected, now, 1. the position of LC backwash valve (2) and 2. being connected, 3. position and 4. being connected, then the solvent in solvent bottle (5) is sent into liquid-phase chromatographic column (7) by LC sampling valve (1) through LC backwash valve (2) and is separated quantitatively encircling sample in (6) through high-pressure pump (9), after UV-detector (8) detects the cut to be measured in sample, rotate LC cut cutting valve (3), the 1. position that makes LC cut cutting valve (3) be 2. connected, 3. position and 4. being connected, solvent enters PTV injection port (13), then enter PTV bushing pipe,
B. shift solvent, retain cut to be measured in PTV bushing pipe: PTV injection port (13) pressure decreased, GC diffluence pass (15) and gas transfer valve (4) are all opened, making pressure retain pre-column (17) higher than the purge gas (19) of PTV injection port pressure through gas transfer valve (4), three-way connection (16), GC discharges from GC diffluence pass (15), purge gas (19) shifts away the solvent vapo(u)r in PTV bushing pipe, and cut to be measured is carried in the adsorbent in PTV bushing pipe;
C. liquid-phase chromatographic column (7) is carried out to backwash, process unnecessary solvent: judge that cut to be measured is transferred to after PTV bushing pipe completely simultaneously, rotate LC backwash valve (2) and LC cut cutting valve (3), make the 1. position of LC backwash valve (2) and 4. be connected, 2. position and 3. being connected, 1. the position of LC cut cutting valve and 4. being connected, 2. position and 3. being connected, solvent enters from the outlet of liquid-phase chromatographic column (7), from entrance out, enter LC cut cutting valve (3) through UV-detector (8) again, then enter the second waste liquid bottle (11), the kapillary of the GC carrier gas entering from GC carrier gas inlet (14) through connecting between PTV injection port (13) and LC cut cutting valve (3), residual solvent in kapillary is discharged from damper tube (12),
D. detect cut to be measured: after judging that purge gas (19) shifts solvent completely, gas transfer valve (4) cuts out, described GC diffluence pass (15) is closed, the pressure of PTV injection port (13) raises, and PTV injection port temperature programme, the GC carrier gas entering from GC carrier gas inlet (14) retains pre-column (17) the cut to be measured adsorbing in PTV bushing pipe through GC and proceeds to gas chromatographic column (18), separate, then enter mass detector and detect.
7. the method for aroma component in analysis tobacco according to claim 6, is characterized in that, described gas transfer valve is by the Valve control module control on PerkinElmer Clarus600T gas chromatography system.
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