CN102818871A - 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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- CN102818871A CN102818871A CN2012101716486A CN201210171648A CN102818871A CN 102818871 A CN102818871 A CN 102818871A CN 2012101716486 A CN2012101716486 A CN 2012101716486A CN 201210171648 A CN201210171648 A CN 201210171648A CN 102818871 A CN102818871 A CN 102818871A
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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, LC (liquid chromatography) commonly used becomes a plurality of cuts to the pre-separation of fragrance thing, for interesting fragrance cut, adopts GC/MS (gas chromatography/mass spectrometry) further to analyze.But, this traditional offline mode, complicated operation, sensitivity is low, poor repeatability, and cause the pollution of sample easily, and be mainly used in isolation identification research, seldom be used for conventional quantitative test, especially trace constituent analysis.The LC-GC on-line coupling is highly sensitive, and good reproducibility pollutes and lacks, and manpower is saved in robotization, and efficient and effect significantly are superior to traditional off-line mode.Therefore; The 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; Its effect is interested LC to be flowed out component change GC over to, interface to the accuracy of LC effluent selectivity cutting with can change it free of losses over to quality that GC has determined its performance.
Propose so far from the LC-GC/MS on-line coupling, people have designed various interface, summarize to get up to be divided three classes: adopt interface on the technological post of retention gap, adopt the quantity tube interface of solvent coevaporation technology, programmed temperature sampling (PTV).Interface comes down to a four-way valve on the post, and this interface structure is simple, easy to operate, owing to be not coated with the finite volume of the pre-column liquid hold-up of stain, can only shift low dose of cut; Quantitative cast interface, commonly used is six-way valve and ten-way valve, but this Interface design is complicated, and sample loss is arranged, and quantitative result is unreliable; Hot injection port generally adopt temperature programme vaporizer (PTV) or in the hot vaporizer of packing material is arranged so that shift big volume of solvent, can successfully be applied to the transfer of bulk sample.But the interfacing of LC-GC/MS coupling is comparatively complicated; The used moving phase of LC and GC is different, and the gas chromatography sample size generally has only the 1-2 microlitre, and the flow of LC moving phase generally is higher than 100 μ l/min; How to remove and desolvate; Component to be measured is introduced GC, promptly carry out the conversion of moving phase, also do not have 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, be used to solve prior art medium sensitivity low, the quantity of solvent that changes the gas chromatography injection port over to is had restriction, can't realize the problem of large volume sample injection.
For realizing above-mentioned purpose and other relevant purposes; Liquid chromatography provided by the invention-gas chromatography/mass spectrometry on-line coupling interface arrangement; Wherein, liquid chromatographic system comprises LC sampling valve, liquid-phase chromatographic column and UV-detector, and gas chromatography system comprises that PTV bushing pipe, GC keep pre-column and gas chromatographic column; The upper end of said PTV bushing pipe is provided with the PTV injection port; One side of said PTV bushing pipe upper end is provided with the GC carrier gas inlet, and the lower end of said PTV bushing pipe links to each other with the inlet that GC keeps pre-column, also comprises the gas transfer valve of LC backwash valve, the cutting of LC cut valve, three-way connection and may command purge gas break-make;
Said LC sampling valve is a six-way valve; 1. the position of said LC sampling valve is the LC injection port; 2. the position of said LC sampling valve with 5. link to each other with the two ends of quantifying ring respectively; 4. the position of said LC sampling valve links to each other with said solvent bottle through pipeline, and the pipeline between said LC sampling valve and the said solvent bottle is provided with high-pressure pump, and the 6. position of said LC sampling valve links to each other with first waste liquid bottle through pipeline;
Said LC backwash valve is a four-way valve; Said LC cut cutting valve is a four-way valve; 3. the position of said LC sampling valve links to each other with the 1. position of LC backwash valve through pipeline; 2. the position of said LC backwash valve links to each other with the inlet of liquid-phase chromatographic column through pipeline, and the outlet of said liquid-phase chromatographic column links to each other with the 4. position of LC backwash valve through pipeline, and the 3. position of said LC backwash valve links to each other with an end of UV-detector through pipeline; The other end of said UV-detector links to each other through the 2. position of pipeline with LC cut cutting valve; 3. the position of said LC cut cutting valve links to each other with second waste liquid bottle through pipeline, and the 4. position of said LC cut cutting valve links to each other with a damper tube through pipeline, and the 1. position of said LC cut cutting valve links to each other with the PTV injection port through kapillary;
One side of said PTV liner at its lower end is provided with the GC diffluence pass; First interface of said three-way connection links to each other with the outlet that GC keeps pre-column; Second interface of said three-way connection links to each other with the inlet of gas chromatographic column, and the 3rd interface of said three-way connection communicates with purge gas through the gas transfer valve.
Preferably, said gas transfer valve is a T-valve, and the 3rd interface of said three-way connection links to each other with the 3. position of gas transfer valve, the logical purge gas in 1. position of said gas transfer valve, and the 2. position of said gas transfer valve is blocked.
Preferably, said gas transfer valve is two transfer valves or multiport valve or stop valve.
Preferably, said PTV bushing pipe is by glass wool or beaded glass or Tenax TA filling.
Preferably, said three-way connection material is glass or quartz or metal.
Preferably, said GC reservation pre-column is a 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 the tobacco, and it may further comprise the steps:
A. sample carries out pre-treatment through liquid chromatographic system: sample is used the quantifying ring constant volume from LC sampling valve hand sampling, this moment the 1. position of LC sampling valve link to each other with 2. position, 3. the position link to each other with 4. position, 5. with 6. link to each other; After sample introduction finishes, rotate the LC sampling valve, make the 2. position of LC sampling valve link to each other with 3. position, 4. the position link to each other with 5. position, 6. with 1. link to each other; At this moment; 1. the position of LC backwash valve links to each other with 2. position, 3. with 4. link to each other, the solvent in the solvent bottle is sent into liquid-phase chromatographic column by the LC sampling valve through the LC backwash valve with the sample in the quantifying ring through high-pressure pump and is separated then, after UV-detector detects the cut to be measured in the sample; Rotate LC cut cutting valve; Make LC cut cutting valve 1. position with 2. link to each other, 3. the position with 4. link to each other, solvent entering PTV injection port gets into the PTV bushing pipe then;
B. shift solvent; Keep cut to be measured in the PTV bushing pipe: PTV injection port pressure reduces; GC diffluence pass and gas transfer valve are all opened; The purge gas that makes pressure be higher than PTV injection port pressure keeps pre-column through gas transfer valve, three-way connection, GC discharges from the GC diffluence pass, and purge gas shifts away the solvent vapo(u)r in the PTV bushing pipe, and cut to be measured is carried in the adsorbent in the PTV bushing pipe;
C. liquid-phase chromatographic column is carried out backwash; Handle unnecessary solvent simultaneously: after judging that cut to be measured is transferred to the PTV bushing pipe fully, rotate LC backwash valve and LC cut cutting valve, make the 1. position of LC backwash valve link to each other with 4. position, 2. with 3. link to each other; 1. the position of LC cut cutting valve links to each other with 4. position, 2. with 3. link to each other; Solvent gets into, comes out from inlet from the outlet of liquid-phase chromatographic column, gets into LC cut cutting valve through UV-detector again, gets into second waste liquid bottle then; From the kapillary of GC carrier gas that the GC carrier gas inlet gets into, the residual solvent in the kapillary is discharged from damper tube through connecting between PTV injection port and the LC cut cutting valve;
D. detect cut to be measured: after judging that purge gas shifts solvent fully; The gas transfer valve cuts out, and said GC diffluence pass is closed, and the pressure of PTV injection port raises; And PTV injection port temperature programme; The GC carrier gas that gets into from the GC carrier gas inlet changes the cut to be measured that adsorbs in the PTV bushing pipe over to gas chromatographic column through GC reservation pre-column, separates, and gets into mass detector then and detects.
Preferably, said gas transfer valve is controlled by the Valve control module on the PerkinElmer Clarus 600T gas chromatography system.
As stated; Liquid chromatography of the present invention-gas chromatography/mass spectrometry on-line coupling interface arrangement and utilize the analytical approach of this device can detect the several important aroma component, and reasonable degree of separation and higher sensitivity are arranged from tobacco sample; And to the not restriction of quantity of solvent that changes the gas chromatography injection port over to; Can realize large volume sample injection, shorten loaded down with trivial details tediously long sample pretreatment step in early stage, analytical effect and efficient can both be greatly improved.
Description of drawings
Fig. 1 is shown as the synoptic diagram of liquid chromatography of the present invention-gas chromatography/mass spectrometry on-line coupling interface arrangement.
Fig. 2 is shown as the synoptic diagram of the LC-GC/MS chromatogram of tobacco sample aroma component among the present invention.
Label declaration among the figure
1 LC sampling valve, 2 LC backwash valve
3 LC cuts cutting valve, 4 gas transfer valves
5 solvent bottles, 6 quantifying ring
7 liquid-phase chromatographic columns, 8 UV-detectors
9 high-pressure pumps, 10 first waste liquid bottles
11 second waste liquid bottles, 12 damper tubes
13 PTV injection ports, 14 GC carrier gas inlets
15 GC diffluence pass, 16 three-way connections
17 GC keep pre-column 18 gas chromatographic columns
19 purge gas
Embodiment
Below by particular specific embodiment embodiment of the present invention is described, be familiar with this technological personage and can understand other advantages of the present invention and effect easily by the content that this instructions disclosed.
See also Fig. 1 to Fig. 2.Notice; The appended graphic structure that illustrates of this instructions, ratio, size etc.; All only in order to cooperate the content that instructions disclosed, understanding and reading for being familiar with this technological personage, is not in order to limit the enforceable qualifications of the present invention; Event is the technical essential meaning of tool not; The adjustment of the modification of any structure, the change of proportionate relationship or size not influencing under effect that the present invention can produce and the purpose that can reach, all should still drop on disclosed technology contents and get in the scope that can contain.Simultaneously; Quoted in this instructions as " on ", D score, " left side ", " right side ", " centre " reach the term of " " etc.; Also be merely be convenient to narrate clear, but not in order to limit the enforceable scope of the present invention, the change of its relativeness or adjustment; Under no essence change technology contents, when also being regarded as the enforceable category of the present invention.
As shown in Figure 1; Liquid chromatography provided by the invention-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, and gas chromatography system comprises that PTV bushing pipe, GC keep 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, and the lower end of PTV bushing pipe links to each other with the inlet that GC keeps pre-column 17, also comprises the gas transfer valve 4 of LC backwash valve 2, the cutting of LC cut valve 3, three-way connection 16 and may command purge gas 19 break-makes;
One side of PTV liner at its lower end is provided with GC diffluence pass 15; First interface of three-way connection 16 links to each other with the outlet that GC keeps pre-column 17; Second interface of three-way connection 16 links to each other with the inlet of gas chromatographic column 18; The 3rd interface of three-way connection 16 communicates with purge gas 19 through gas transfer valve 4, and gas transfer valve 4 as shown in Figure 1 is a T-valve, and the 3rd interface of three-way connection 16 links to each other 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.
The 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 keeps pre-column 17.
The present invention also provides the analytical approach of utilizing said apparatus to analyze aroma component in the tobacco, and it may further comprise the steps:
A. tobacco sample carries out pre-treatment through liquid chromatographic system: hand sampling, and sample gets into from the 1. position of LC sampling valve 1, with 20 μ l quantifying ring, 6 constant volumes; This moment the 1. position of LC sampling valve link to each other with 2. position, 3. the position link to each other with 4. position, 5. with 6. link to each other; After sample introduction finishes, rotate LC sampling valve 1, make the 2. position of LC sampling valve 1 link to each other with 3. position, 4. the position link to each other with 5. position, 6. with 1. link to each other; At this moment; 1. the position of LC backwash valve 2 links to each other with 2. position, 3. with 4. link to each other, ether is sent into liquid-phase chromatographic column 7 by LC sampling valve 1 through LC backwash valve 2 with the sample in the quantifying ring 6 through high-pressure pump 9 with the mixed solvent of pentane and is separated in the solvent bottle 5 then, after UV-detector 8 detects the cut to be measured in the sample; Rotate LC cut cutting valve 3; Make LC cut cutting valve 3 1. position with 2. link to each other, 3. the position with 4. link to each other, solvent entering PTV injection port 13 gets into the PTV bushing pipe then;
B. shift solvent, keep cut to be measured in the PTV bushing pipe: when solvent got into the PTV injection port, PTV injection port 13 pressure reduced; Reduce to 0.5psi by 15psi; GC diffluence pass 15 is all opened (the 1. position of gas transfer valve 4 with 3. link to each other) with gas transfer valve 4, purge gas 19 is provided, and purge gas 19 pressure are 15-50psi; Flow is 3-10ml/min;, purge gas 19 keeps pre-column 17 through gas transfer valve 4, three-way connection 16, GC discharges from GC diffluence pass 15 against the carrier gas direction, and (temperature of PTV injection port is higher than solvent boiling point to purge gas 19 with the solvent vapo(u)r in the PTV bushing pipe; Make liquid solvent vaporize) shift away, and cut to be measured is carried among the adsorbent Tenax TA in the PTV bushing pipe; In addition, the GC nebulizer gas pressure that gets into from GC carrier gas inlet 14 is lower and pressure purge gas 19 is higher, has avoided solvent to get into mass detector (MS) so fully and vacuum system is impacted;
C. liquid-phase chromatographic column 7 is carried out backwash; Handle unnecessary solvent simultaneously: after judging that cut to be measured is transferred to the PTV bushing pipe fully; Rotate LC backwash valve 2 and LC cut cutting valve 3, make the 1. position of LC backwash valve 2 link to each other, 2. the position links to each other with 3. position with 4. position, the 1. position of LC cut cutting valve with 4. link to each other, 2. with 3. link to each other; Thereby solvent gets into, comes out from inlet from the outlet of liquid-phase chromatographic column 7; Reach liquid-phase chromatographic column 7 purpose of wash-out that recoils,, reduce pollution liquid-phase chromatographic column 7 so that the stronger composition of adsorptive power is eluted more easily; Solvent gets into LC cut cutting valve 3 through UV-detector 8 more then; Get into second waste liquid bottle 11 then; Cut the kapillary that connects between the valve 3 from the GC carrier gas that GC carrier gas inlet 14 gets into through PTV injection port 13 and LC cut; Residual solvent in the 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 fully, gas transfer valve 4 cuts out, and makes it 1. break off with 3. position the position; Promptly close purge gas 19; And GC diffluence pass 15 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 gets into changes the cut to be measured that adsorbs in the PTV bushing pipe over to gas chromatographic column 18 through GC reservation pre-column 17 and separates, and gets into mass detector (MS) then and detects.
Can know by above analytical approach of the present invention; Because cut to be measured gets into before the gas chromatographic column, solvent is transferred away, so utilization analysis of design method of the present invention; To the not restriction of quantity of solvent that changes the gas chromatography injection port over to; Can realize large volume sample injection, shorten loaded down with trivial details tediously long sample pretreatment step in early stage, analytical effect and efficient can both be greatly improved.
In the above analytical approach, gas transfer valve 4 only has two patterns of ON/OFF by the control of the Valve control module on the PerkinElmer Clarus 600T gas chromatography.The LC-GC/MS testing result of aroma component is shown in Fig. 2 and table 1 in the tobacco sample; Therefrom can find out; Through simple sample pre-treatments; Liquid chromatography-gas chromatography/mass spectrometry on-line coupling the interface arrangement and the analytical approach of utilization the present invention design can detect the several important aroma component, and reasonable degree of separation and higher sensitivity are arranged from tobacco sample; Explain the liquid chromatography-gas chromatography/mass spectrometry on-line coupling interface arrangement of design and installation of the present invention can be accurately and important in the fast measuring tobacco cause 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 based on following parameter acquisition:
Sample pre-treatments: 0.2g offal (Hunan flue-cured tobacco), add 5ml normal hexane extraction solvent and 100 μ l acetate benzene ester inner mark solution (0.024mg/ml), ultrasonic extraction 2-3min, 3000 leave heart 10min, get 1-2 milliliter supernatant to the 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; Moving phase: ether and pentane mixed liquor (1:1), flow velocity 0.15ml/min, clipping time 6min, hand sampling valve, sample size 50 μ l, quantifying ring 20 μ l.
The gas chromatography-mass spectrum condition
The 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 m); Carrier gas: helium, column head pressure 15psi; The furnace temperature case: 40 ° of C kept 11 minutes, were warming up to 230 ° of C with 8 ° of C/min and kept 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 the interface arrangement of the present invention design and utilize the analytical approach of this device can detect the several important aroma component, and reasonable degree of separation and higher sensitivity are arranged from tobacco sample; And to the not restriction of quantity of solvent that changes the gas chromatography injection port over to; Can realize large volume sample injection, shorten loaded down with trivial details tediously long sample pretreatment step in early stage, analytical effect and efficient can both be greatly improved.So the present invention has effectively overcome various shortcoming of the prior art and the tool high industrial utilization.
The foregoing description is illustrative principle of the present invention and effect thereof only, but not is used to limit the present invention.Any be familiar with this technological personage all can be under spirit of the present invention and category, the foregoing description is modified or is changed.Therefore, have common knowledge the knowledgeable in the affiliated such as technical field, must contain by claim of the present invention not breaking away from all equivalence modifications of being accomplished under disclosed spirit and the technological thought or changing.
Claims (8)
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 that PTV bushing pipe, GC keep pre-column (17) and gas chromatographic column (18); The upper end of said PTV bushing pipe is provided with PTV injection port (13), and a side of said PTV bushing pipe upper end is provided with GC carrier gas inlet (14), and the lower end of said PTV bushing pipe links to each other with the inlet that GC keeps pre-column (17); It is characterized in that, also comprise the gas transfer valve (4) of LC backwash valve (2), the cutting of LC cut valve (3), three-way connection (16) and may command purge gas (19) break-make;
Said LC sampling valve (1) is a six-way valve; 1. the position of said LC sampling valve (1) is the LC injection port; 2. the position of said LC sampling valve (1) with 5. link to each other with the two ends of quantifying ring (6) respectively; 4. the position of said LC sampling valve (1) links to each other with said solvent bottle (5) through pipeline, and the pipeline between said LC sampling valve (1) and the said solvent bottle (5) is provided with high-pressure pump (9), and the 6. position of said LC sampling valve (1) links to each other with first waste liquid bottle (10) through pipeline; Said LC backwash valve (2) is a four-way valve; Said LC cut cutting valve (3) is a four-way valve; 3. the position of said LC sampling valve (1) links to each other with the 1. position of LC backwash valve (2) through pipeline; 2. the position of said LC backwash valve (2) links to each other with the inlet of liquid-phase chromatographic column (7) through pipeline; The outlet of said liquid-phase chromatographic column (7) links to each other with the 4. position of LC backwash valve (2) through pipeline; 3. the position of said LC backwash valve (2) links to each other with an end of UV-detector (8) through pipeline, and the other end of said UV-detector (8) links to each other with the 2. position of LC cut cutting valve (3) through pipeline, and the 3. position of said LC cut cutting valve (3) links to each other with second waste liquid bottle (11) through pipeline; 4. the position of said LC cut cutting valve (3) links to each other with a damper tube (12) through pipeline, and the 1. position of said LC cut cutting valve (3) links to each other with PTV injection port (13) through kapillary;
One side of said PTV liner at its lower end is provided with GC diffluence pass (15); First interface of said three-way connection (16) links to each other with the outlet that GC keeps pre-column (17); Second interface of said three-way connection (16) links to each other with the inlet of gas chromatographic column (18), and the 3rd interface of said three-way connection (16) communicates with purge gas (19) through gas transfer valve (4).
2. liquid chromatography according to claim 1-gas chromatography/mass spectrometry on-line coupling interface arrangement; It is characterized in that; Said gas transfer valve (4) is a T-valve; The 3rd interface of said three-way connection (16) links to each other with the 3. position of gas transfer valve (4), the 1. position logical purge gas (19) of said gas transfer valve (4), and the 2. position of said gas transfer valve is blocked.
3. liquid chromatography according to claim 1-gas chromatography/mass spectrometry on-line coupling interface arrangement is characterized in that, said gas transfer valve (4) is two transfer valves or multiport valve or stop valve.
4. liquid chromatography according to claim 1-gas chromatography/mass spectrometry on-line coupling interface arrangement is characterized in that, said PTV bushing pipe is by glass wool or beaded glass or Tenax TA filling.
5. liquid chromatography according to claim 1-gas chromatography/mass spectrometry on-line coupling interface arrangement is characterized in that, said three-way connection (16) material is glass or quartz or metal.
6. liquid chromatography according to claim 1-gas chromatography/mass spectrometry on-line coupling interface arrangement is characterized in that, it is quartz capillary that said GC keeps pre-column (17).
7. a method of utilizing the described liquid chromatography of claim 1-gas chromatography/mass spectrometry on-line coupling interface arrangement to analyze aroma component in the tobacco is characterized in that, may further comprise the steps:
A. sample carries out pre-treatment through liquid chromatographic system: sample is from LC sampling valve (1) hand sampling; With quantifying ring (6) constant volume, this moment the 1. position of LC sampling valve link to each other with 2. position, 3. the position link to each other with 4. position, 5. with 6. link to each other, after sample introduction finishes; Rotate LC sampling valve (1); Make the 2. position of LC sampling valve (1) link to each other with 3. position, 4. the position links to each other with 5. position, 6. the position links to each other with 1. position, at this moment, LC backwash valve (2) 1. with 2. link to each other, 3. with 4. link to each other; Solvent in the solvent bottle (5) is sent into liquid-phase chromatographic column (7) by LC sampling valve (1) through LC backwash valve (2) with the sample in the quantifying ring (6) through high-pressure pump (9) and is separated then; After UV-detector (8) detects the cut to be measured in the sample, rotate LC cut cutting valve (3), make LC cut cutting valve (3) 1. position with 2. link to each other, 3. with 4. link to each other; Solvent gets into PTV injection port (13), gets into the PTV bushing pipe then;
B. shift solvent; Keep cut to be measured in the PTV bushing pipe: PTV injection port (13) pressure reduces; GC diffluence pass (15) and gas transfer valve (4) are all opened; Make pressure be higher than the purge gas of PTV injection port pressure (19) and keep pre-column (17) from GC diffluence pass (15) discharge through gas transfer valve (4), three-way connection (16), GC, purge gas (19) shifts away the solvent vapo(u)r in the PTV bushing pipe, and cut to be measured is carried in the adsorbent in the PTV bushing pipe;
C. liquid-phase chromatographic column (7) is carried out backwash; Handle unnecessary solvent simultaneously: after judging that cut to be measured is transferred to the PTV bushing pipe fully; Rotate LC backwash valve (2) and LC cut cutting valve (3); Make the 1. position of LC backwash valve (2) link to each other with 4. position, 2. the position links to each other with 3. position, the 1. position of LC cut cutting valve links to each other with 4. position, 2. with 3. link to each other, solvent is from the outlet entering of liquid-phase chromatographic column (7), from entering the mouth; Get into LC cut cutting valve (3) through UV-detector (8) again; Get into second waste liquid bottle (11) then,, the residual solvent in the kapillary is discharged from damper tube (12) from the kapillary of GC carrier gas that GC carrier gas inlet (14) gets into through connecting between PTV injection port (13) and the LC cut cutting valve (3);
D. detect cut to be measured: after judging that purge gas (19) shifts solvent fully; Gas transfer valve (4) cuts out, and said GC diffluence pass (15) is closed, and the pressure of PTV injection port (13) raises; And PTV injection port temperature programme; The GC carrier gas that gets into from GC carrier gas inlet (14) keeps pre-column (17) to the cut to be measured that adsorbs in the PTV bushing pipe through GC and changes gas chromatographic column (18) over to, separates, and gets into mass detector then and detects.
8. the method for aroma component is characterized in that said gas transfer valve is controlled by the Valve control module on the PerkinElmer Clarus 600 T gas chromatography systems in the analysis tobacco according to claim 7.
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103278589A (en) * | 2013-05-03 | 2013-09-04 | 云南烟草科学研究院 | Detection method and device for volatile and semi-volatile components |
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| CN104133031A (en) * | 2014-07-31 | 2014-11-05 | 云南中烟工业有限责任公司 | Method and device for determination of cigarette smoke benzo[alpha]pyrene by on-line solid phase extraction |
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| CN105372365A (en) * | 2015-10-30 | 2016-03-02 | 中国烟草总公司郑州烟草研究院 | Method for online detection of ethylene oxide and propylene oxide in smoke of cigarettes |
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| CN112595789A (en) * | 2020-12-17 | 2021-04-02 | 广州禾信仪器股份有限公司 | Multifunctional gas chromatography-mass spectrometry device and analysis method |
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| CN117517696A (en) * | 2023-12-29 | 2024-02-06 | 杭州谱聚医疗科技有限公司 | System and sampling method for obtaining samples in situ on line |
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| WO2014127602A1 (en) * | 2013-02-20 | 2014-08-28 | 上海烟草集团有限责任公司 | Gas chromatography/mass spectrometry large-volume sample introduction device system and analysis method thereof |
| CN103278589A (en) * | 2013-05-03 | 2013-09-04 | 云南烟草科学研究院 | Detection method and device for volatile and semi-volatile components |
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| CN105445406B (en) * | 2015-12-14 | 2018-03-09 | 云南中烟工业有限责任公司 | A kind of liquid phase gas phase Two way chromatograms analytical equipment and analysis method for being used to determine tobacco-specific nitrosamine content |
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| CN109060591A (en) * | 2018-07-12 | 2018-12-21 | 天津大学 | A kind of evaluating apparatus and evaluation method for escaping gas performance of the adsorbent |
| CN112595789A (en) * | 2020-12-17 | 2021-04-02 | 广州禾信仪器股份有限公司 | Multifunctional gas chromatography-mass spectrometry device and analysis method |
| CN112595789B (en) * | 2020-12-17 | 2021-10-15 | 广州禾信仪器股份有限公司 | Multifunctional gas chromatography-mass spectrometry device and analysis method |
| CN115184511A (en) * | 2022-08-25 | 2022-10-14 | 宜宾五粮液股份有限公司 | Method for in-situ determination of volatile phenols in white spirit |
| CN115184511B (en) * | 2022-08-25 | 2023-09-19 | 宜宾五粮液股份有限公司 | Method for in-situ determination of volatile phenolic substances in white spirit |
| CN117517696A (en) * | 2023-12-29 | 2024-02-06 | 杭州谱聚医疗科技有限公司 | System and sampling method for obtaining samples in situ on line |
| CN117517696B (en) * | 2023-12-29 | 2024-03-29 | 杭州谱聚医疗科技有限公司 | System and sampling method for obtaining samples in situ on line |
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