CN108074794A - A kind of general type ionization apparatus and its application - Google Patents
A kind of general type ionization apparatus and its application Download PDFInfo
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- CN108074794A CN108074794A CN201611004733.8A CN201611004733A CN108074794A CN 108074794 A CN108074794 A CN 108074794A CN 201611004733 A CN201611004733 A CN 201611004733A CN 108074794 A CN108074794 A CN 108074794A
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- 238000010183 spectrum analysis Methods 0.000 claims abstract description 78
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- 238000005070 sampling Methods 0.000 claims abstract description 16
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- 238000001819 mass spectrum Methods 0.000 claims description 26
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- 239000007788 liquid Substances 0.000 description 8
- BBEAQIROQSPTKN-UHFFFAOYSA-N pyrene Chemical compound C1=CC=C2C=CC3=CC=CC4=CC=C1C2=C43 BBEAQIROQSPTKN-UHFFFAOYSA-N 0.000 description 8
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- 239000012530 fluid Substances 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 5
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- 150000002500 ions Chemical class 0.000 description 5
- 230000000241 respiratory effect Effects 0.000 description 5
- 238000004587 chromatography analysis Methods 0.000 description 4
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- 229940079593 drug Drugs 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- GVEPBJHOBDJJJI-UHFFFAOYSA-N fluoranthrene Natural products C1=CC(C2=CC=CC=C22)=C3C2=CC=CC3=C1 GVEPBJHOBDJJJI-UHFFFAOYSA-N 0.000 description 4
- 238000000034 method Methods 0.000 description 4
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- 239000000126 substance Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- JJHHIJFTHRNPIK-UHFFFAOYSA-N Diphenyl sulfoxide Chemical compound C=1C=CC=CC=1S(=O)C1=CC=CC=C1 JJHHIJFTHRNPIK-UHFFFAOYSA-N 0.000 description 3
- 239000004472 Lysine Substances 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000000835 fiber Substances 0.000 description 3
- 238000004817 gas chromatography Methods 0.000 description 3
- MYWUZJCMWCOHBA-VIFPVBQESA-N methamphetamine Chemical compound CN[C@@H](C)CC1=CC=CC=C1 MYWUZJCMWCOHBA-VIFPVBQESA-N 0.000 description 3
- 229960001252 methamphetamine Drugs 0.000 description 3
- 238000002203 pretreatment Methods 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 210000002700 urine Anatomy 0.000 description 3
- FTVWIRXFELQLPI-ZDUSSCGKSA-N (S)-naringenin Chemical compound C1=CC(O)=CC=C1[C@H]1OC2=CC(O)=CC(O)=C2C(=O)C1 FTVWIRXFELQLPI-ZDUSSCGKSA-N 0.000 description 2
- IKCLCGXPQILATA-UHFFFAOYSA-N 2-chlorobenzoic acid Chemical class OC(=O)C1=CC=CC=C1Cl IKCLCGXPQILATA-UHFFFAOYSA-N 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- JDLKFOPOAOFWQN-VIFPVBQESA-N Allicin Natural products C=CCS[S@](=O)CC=C JDLKFOPOAOFWQN-VIFPVBQESA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- YQEZLKZALYSWHR-UHFFFAOYSA-N Ketamine Chemical compound C=1C=CC=C(Cl)C=1C1(NC)CCCCC1=O YQEZLKZALYSWHR-UHFFFAOYSA-N 0.000 description 2
- OUYCCCASQSFEME-QMMMGPOBSA-N L-tyrosine Chemical compound OC(=O)[C@@H](N)CC1=CC=C(O)C=C1 OUYCCCASQSFEME-QMMMGPOBSA-N 0.000 description 2
- KDXKERNSBIXSRK-UHFFFAOYSA-N Lysine Natural products NCCCCC(N)C(O)=O KDXKERNSBIXSRK-UHFFFAOYSA-N 0.000 description 2
- XADCESSVHJOZHK-UHFFFAOYSA-N Meperidine Chemical compound C=1C=CC=CC=1C1(C(=O)OCC)CCN(C)CC1 XADCESSVHJOZHK-UHFFFAOYSA-N 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 2
- JDLKFOPOAOFWQN-UHFFFAOYSA-N allicin Chemical compound C=CCSS(=O)CC=C JDLKFOPOAOFWQN-UHFFFAOYSA-N 0.000 description 2
- 235000010081 allicin Nutrition 0.000 description 2
- 150000001413 amino acids Chemical class 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- DDRJAANPRJIHGJ-UHFFFAOYSA-N creatinine Chemical compound CN1CC(=O)NC1=N DDRJAANPRJIHGJ-UHFFFAOYSA-N 0.000 description 2
- 238000000688 desorption electrospray ionisation Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000000375 direct analysis in real time Methods 0.000 description 2
- 230000003670 easy-to-clean Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000005040 ion trap Methods 0.000 description 2
- 229960003299 ketamine Drugs 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000012046 mixed solvent Substances 0.000 description 2
- 229940117954 naringenin Drugs 0.000 description 2
- WGEYAGZBLYNDFV-UHFFFAOYSA-N naringenin Natural products C1(=O)C2=C(O)C=C(O)C=C2OC(C1)C1=CC=C(CC1)O WGEYAGZBLYNDFV-UHFFFAOYSA-N 0.000 description 2
- 235000007625 naringenin Nutrition 0.000 description 2
- 229960000482 pethidine Drugs 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- 229920005547 polycyclic aromatic hydrocarbon Polymers 0.000 description 2
- RXHIKAIVEMAPRU-JRIGQVHBSA-N sequiterpene Natural products C1=C(C)[C@@H](OC(C)=O)[C@H](O)[C@@]2(O)[C@H](C)CC[C@@H](C(C)=C)[C@H]21 RXHIKAIVEMAPRU-JRIGQVHBSA-N 0.000 description 2
- 150000003384 small molecules Chemical class 0.000 description 2
- 230000003637 steroidlike Effects 0.000 description 2
- OUYCCCASQSFEME-UHFFFAOYSA-N tyrosine Natural products OC(=O)C(N)CC1=CC=C(O)C=C1 OUYCCCASQSFEME-UHFFFAOYSA-N 0.000 description 2
- 239000000341 volatile oil Substances 0.000 description 2
- CITHEXJVPOWHKC-UUWRZZSWSA-N 1,2-di-O-myristoyl-sn-glycero-3-phosphocholine Chemical compound CCCCCCCCCCCCCC(=O)OC[C@H](COP([O-])(=O)OCC[N+](C)(C)C)OC(=O)CCCCCCCCCCCCC CITHEXJVPOWHKC-UUWRZZSWSA-N 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 244000245420 ail Species 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 239000013060 biological fluid Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
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- 238000011840 criminal investigation Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 229960003724 dimyristoylphosphatidylcholine Drugs 0.000 description 1
- KTWOOEGAPBSYNW-UHFFFAOYSA-N ferrocene Chemical compound [Fe+2].C=1C=C[CH-]C=1.C=1C=C[CH-]C=1 KTWOOEGAPBSYNW-UHFFFAOYSA-N 0.000 description 1
- 235000004611 garlic Nutrition 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
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- 150000002576 ketones Chemical class 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
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- 125000002524 organometallic group Chemical group 0.000 description 1
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- 125000005575 polycyclic aromatic hydrocarbon group Chemical group 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
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Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
- H01J49/10—Ion sources; Ion guns
Abstract
The invention discloses a kind of general type ionization apparatus and its application, the general type ionization apparatus includes high voltage power supply and carbon fiber bundle, and the front end of the carbon fiber bundle is sampling end and ionization end；The afterbody of the carbon fiber bundle is arranged with fixing device, and the rear end of the fixing device is connected with the introduction passage for mobile phase or/and sample, and the afterbody of the carbon fiber bundle is penetrated simultaneously in the introduction passage；Also, at least one of the fixing device and the introduction passage can be conductive, and the high voltage power supply is electrically connected with fixing device or/and introduction passage that can be conductive.Ionization apparatus of the present invention cannot be only used for ionizing the mobile phase of supercritical fluid chromatography, to realize supercritical fluid chromatography and mass spectrographic combination, and it can be used for mutually ionizing gaseous flow, to realize that the ingredient to exhaled gas carries out mass spectral analysis, it can be additionally used in the mass spectral analysis to micro sample to be tested, there is universality and broad application value.
Description
Technical field
The present invention is to be related to a kind of ionization apparatus and its application, is to be related to a kind of general type ionization apparatus specifically
And its application, belong to analytical technique of mass spectrum field.
Background technology
Mass spectrum (MS) is presently the most one of strong chemical analysis means, while also because it is providing analysans point
Protonatomic mass, high sensitivity, selectivity and accuracy in terms of chemical constitution, plays an important role in more and more fields.
Especially, open type ionization massspectrum can make sample obtain detecting under itself state and preceding handled without complicated
Journey, thus played extremely important effect in fields such as real-time, internal analyses.Since desorption electrospray ionization (DESI) and
After Direct Analysis in Real Time (DART) technological invention, 40 kinds of different open type ioning methods are had more than and have been reported.However,
The application of open type ionization is also limited at many aspects, and reason includes the limitation of test compounds species and solvent, because
Low polar compound in nonpolar solvent and gas phase is difficult to realize ionize；Lack the direct injected being connected with mass spectrum to connect
Mouthful and the big surface and solvent of more difficult Direct Analysis in compound.
In addition, supercritical fluid chromatography (SFC) is development the 1980s and a kind of new technology for improving, be with
Supercritical fluid does mobile phase, and the chromatographic process for being separated, being analyzed by the solvability of mobile phase has gas phase color concurrently
The characteristics of spectrum and liquid chromatogram, the unconformable higher boiling of gas-chromatography, low volatility sample can be not only analyzed, but also has compared high-efficient liquid phase color
Spectrum has faster analyze speed and condition, can be connected with existing any liquid phase or vapor detection device, has at qualitative, quantitative aspect
Larger range of choice.But can realize there is presently no a kind of mass ion source and be adapted to the preferable of supercritical fluid, because
It is relatively low to the Ionization Efficiency of low polarity sample for common ESI ion sources, and the addition of modifying agent not only makes analysis operation numerous
It is trivial, while the ionization of sample is a greater impact.
In short, there is presently no the ionization that a kind of ionization apparatus not only can be suitably used for polar solvent, but also can be suitably used for non-
Therefore the ionization of polar solvent, can't realize the combination of gas-chromatography and supercritical fluid chromatography and mass spectral analysis so far,
And it can't realize that the actual sample of complexity this to characteristics of contaminated respiratory droplets gas carries out the relevant report of direct mass spectral analysis at present.
The content of the invention
In view of the above-mentioned problems existing in the prior art, it both can be suitably used for polar solvent the object of the present invention is to provide a kind of
Ionization, and the ionization of nonpolar solvent is can be suitably used for, it can especially realize gas-chromatography and supercritical fluid chromatography and mass spectrum
Analyze the general type ionization apparatus being combined and its application.
To achieve the above object, the technical solution adopted by the present invention is as follows：
A kind of general type ionization apparatus, including high voltage power supply and carbon fiber bundle, the front end of the carbon fiber bundle is sampling
End and ionization end, the afterbody of the carbon fiber bundle are arranged with fixing device, and the rear end of the fixing device is connected with to flow
The introduction passage of dynamic phase or/and sample, the afterbody of the carbon fiber bundle are penetrated simultaneously in the introduction passage；It is also, described
At least one of fixing device and the introduction passage can be conductive, the high voltage power supply with can conduction fixing device or/and draw
Enter passage electrical connection.
Preferably, the carbon fiber bundle is made of at least 100 a diameter of 5~10 μm of carbon fiber wires.
As further preferred scheme, the carbon fiber bundle is by least 1000 a diameter of 5~10 μm of carbon fiber wires
Composition.
As still more preferably scheme, the carbon fiber bundle is by least 3000 a diameter of 5~10 μm of carbon fibers
Silk composition.
Preferably, the front end of the carbon fiber bundle protrude from the length of the front end of the fixing device for 0.5~
2cm。
Preferably, the fixing device is the peek that internal diameter is adapted with the carbon fiber bundle and introduction passage
Pipe fitting, conducting metal adapter or conductive metal pipe.
Preferably, the introduction passage is peek pipes or conductive metal pipe.
As further preferred scheme, the conducting metal is stainless steel.
Preferably, it is detachable connection between the fixing device and the introduction passage.
Preferably, the introduction passage tail end be arranged with for mobile phase or/and sample effuser phase
The adapter of connection.
Preferably, the operating voltage of the general type ionization apparatus is 500~4000V.
Preferably, the axis of the front end of the carbon fiber bundle and mass spectrum sample intake passage is in same horizontal line or is in
Obtuse angle.
Preferably, the front-end port of the carbon fiber bundle and the port distance of mass spectrum sample intake passage are 2~10mm.
Experiment proves：Using ionization apparatus of the present invention, not only polar solvent, nonpolar solvent can be realized from
Sonization, and solid sample, gaseous sample, liquid sample and the supercritical fluid between liquid and gaseous state can be realized
Efficient ionization, especially can be to polycyclic aromatic hydrocarbon (PAH), and drugs, phosphate, steroidal compounds, sequiterpene and metal have
The classes of compounds such as machine compound are respectively provided with good ionising effect, it can be achieved that supercritical fluid chromatography (SFC), gel infiltration
The analysis means such as chromatography (GPC), positive chromatography (NPLC), liquid chromatogram and the combination of mass spectral analysis；In addition, it is of the present invention from
Son makeup, which is put, to carry out sample pre-treatment and sampling is convenient：It may be employed and pick or that mode is added dropwise is direct for fluid sample
Sampling directly can gently sweep solid sample collection sampling, cannot be only used for the mass spectral analysis of micro sample to be tested, and can be used for
Direct mass spectral analysis is carried out to characteristics of contaminated respiratory droplets gas componant, there is very strong universality, and also there is simple in structure, operation letter
Just, it is of low cost, the advantages that environmentally friendly (being cleaned and reused completely by baked wheaten cake method) easy to clean, can with it is normal
The mass spectrograph seen is (such as：Triple quadrupole mass spectrometer, time of-flight mass spectrometer, ion trap mass spectrometer etc.) it is mutually compatible with, application range
Extensively, it is highly practical, there is apparent application value.
Description of the drawings
Fig. 1 is a kind of structure diagram for ionization apparatus that the embodiment of the present invention 1 provides；
Fig. 2 is the structure diagram for another ionization apparatus that the embodiment of the present invention 2 provides；
Fig. 3 is the mounting structure schematic diagram when ionization apparatus that the embodiment of the present invention 3 provides is used for mass spectral analysis；
Fig. 3-a are the mass spectral analysis figure of gaultherolin in the embodiment of the present invention 3；
Fig. 3-b are the mass spectral analysis figure of ocimenum in the embodiment of the present invention 3；
Fig. 3-c are the mass spectral analysis figure of 2- cyclopentanone in the embodiment of the present invention 3；
Fig. 3-d are the mass spectral analysis figure of diphenyl sulfoxide in the embodiment of the present invention 3；
Fig. 4-a are the mass spectral analysis figure of ketamine in the embodiment of the present invention 4；
Fig. 4-b are the mass spectral analysis figure of pethidine in the embodiment of the present invention 4；
Fig. 5 is the mass spectral analysis figure of the embodiment of the present invention 5；
Fig. 6 is the mass spectral analysis figure of the embodiment of the present invention 6；
Fig. 7-a are the mass spectral analysis figure of pyrene in the embodiment of the present invention 7；
Fig. 7-b are the mass spectral analysis figure of anthracene in the embodiment of the present invention 7；
Fig. 8 is the mass spectral analysis figure of the embodiment of the present invention 8；
Fig. 9-a are the mass spectral analysis figure of naringenin in the embodiment of the present invention 9；
Fig. 9-b are the mass spectral analysis figure of 2- chlorobenzoic acids in the embodiment of the present invention 9；
Fig. 9-c are the mass spectral analysis figure of 3- fluobenzoic acids in the embodiment of the present invention 9；
Figure 10-a are the mass spectral analysis figure of lysine in the embodiment of the present invention 10；
Figure 10-b are the mass spectral analysis figure of tyrosine in the embodiment of the present invention 10；
Figure 11 is the mass spectral analysis figure of the embodiment of the present invention 11；
Figure 12-a for volunteer a institutes exhaled gas in the embodiment of the present invention 12 mass spectral analysis figure；
Figure 12-b for volunteer b institutes exhaled gas in the embodiment of the present invention 12 mass spectral analysis figure；
Figure 12-c for volunteer c institutes exhaled gas in the embodiment of the present invention 12 mass spectral analysis figure；
Figure 13-a are the mass spectral analysis figure of ocimenum in the embodiment of the present invention 13；
Figure 13-b are the mass spectral analysis figure of allicin in the embodiment of the present invention 13；
In figure：1st, high voltage power supply；2nd, carbon fiber bundle；3rd, fixing device；4th, introduction passage；5th, adapter；6- mass spectrum sample introductions
Passage.
Specific embodiment
Technical solution of the present invention is described in further detail and completely with reference to embodiment and attached drawing.
Embodiment 1
As shown in Figure 1：A kind of general type ionization apparatus provided by the invention, including high voltage power supply 1 and carbon fiber bundle 2,
The front end of the carbon fiber bundle 2 is sampling end and ionization end, and the afterbody of the carbon fiber bundle 2 is arranged with fixing device 3, described
The rear end of fixing device 3 is connected with for mobile phase or/and the introduction passage of sample 4, and the afterbody of the carbon fiber bundle 2 is worn simultaneously
Enter in the introduction passage 4；Also, at least one of the fixing device 3 and the introduction passage 4 can be conductive, this implementation
The introduction passage 4 of the mobile phase or/and sample in example for conductive metal pipe (such as：Stainless steel metal pipe), the high pressure
Power supply 1 is electrically connected with the introduction passage 4, by conductive introduction passage 4 by potential conduction to carbon fiber bundle 2, so that carbon
The sample of 2 front-end collection of fibre bundle ionizes.
Fixing device 3 described in the present embodiment can be that internal diameter is adapted with the carbon fiber bundle 2 and introduction passage 4
Peek pipe fittings, conducting metal adapter or conductive metal pipe.
When being arranged with adapter 5 in the rear end of the mobile phase or/and the introduction passage of sample 4, adapter 5 can be passed through
Realize that the effuser of mobile phase or/and sample is connected with introduction passage 4, so as to fulfill the combination with other analytical instrument.
Embodiment 2
As shown in Figure 2：Another kind general type ionization apparatus provided by the invention, including high voltage power supply 1 and carbon fiber bundle
2, the front end of the carbon fiber bundle 2 is sampling end and ionization end, and the afterbody of the carbon fiber bundle 2 is arranged with fixing device 3, institute
The rear end for stating fixing device 3 is connected with for mobile phase or/and the introduction passage of sample 4, and the afterbody of the carbon fiber bundle 2 is simultaneously
It penetrates in the introduction passage 4；Also, at least one of the fixing device 3 and the introduction passage 4 can be conductive, this reality
It is the fixing device 3 for conducting metal adapter or conductive metal pipe to apply in example, the high voltage power supply 1 and the fixing device
3 electrical connections, by conductive fixing device 3 by potential conduction to carbon fiber bundle 2, so that the sample of 2 front-end collection of carbon fiber bundle
Product ionize.
Introduction passage 4 described in the present embodiment can be peek pipe or conductive metal pipe (such as：Stainless steel metal pipe).
When being arranged with adapter 5 in the rear end of the mobile phase or/and the introduction passage of sample 4, adapter 5 can be passed through
Realize that the effuser of mobile phase or/and sample is connected with introduction passage 4, so as to fulfill the combination with other analytical instrument.
Embodiment 3
As shown in figure 3, general type ionization apparatus provided by the invention includes high voltage power supply 1 and carbon fiber bundle 2, the carbon
The front end of fibre bundle 2 is sampling end and ionization end, and the afterbody of the carbon fiber bundle 2 is arranged with fixing device 3, the fixed dress
It puts 3 rear end to be connected with for mobile phase or/and the introduction passage of sample 4, the afterbody of the carbon fiber bundle 2 penetrates described simultaneously
Introduction passage 4 in；Adapter 5 is also arranged in the rear end of the mobile phase or/and the introduction passage of sample 4.The carbon is fine
The axis for tieing up front end and the mass spectrum sample intake passage 6 of beam 2 is in same horizontal line or in obtuse angle (i.e.：90 ° of ＜ α≤180 °), it is described
The front-end port of carbon fiber bundle 2 is 2~10mm with the port distance d of mass spectrum sample intake passage 6.
The fixing device 3 can be that internal diameter connects with the peek pipes that the carbon fiber bundle 2 and introduction passage 4 are adapted
Head, conducting metal adapter or conductive metal pipe, the introduction passage 4 can be peek pipes or conductive metal pipe, but described solid
Determining at least one of device 3 and the introduction passage 4 can be conductive, the high voltage power supply 1 with can be conductive fixing device 3 or/and
Introduction passage 4 is electrically connected；The conducting metal can be stainless steel.
The carbon fiber bundle 2 is made of at least 100 a diameter of 5~10 μm of carbon fiber wires, straight at least 1000
The carbon fiber wire composition that footpath is 5~10 μm is preferable, and it is optimal to be formed at least 3000 a diameter of 5~10 μm of carbon fiber wires.
The length that the front end of the carbon fiber bundle 2 protrudes from the front end of the fixing device 3 is preferably 0.5~2cm.
It is detachable connection between the fixing device 3 and the introduction passage 4, with lower carbon fiber bundle 2 easy to disassemble
It is sampled or cleaning treatment.
Use above-mentioned ionization apparatus with mass spectrograph (mass analyzer is triple quadrupole bar) to following compound solution
Supercritical fluid chromatography effluent carry out mass spectral analysis：
Corresponding compound is configured to the testing sample solution that concentration is 0.1mg/mL by the solvent in table respectively；
The effuser of supercritical fluid chromatography with the adapter 5 in the ionization apparatus is connected, makes shooting flow
The effluent of body colour spectrum enters the introduction passage 4 and then reaches the front end of carbon fiber bundle 2；
Using carbon dioxide as the mobile phase of supercritical fluid chromatography, flow velocity is 0.2~1mL/min, while it is molten to add in methanol
Agent, the percentage that methanol mutually accounts for overall flow rate phase volume are 2~10%, and sample size is 1~5 μ L；Power on, voltage is made gradually to rise
To 2.5kV, the sample of 2 front-end collection of carbon fiber bundle is caused to ionize, carried out by mass spectrum sample intake passage 6 into mass spectrograph
Mass spectral analysis.
The mass spectral analysis figure for the gaultherolin that Fig. 3-a are (occurs [M+H] in figure at m/z=153+Ion
Peak), the mass spectral analysis figure for the ocimenum that Fig. 3-b are (occurs [M+H] in figure at m/z=137+Quasi-molecular ions), Fig. 3-c
The mass spectral analysis figure of 2- cyclopentanone to obtain (occurs [M+H] in figure at m/z=99+Quasi-molecular ions), Fig. 3-d are obtained
The mass spectral analysis figure of diphenyl sulfoxide (occurs [M+H] in figure at m/z=203+Quasi-molecular ions), and without too many miscellaneous in figure
Matter quasi-molecular ions disturbs, and illustrates to be used in combination with supercritical fluid chromatography using ionization apparatus of the present invention, and on
4 kinds of compounds are stated, only diphenyl sulfoxide can realize ionization under the conditions of existing ESI, and other 3 kinds of compounds cannot be real
It now ionizes, further illustrates the present invention and achieve conspicuousness progress compared with the prior art.
Embodiment 4
Use ionization apparatus shown in Fig. 3 with mass spectrograph (mass analyzer is triple quadrupole bar) to material surface solid-state
Sample carries out gently sweeping collection and carries out mass spectral analysis：
Scene of a crime is simulated at one, we expose the drugs sample for having denier on the surface：KetamineAnd pethidine50ng samples are dissolved using 2 μ L methanol and are coated on 1cm2Solid table
Face；Entire carbon fiber bundle is taken out, and is gently swept using its front end and collects the surface of solids to sample；
After sampling, the ionization apparatus is installed, secondary solvent methanol (polarity is then passed through by introduction passage 4
Solvent)；Power on, voltage is made to be gradually increased to 1.8kV, the sample of 2 front-end collection of carbon fiber bundle is caused to ionize, is passed through
Mass spectrum sample intake passage 6 carries out mass spectral analysis into mass spectrograph.
The mass spectral analysis figure for the ketamine that Fig. 4-a are (occurs [M+H] in figure at m/z=238+Quasi-molecular ions),
The mass spectral analysis figure for the pethidine that Fig. 4-b are (occurs [M+H] in figure at m/z=248+Quasi-molecular ions), and in figure
It disturbs, illustrates using ionization apparatus of the present invention on solid matter surface without other apparent foreign ion peaks
Solid sample also have good concentration effect and Ionization Efficiency, this convenient, diversified sampling means also for criminal investigation,
The mass spectral analysis of solid-state sample during medicine etc. is provided convenience, and is further illustrated the present invention and is obtained compared with the prior art
Conspicuousness progress.
Embodiment 5
Use ionization apparatus shown in Fig. 3 with mass spectrograph (mass analyzer is triple quadrupole bar) to actual sample：People
Drugs (crystal methamphetamine in body urine) carry out mass spectral analysis：
Seldom crystal methamphetamine (0.1 μ gmL are added in not diluted human urine sample 1mL-1), entire carbon is fine
It ties up beam to take out, and its front end is made to be directly immersed in urine sample solution and is sampled；
After sampling, the ionization apparatus is installed, then powers on, voltage is made to be gradually increased to 1.8kV, cause carbon
The sample of 2 front-end collection of fibre bundle ionizes, and mass spectral analysis is carried out into mass spectrograph by mass spectrum sample intake passage 6.
The mass spectral analysis figure that Fig. 5 is, as seen from Figure 5：Except some endogenous materials such as urea and kreatinin from
Occur [M+H] of the crystal methamphetamine at m/z=150 beyond sub- peak, in figure+Quasi-molecular ions illustrates using of the present invention
Ionization apparatus also has good Ionization Efficiency for actual samples such as biological fluids, and analysis is very simple and effective,
Sample pre-treatments need not be carried out, further illustrates the present invention and achieves conspicuousness progress compared with the prior art.
Embodiment 6
Use ionization apparatus shown in Fig. 3 with mass spectrograph (mass analyzer is triple quadrupole bar) to phosphatide cpd two
Dimyristoylphosphatidycholine：Carry out mass spectrum
Analysis：
Use methanol：Water (volume ratio 1:1) dimyristoyl phosphatidyl choline is configured to about 10 μ g/ by mixed solvent
The testing sample solution of mL；The front end that 2 μ L are added drop-wise to carbon fiber bundle 2 is pipetted using pipettor；Then power on, make voltage by
It edges up to 3.0kV, the sample of 2 front-end collection of carbon fiber bundle is caused to ionize, mass spectrograph is entered by mass spectrum sample intake passage 6
Carry out mass spectral analysis.
The mass spectral analysis figure that Fig. 6 is, as seen from Figure 6：Occur in figure and the relevant quasi-molecular ions [M+ of the compound
H]+=674, it disturbs, illustrates using ionization apparatus of the present invention for larger point almost without other impurity peaks
Sub- phosphatide cpd also has good Ionization Efficiency, further illustrates the present invention and achieves conspicuousness compared with the prior art
Progress.
Embodiment 7
Use ionization apparatus shown in Fig. 3 with mass spectrograph (mass analyzer is triple quadrupole bar) to polycyclic aromatic hydrocarbon pyrene：And anthracene：Carry out mass spectral analysis：
Pyrene and anthracene are each configured to the testing sample solution of about 10 μ g/mL using toluene for solvent；
Pipette the front end that 2 μ L are added drop-wise to carbon fiber bundle 2 respectively using pipettor；Then power on, voltage is made gradually to rise
To 1.5kV, the sample of 2 front-end collection of carbon fiber bundle is caused to ionize, carried out by mass spectrum sample intake passage 6 into mass spectrograph
Mass spectral analysis.
The mass spectral analysis figure for the pyrene that Fig. 7-a are (occurs [M] in figure at m/z=202+.Quasi-molecular ions), Fig. 7-b are
The mass spectral analysis figure of obtained anthracene (occurs [M] in figure at m/z=178+.Quasi-molecular ions), and almost without other in figure
Impurity peaks interference, illustrate the use ionization apparatus of the present invention multiring aromatic hydrocarbon that is difficult to ionize for existing ESI
Closing object also has good Ionization Efficiency, while it can be that low polarity as toluene is molten to ionize selected secondary solvent
Agent without being limited to polar solvent as ESI, further illustrates the present invention and achieves conspicuousness compared with the prior art
Progress.
Embodiment 8
Ionization apparatus shown in Fig. 3 is used to be closed with mass spectrograph (mass analyzer is triple quadrupole bar) to Organometallic
Object ferroceneCarry out mass spectral analysis：
Ferrocene is configured to the testing sample solution of about 10 μ g/mL using toluene for solvent；
The front end that 2 μ L are added drop-wise to carbon fiber bundle 2 is pipetted using pipettor；Then power on, be gradually increased to voltage
2.5kV causes the sample of 2 front-end collection of carbon fiber bundle to ionize, and matter is carried out into mass spectrograph by mass spectrum sample intake passage 6
Spectrum analysis.
The mass spectral analysis figure that Fig. 8 is occurs [M] at m/z=186 in figure+.Quasi-molecular ions, and almost do not have in figure
There are other impurity peaks to disturb, illustrate have for the existing ESI metals for being difficult to ionize using ionization apparatus of the present invention
Machine compound also has good Ionization Efficiency, while it can be low polarity as toluene to ionize selected secondary solvent
Solvent without being limited to polar solvent as ESI, is further illustrated the present invention and achieved significantly compared with the prior art
Property progress.
Embodiment 9
Use ionization apparatus shown in Fig. 3 with mass spectrograph (mass analyzer is triple quadrupole bar) in following form
Compound carries out the negative ion mass spectrum analysis under the conditions of negative high voltage：
Corresponding compound is configured to the testing sample solution that concentration is 10 μ g/mL by the solvent in table respectively；
Sample solution is guided to by carbon fiber bundle 2 by introduction passage 4 with the flow velocity of 2~15 μ L/min by sampling pump respectively
Front end；Then power on, voltage made to be gradually increased to 2.5kV, the sample of 2 front-end collection of carbon fiber bundle is caused to ionize,
Mass spectral analysis is carried out into mass spectrograph by mass spectrum sample intake passage 6.
The mass spectral analysis figure for the naringenin that Fig. 9-a are (occurs [M-H] in figure at m/z=271-Quasi-molecular ions),
The mass spectral analysis figure for the 2- chlorobenzoic acids that Fig. 9-b are (occurs [M-H] in figure at m/z=155-Quasi-molecular ions), Fig. 9-c
The mass spectral analysis figure of 3- fluobenzoic acids to obtain (occurs [M-H] in figure at m/z=139-Quasi-molecular ions), and in figure
It is disturbed almost without other impurity peaks, illustrates to treat when connecting negative high voltage power source using ionization apparatus of the present invention
Surveying compound also has good Ionization Efficiency, can obtain the mass spectrogram of its anion；In addition, the incorporation way of sample removes
It can be added dropwise with micro- sample sample injector outer, the front end of carbon fiber bundle 2 can also be guided to by introduction passage 4 by peristaltic pump, so as to
It can be mutually combined with liquid chromatogram, realize the continuity detection and analysis to sample, further illustrate the present invention compared with existing skill
Art achieves conspicuousness progress.
Embodiment 10
Use ionization apparatus shown in Fig. 3 with mass spectrograph (mass analyzer is triple quadrupole bar) to lysineAnd tyrosineCarry out mass spectral analysis：
Use methanol：Water (volume ratio 1:1) both the above amino acid is each configured to about 10 μ g/mL by mixed solvent
Testing sample solution；
Pipette the front end that 2 μ L are added drop-wise to carbon fiber bundle 2 respectively using pipettor；Then power on, voltage is made gradually to rise
To 1.5kV, the sample of 2 front-end collection of carbon fiber bundle is caused to ionize, carried out by mass spectrum sample intake passage 6 into mass spectrograph
Mass spectral analysis.
The mass spectral analysis figure for the lysine that Figure 10-a are (occurs [M+H] in figure at m/z=147+Quasi-molecular ions),
The mass spectral analysis figure for the tyrosine that Figure 10-b are (occurs [M+H] in figure at m/z=182+Quasi-molecular ions), and in figure
It is disturbed almost without other impurity peaks, illustrates for amino acid also to have using ionization apparatus of the present invention good
Ionization Efficiency.
Embodiment 11
Use ionization apparatus shown in Fig. 3 with mass spectrograph (mass analyzer is triple quadrupole bar) to small-molecule substance third
Ketone:Carry out mass spectral analysis：
Acetone is guided to the front end of carbon fiber bundle 2 by sampling pump with the flow velocity of 2~15 μ L/min by introduction passage 4；So
After power on, voltage is made to be gradually increased to 1.0kV, the sample of 2 front-end collection of carbon fiber bundle is caused to ionize, passes through mass spectrum
Sample intake passage 6 carries out mass spectral analysis into mass spectrograph.
The mass spectral analysis figure that Figure 11 is occurs [M+H] at m/z=59 in figure+Quasi-molecular ions, and in figure almost
It is disturbed without others impurity peaks, illustrates to be less than 100 small molecule chemical combination for m/z using ionization apparatus of the present invention
Object also has good Ionization Efficiency.
Embodiment 12
Use ionization apparatus shown in Fig. 3 with mass spectrograph (mass analyzer is triple quadrupole bar) to characteristics of contaminated respiratory droplets gas
Ingredient carries out direct mass spectral analysis：
It first passes through micro syringe or pipettor and 2~10 μ L water or acetonitrile or arbitrary is directly added dropwise in 2 front end of carbon fiber bundle
Other not volatile solvents are to soak 2 front end of carbon fiber bundle；
The adapter 5 of 4 tail end of introduction passage is made to be connected with gas-guide tube, is then directly exhaled against gas-guide tube；
Power on, voltage is made to be gradually increased to 3.0kV, the sample of 2 front-end collection of carbon fiber bundle is caused to ionize, lead to
It crosses mass spectrum sample intake passage 6 and carries out mass spectral analysis into mass spectrograph.
Figure 12-a, 12-b and 12-c are respectively the mass spectral analysis of compound in different volunteer a, b, c institutes exhaled gas
Figure illustrate use ionization apparatus of the present invention for the polarity in this complex sample of characteristics of contaminated respiratory droplets gas, volatility/
Involatile constituent, and under the conditions of gas phase mobile phase, it may have good Ionization Efficiency has broad application prospects.
Embodiment 13
Use ionization apparatus shown in Fig. 3 with mass spectrograph (mass analyzer is triple quadrupole bar) to using nitrogen as flowing
The volatile compound of phase carries out mass spectral analysis：
2~10 μ L water or acetonitrile or arbitrarily its is directly added dropwise in 2 front end of carbon fiber bundle by micro syringe or pipettor
Its not volatile solvent is to soak 2 front end of carbon fiber bundle；
The adapter 5 of 4 tail end of introduction passage is made to be connected with a hollow tube, is then put into a gas phase bottle to be measured
Compound：(a) ethanol solution (10 μ g/mL) of volatile oil component ocimenum, the section of (b) fresh garlic；It is direct to incite somebody to action nitrogen all the way
Gas phase bottle is passed through, another head space that sample to be tested is collected with gas-guide tube is excluded by nitrogen help, and is introduced directly into hose；
Power on, voltage is made to be gradually increased to 2.0kV, the sample of 2 front-end collection of carbon fiber bundle is caused to ionize, lead to
It crosses mass spectrum sample intake passage 6 and carries out mass spectral analysis into mass spectrograph.
The mass spectral analysis figure for the ocimenum that Figure 13-a are (occurs [M+H] in figure at m/z=137+Quasi-molecular ions),
The mass spectral analysis figure for the allicin that Figure 13-b are (occurs [M+H] in figure at m/z=163+Quasi-molecular ions), and in figure
It disturbs, illustrates using ionization apparatus of the present invention in nitrogen buffer gas almost without other impurity peaks, it can
Mass spectral analysis is directly carried out to the head space of volatile oil component and actual sample, and with good Ionization Efficiency.
Above-mentioned experiment proves：It, not only can be real to polar solvent, nonpolar solvent using ionization apparatus of the present invention
Now ionize, and to solid sample, gaseous sample, liquid sample and the equal energy of supercritical fluid between liquid and gaseous state
Realize efficient ionization, it especially can be to polycyclic aromatic hydrocarbon (PAH), drugs, phosphate, steroidal compounds, sequiterpene and gold
Belong to the classes of compounds such as organic compound and be respectively provided with good ionising effect, it can be achieved that supercritical fluid chromatography (SFC), gel
The analysis means such as permeation chromatography (GPC), positive chromatography (NPLC), liquid chromatogram and the combination of mass spectral analysis；In addition, institute of the present invention
Ionization apparatus is stated without carrying out pre-treatment to sample and sampling conveniently：It may be employed for fluid sample and pick or be added dropwise mode
It directly samples, collection sampling directly can be gently swept to solid sample, cannot be only used for the mass spectral analysis of micro sample to be tested, Er Qieke
For carrying out direct mass spectral analysis to characteristics of contaminated respiratory droplets gas componant, there is very strong universality, and also there is simple in structure, behaviour
Make it is easy, it is of low cost, can be with the advantages that environmentally friendly (being cleaned and reused completely by baked wheaten cake method) easy to clean
With common mass spectrograph (such as：Triple quadrupole mass spectrometer, time of-flight mass spectrometer, ion trap mass spectrometer etc.) mutually it is compatible with, it applies
Scope is wide, highly practical, has apparent application value.
It is it is necessary to described herein finally：More than content is served only for making in further detail technical scheme
Explanation, it is impossible to be interpreted as limiting the scope of the invention, those skilled in the art's the above according to the present invention is made
Some the nonessential modifications and adaptations gone out all belong to the scope of protection of the present invention.
Claims (10)
1. a kind of general type ionization apparatus, including high voltage power supply and carbon fiber bundle, the front end of the carbon fiber bundle is sampling end
With ionization end；It is characterized in that：The afterbody of the carbon fiber bundle is arranged with fixing device, the rear end connection of the fixing device
Mobile phase or/and the introduction passage of sample are useful for, the afterbody of the carbon fiber bundle is penetrated simultaneously in the introduction passage；And
And at least one of the fixing device and the introduction passage can be conductive, the high voltage power supply and fixing device that can be conductive
Or/and introduction passage electrical connection.
2. general type ionization apparatus according to claim 1, it is characterised in that：The carbon fiber bundle is by least 100
The carbon fiber wire composition that a diameter of 5~10 μm of root.
3. general type ionization apparatus according to claim 1, it is characterised in that：The front end of the carbon fiber bundle protrudes from
The length of the front end of the fixing device is 0.5~2cm.
4. general type ionization apparatus according to claim 1, it is characterised in that：The fixing device be internal diameter with it is described
Peek pipe fittings, conducting metal adapter or the conductive metal pipe that carbon fiber bundle and introduction passage are adapted；Described introduce is led to
Road is managed for peek or conductive metal pipe.
5. general type ionization apparatus according to claim 1, it is characterised in that：It is arranged in the tail end of the introduction passage
There is adapter.
6. general type ionization apparatus according to claim 1, it is characterised in that：The front end of the carbon fiber bundle and mass spectrum
The axis of sample intake passage is in same horizontal line or in obtuse angle.
7. general type ionization apparatus according to claim 1, it is characterised in that：The front-end port of the carbon fiber bundle with
The port distance of mass spectrum sample intake passage is 2~10mm.
8. a kind of application of the general type ionization apparatus any one of claim 1 to 7, it is characterised in that：For right
The mobile phase of supercritical fluid chromatography is ionized, to realize the combination of supercritical fluid chromatography analysis and mass spectral analysis.
9. a kind of application of the general type ionization apparatus any one of claim 1 to 7, it is characterised in that：For right
Gaseous flow is mutually ionized, to realize that the ingredient to exhaled gas carries out mass spectral analysis.
10. a kind of application of the general type ionization apparatus any one of claim 1 to 7, it is characterised in that：For right
The mass spectral analysis of micro sample to be tested.
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| CN110398532A (en) * | 2019-08-22 | 2019-11-01 | 中国科学院上海有机化学研究所 | A kind of ultrasonic extraction atomization auxiliary carbon fiber ionization apparatus and the method using device realization ionization |
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| CN103258711A (en) * | 2013-05-21 | 2013-08-21 | 中国科学院上海有机化学研究所 | Solvent auxiliary electrospray ionization device and method for achieving electrospray ionization by utilizing same |
| CN104599935A (en) * | 2015-01-29 | 2015-05-06 | 中国科学院上海有机化学研究所 | Carbon fiber electric atomizing ionization device and method for realizing electric atomizing ionization by using device |
| CN206179823U (en) * | 2016-11-15 | 2017-05-17 | 中国科学院上海有机化学研究所 | General right type ionizationoun device |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103258711A (en) * | 2013-05-21 | 2013-08-21 | 中国科学院上海有机化学研究所 | Solvent auxiliary electrospray ionization device and method for achieving electrospray ionization by utilizing same |
| CN104599935A (en) * | 2015-01-29 | 2015-05-06 | 中国科学院上海有机化学研究所 | Carbon fiber electric atomizing ionization device and method for realizing electric atomizing ionization by using device |
| CN206179823U (en) * | 2016-11-15 | 2017-05-17 | 中国科学院上海有机化学研究所 | General right type ionizationoun device |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110398532A (en) * | 2019-08-22 | 2019-11-01 | 中国科学院上海有机化学研究所 | A kind of ultrasonic extraction atomization auxiliary carbon fiber ionization apparatus and the method using device realization ionization |
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