CN110364412A - A kind of flame assisted electrospray ionization apparatus and the method using device realization ionization - Google Patents
A kind of flame assisted electrospray ionization apparatus and the method using device realization ionization Download PDFInfo
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- CN110364412A CN110364412A CN201910665569.2A CN201910665569A CN110364412A CN 110364412 A CN110364412 A CN 110364412A CN 201910665569 A CN201910665569 A CN 201910665569A CN 110364412 A CN110364412 A CN 110364412A
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- 238000000132 electrospray ionisation Methods 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 27
- 238000001819 mass spectrum Methods 0.000 claims abstract description 71
- 239000007921 spray Substances 0.000 claims abstract description 68
- 239000000523 sample Substances 0.000 claims description 92
- 239000000446 fuel Substances 0.000 claims description 44
- 150000002500 ions Chemical class 0.000 claims description 28
- 239000012488 sample solution Substances 0.000 claims description 22
- 238000012360 testing method Methods 0.000 claims description 19
- 238000000889 atomisation Methods 0.000 claims description 7
- 230000015572 biosynthetic process Effects 0.000 claims description 7
- 230000005540 biological transmission Effects 0.000 claims description 5
- 150000001875 compounds Chemical class 0.000 abstract description 10
- 239000011159 matrix material Substances 0.000 abstract description 10
- -1 small molecule compound Chemical class 0.000 abstract description 9
- 239000002904 solvent Substances 0.000 abstract description 6
- 238000010183 spectrum analysis Methods 0.000 description 23
- REFJWTPEDVJJIY-UHFFFAOYSA-N Quercetin Chemical compound C=1C(O)=CC(O)=C(C(C=2O)=O)C=1OC=2C1=CC=C(O)C(O)=C1 REFJWTPEDVJJIY-UHFFFAOYSA-N 0.000 description 22
- AYFVYJQAPQTCCC-GBXIJSLDSA-N L-threonine Chemical compound C[C@@H](O)[C@H](N)C(O)=O AYFVYJQAPQTCCC-GBXIJSLDSA-N 0.000 description 14
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 12
- ZVOLCUVKHLEPEV-UHFFFAOYSA-N Quercetagetin Natural products C1=C(O)C(O)=CC=C1C1=C(O)C(=O)C2=C(O)C(O)=C(O)C=C2O1 ZVOLCUVKHLEPEV-UHFFFAOYSA-N 0.000 description 11
- HWTZYBCRDDUBJY-UHFFFAOYSA-N Rhynchosin Natural products C1=C(O)C(O)=CC=C1C1=C(O)C(=O)C2=CC(O)=C(O)C=C2O1 HWTZYBCRDDUBJY-UHFFFAOYSA-N 0.000 description 11
- 238000004458 analytical method Methods 0.000 description 11
- MWDZOUNAPSSOEL-UHFFFAOYSA-N kaempferol Natural products OC1=C(C(=O)c2cc(O)cc(O)c2O1)c3ccc(O)cc3 MWDZOUNAPSSOEL-UHFFFAOYSA-N 0.000 description 11
- 229960001285 quercetin Drugs 0.000 description 11
- 235000005875 quercetin Nutrition 0.000 description 11
- 230000000694 effects Effects 0.000 description 10
- ZYGHJZDHTFUPRJ-UHFFFAOYSA-N coumarin Chemical compound C1=CC=C2OC(=O)C=CC2=C1 ZYGHJZDHTFUPRJ-UHFFFAOYSA-N 0.000 description 9
- 238000004949 mass spectrometry Methods 0.000 description 9
- 239000001257 hydrogen Substances 0.000 description 8
- 229910052739 hydrogen Inorganic materials 0.000 description 8
- PQMOXTJVIYEOQL-UHFFFAOYSA-N Cumarin Natural products CC(C)=CCC1=C(O)C(C(=O)C(C)CC)=C(O)C2=C1OC(=O)C=C2CCC PQMOXTJVIYEOQL-UHFFFAOYSA-N 0.000 description 7
- FSOGIJPGPZWNGO-UHFFFAOYSA-N Meomammein Natural products CCC(C)C(=O)C1=C(O)C(CC=C(C)C)=C(O)C2=C1OC(=O)C=C2CCC FSOGIJPGPZWNGO-UHFFFAOYSA-N 0.000 description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 6
- QNAYBMKLOCPYGJ-REOHCLBHSA-N L-alanine Chemical compound C[C@H](N)C(O)=O QNAYBMKLOCPYGJ-REOHCLBHSA-N 0.000 description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 239000004473 Threonine Substances 0.000 description 6
- 229960002898 threonine Drugs 0.000 description 6
- 229940024606 amino acid Drugs 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 229910001414 potassium ion Inorganic materials 0.000 description 5
- 229910001415 sodium ion Inorganic materials 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- NPYPAHLBTDXSSS-UHFFFAOYSA-N Potassium ion Chemical compound [K+] NPYPAHLBTDXSSS-UHFFFAOYSA-N 0.000 description 4
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 4
- 150000001413 amino acids Chemical class 0.000 description 4
- 238000002485 combustion reaction Methods 0.000 description 4
- 239000012046 mixed solvent Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 230000002572 peristaltic effect Effects 0.000 description 4
- 150000003384 small molecules Chemical class 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 150000001335 aliphatic alkanes Chemical class 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 229930195733 hydrocarbon Natural products 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- 125000003412 L-alanyl group Chemical group [H]N([H])[C@@](C([H])([H])[H])(C(=O)[*])[H] 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 2
- 229910001413 alkali metal ion Inorganic materials 0.000 description 2
- 238000000065 atmospheric pressure chemical ionisation Methods 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 238000000688 desorption electrospray ionisation Methods 0.000 description 2
- 239000000539 dimer Substances 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- 150000002170 ethers Chemical class 0.000 description 2
- 239000002828 fuel tank Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 150000002576 ketones Chemical class 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 239000003595 mist Substances 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 239000012086 standard solution Substances 0.000 description 2
- QNAYBMKLOCPYGJ-UHFFFAOYSA-N D-alpha-Ala Natural products CC([NH3+])C([O-])=O QNAYBMKLOCPYGJ-UHFFFAOYSA-N 0.000 description 1
- 239000007836 KH2PO4 Substances 0.000 description 1
- QNAYBMKLOCPYGJ-UWTATZPHSA-N L-Alanine Natural products C[C@@H](N)C(O)=O QNAYBMKLOCPYGJ-UWTATZPHSA-N 0.000 description 1
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229960003767 alanine Drugs 0.000 description 1
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000012491 analyte Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229960000956 coumarin Drugs 0.000 description 1
- 235000001671 coumarin Nutrition 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000002283 diesel fuel Substances 0.000 description 1
- 239000002552 dosage form Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 description 1
- 238000013467 fragmentation Methods 0.000 description 1
- 238000006062 fragmentation reaction Methods 0.000 description 1
- 239000003502 gasoline Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000005040 ion trap Methods 0.000 description 1
- 238000010884 ion-beam technique Methods 0.000 description 1
- 238000000816 matrix-assisted laser desorption--ionisation Methods 0.000 description 1
- 229910000402 monopotassium phosphate Inorganic materials 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- GNSKLFRGEWLPPA-UHFFFAOYSA-M potassium dihydrogen phosphate Chemical compound [K+].OP(O)([O-])=O GNSKLFRGEWLPPA-UHFFFAOYSA-M 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- IJDNQMDRQITEOD-UHFFFAOYSA-N sec-butylidene Natural products CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/0027—Methods for using particle spectrometers
- H01J49/0031—Step by step routines describing the use of the apparatus
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
- H01J49/04—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components
- H01J49/0431—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components for liquid samples
- H01J49/0445—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components for liquid samples with means for introducing as a spray, a jet or an aerosol
-
- 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
- H01J49/16—Ion sources; Ion guns using surface ionisation, e.g. field-, thermionic- or photo-emission
- H01J49/165—Electrospray ionisation
Landscapes
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Physics & Mathematics (AREA)
- Engineering & Computer Science (AREA)
- Plasma & Fusion (AREA)
- Dispersion Chemistry (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Electron Tubes For Measurement (AREA)
Abstract
The invention discloses a kind of flame assisted electrospray ionization apparatus and the methods for realizing ionization using the device, described device includes that can introduce the electron spray channel of sample to be tested, the outlet ends in the electron spray channel are located in front of the port of mass spectrum sample intake passage, flame generating device is equipped between the outlet ends in electron spray channel and the port of mass spectrum sample intake passage, the flame that the flame generating device generates is in contact or around the port of mass spectrum sample intake passage with the port of mass spectrum sample intake passage.Flame assisted electrospray ionization apparatus provided by the invention and method, the poly phenomenon of small molecule compound can not only be effectively reduced, and the interference of matrix reasons for its use signal can be effectively reduced, the interference of the cluster ion signal of solvent molecule generation can also be effectively reduced, the ionization of the compound of the small molecule compound easily polymerizeing, matrix complexity may be implemented, it is easy to operate, it is low in cost, it is easily achieved, universality is strong.
Description
Technical field
The present invention relates to a kind of flame assisted electrospray ionization apparatus and the methods for realizing ionization using the device, belong to
In analytical technique of mass spectrum field.
Background technique
Mass spectrum (MS) be it is a kind of can analyze complex mixture, provide related molecular weight information, element composition and analyte
The important tools of analysis of chemical structure, specificity and sensitivity with height.The basic principle of mass spectral analysis is made in sample
Each component ionizes in an ion source, generates the positively charged ion of different charge-mass ratios, and the effect of accelerated electric field is formed
Then in the mass analyser ion beam, recycles electric and magnetic fields to make that opposite speed color occurs into mass analyzer
It dissipates, they is focused respectively and obtains mass spectrogram, so that it is determined that its quality.Therefore, ionization techniques have mass spectrometry results
It has a major impact.In recent years, it constantly bringing forth new ideas and improving with ionization techniques and mass analyzer as compound is desorbed, mass spectrum
As one of most rapid analytical technology is developed, at present mass-spectrometric technique chemistry and chemical industry, biology and life science, medicine,
The fields such as pharmacy, material science, environmental protection using more and more extensive.
The common ioning method of mass spectrum mainly includes electrospray ionisation (ESI), atmospheric pressure chemical ionization (APCI) at present
With substance assistant laser desorpted ionized ionization (MALDI).Wherein electro-spray ionization technology (ESI) is from last century the seventies
Since appearance, the soft ionization characteristic that is not easy to cause fragmentation because of it, it has also become the most widely used ionization side in mass spectral analysis field
Method.And after the R.G.Cooks in the U.S. in 2004 professor research group develops desorption electrospray ionization technology (DESI), it opens
Open type ionization techniques are grown rapidly.It is this kind of that ionization techniques that sample is quickly directly analyzed may be implemented also because of its ion
The transformation in source is flexible and convenient and obtains development with rapid changepl. never-ending changes and improvements, thus for make up the deficiency of traditional ESI ion source provide it is a variety of
Possibility.
But there is also many defects for above-mentioned electron spray class ionization techniques, and such as: when there are salt etc. in sample to be tested
When complex matrices, ion depression effect is serious；In the higher concentration sample of the small molecule compounds such as analysis of amino acid, exist tight
The sample poly phenomenon of weight；When analyzing the sample solution of certain compounds, the small molecule solvent in sample solution is easy to produce
Cluster ion, impact analysis result.
Summary of the invention
In view of the above-mentioned problems existing in the prior art, the object of the present invention is to provide a kind of ionizations of flame assisted electrospray
Device and the method for realizing ionization using the device.
To solve the above problems, the present invention adopts the following technical scheme:
A kind of flame assisted electrospray ionization apparatus, the electron spray channel including sample to be tested can be introduced, the EFI
The outlet ends in mist channel are located in front of the port of mass spectrum sample intake passage, and the outlet ends and mass spectrum sample introduction in electron spray channel are logical
Flame generating device, the port phase of flame and mass spectrum sample intake passage that the flame generating device generates are equipped between the port in road
It contacts or around the port of mass spectrum sample intake passage.
Preferably, the angle between the axis in electron spray channel and the axis of mass spectrum sample intake passage is obtuse angle or 180
Degree.
Preferably, the distance between port of the outlet ends in electron spray channel and mass spectrum sample intake passage for 3~
15mm。
Preferably, electron spray channel is applied with the voltage of 2000~3800V.
Preferably, the distance between port of flame and mass spectrum sample intake passage is 0~8mm.
Preferably, the flame generating device includes fuel introduction passage, the outlet ends of fuel introduction passage
For flame ignition end, flame ignition end is located between the outlet ends in electron spray channel and the port of mass spectrum sample intake passage.
Preferably, the flame by inorganic fuel or organic-fuel burning generate, the inorganic fuel include but
It is not limited to hydrogen, the organic-fuel includes but is not limited to HC fuel, Aalcohols fuel, ketone fuel, ethers fuel or esters
Fuel, the HC fuel include but is not limited to saturated alkane class, unsaturated alkanes or are made of a variety of hydrocarbons
Mixture.
As further preferred scheme, the flame is generated by gas fuel combustion, the preferred hydrogen of gaseous fuel.
Preferably, heat-resisting material is selected at the flame ignition end, and the heat-resisting material includes but is not limited to
Glass, ceramics or metal material resistant to high temperature.
A method of it is realized and is ionized using above-mentioned flame assisted electrospray ionization apparatus, included the following steps:
A) testing sample solution is introduced into electron spray channel；
B) flame generating device is made to generate flame, make flame be in contact with the port of mass spectrum sample intake passage or positioned at mass spectrum into
Around the port in sample channel, the port of mass spectrum sample intake passage is burnt to red heat state by flame；
C) electron spray channel carries out electron spray to testing sample solution, and the sample for the atomization that electron spray is formed is transferred to matter
It composes the port of sample intake passage and desolventizing forms sample ions under the action of flame.
Preferably, the flow velocity of testing sample solution is 3~7 mul/min.
Preferably, flame and mass ions transmission pipe port distance are 0~8mm.
Preferably, the ionization voltage for carrying out electron spray is 2000~3800V.
Compared to the prior art, the beneficial technical effect of the present invention lies in:
Flame assisted electrospray ionization apparatus provided by the invention and method, when ionization, can not only be effectively reduced small point
The poly phenomenon of sub- compound, and the interference of matrix reasons for its use signal can be effectively reduced, moreover it is possible to solvent molecule is effectively reduced
The ionization of the compound of the small molecule compound easily polymerizeing, matrix complexity may be implemented in the interference of the cluster ion signal of generation,
It is easy to operate, it is low in cost, it is easy to accomplish, universality is strong, compared with the existing technology, has conspicuousness progress and practical value.
Detailed description of the invention
Fig. 1 is the schematic illustration of flame assisted electrospray ionization apparatus provided by the invention；
Fig. 2 is the L-threonine obtained in inventive embodiments 1 using flame assisted electrospray ionization apparatus of the invention
Mass spectral analysis figure；
Fig. 3 is in inventive embodiments 1 using the mass spectral analysis figure of the obtained L-threonine of traditional ESI；
Fig. 4 is to be added with sodium using what flame assisted electrospray ionization apparatus of the invention obtained in inventive embodiments 2
The mass spectral analysis figure of the cumarin of ion；
Fig. 5 is in inventive embodiments 2 using the mass spectral analysis of the obtained cumarin added with sodium ion of traditional ESI
Figure；
Fig. 6 is to be added with potassium using what flame assisted electrospray ionization apparatus of the invention obtained in inventive embodiments 3
The mass spectral analysis figure of the l-Alanine of ion；
Fig. 7 is in inventive embodiments 3 using the mass spectral analysis of the obtained l-Alanine added with potassium ion of traditional ESI
Figure；
Fig. 8 is molten for the Quercetin obtained in inventive embodiments 4 using flame assisted electrospray ionization apparatus of the invention
The mass spectral analysis figure of liquid；
Fig. 9 is in inventive embodiments 4 using the mass spectral analysis figure of the obtained Quercetin solution of traditional ESI；
Figure label is schematically as follows: 1, electron spray channel；2, mass spectrum sample intake passage；3, flame generating device；31, flame draws
Fire end；4, flame.
Specific embodiment
Technical solution of the present invention is described in further detail and completely with reference to the accompanying drawing.
A kind of flame assisted electrospray ionization apparatus provided by the invention as shown in Figure 1:, including sample to be tested can be introduced
Electron spray channel 1, the outlet ends in the electron spray channel 1 are located in front of the port of mass spectrum sample intake passage 2, logical in electron spray
Flame generating device 3 is equipped between the outlet ends in road 1 and the port of mass spectrum sample intake passage 2, the flame generating device 3 generates
Flame 4 be in contact with the port of mass spectrum sample intake passage 2 or around the port of mass spectrum sample intake passage 2.Electron spray channel 1
Axis and mass spectrum sample intake passage 2 axis between angle α be obtuse angle or 180 degree, α be 180 degree when, that is, represent electron spray channel
1 axis and the axis of mass spectrum sample intake passage 2 are located in same horizontal line.
Electron spray channel 1 described herein is using electron spray channel used in general electro-spray ionization technology
Can, including electron spray nozzle needle and high-voltage line (specific structure is identical as existing electro-spray ionization technology), this partly belongs to known
Technology, herein without being described in detail.Testing sample solution is introduced directly into electron spray channel 1, then through the ionization of electron spray channel 1 and mist
Change.In the application, electron spray channel 1 is applied with the voltage of 2000~3800V, and the HV in Fig. 1 is to represent the high tension voltage applied.
In the application, electron spray channel 1, mass spectrum sample intake passage 2, between 4 three of flame can with separated state, three it
Between mutual alignment it is adjustable.For example, between the outlet ends in electron spray channel 1 and the port of mass spectrum sample intake passage 2 away from
It is 3~15mm from d1.The distance between the port of flame 4 and mass spectrum sample intake passage 2 d2 is 0~8mm, d2 be 0 represent flame with
The port of mass spectrum sample intake passage 2 is in contact.
The flame generating device 3 includes fuel introduction passage, and the outlet ends of fuel introduction passage are flame ignition end
31, flame ignition end 31 is located between the outlet ends in electron spray channel 1 and the port of mass spectrum sample intake passage 2.When use,
Fuel is introduced in flame ignition end 31 by fuel introduction passage, is then ignited and generates flame 4.The flame 4 is by inorganic
Fuel or organic-fuel burning generate, and the inorganic fuel includes but is not limited to hydrogen, and the organic-fuel includes but is not limited to
HC fuel, Aalcohols fuel, ketone fuel, ethers fuel or esters fuel, the HC fuel include but is not limited to be saturated alkane
Hydro carbons, unsaturated alkanes or the mixture being made of a variety of hydrocarbons, preferably propane, normal butane, acetylene, gasoline or
Diesel oil.In the application, flame 4 is generated by gas fuel combustion, is further generated by combustion of hydrogen.
Heat-resisting material is selected at the flame ignition end 31, and the heat-resisting material includes but is not limited to glass resistant to high temperature
Glass, ceramics or metal material.
Flame assisted electrospray ionization apparatus of the present invention can be with common mass spectrograph (such as: triple quadrupole bar matter
Spectrometer, time of-flight mass spectrometer, ion trap mass spectrometer etc.) mutually it is compatible with, it can also promote the use of in other mass spectral analyses, be used for matter
When spectrum analysis, it is combined, has a wide range of application with common mass spectrograph, it is practical.
In addition, flame generating device 3 can be connected with fuel supply system (not shown), fuel supply system includes fuel tank
With fuel transmission pipe, when use, the fuel in fuel tank is transported to the combustion in flame generating device 3 through fuel transmission pipe
Expect finally to be transported to flame ignition end 31 in introduction passage and ignite.
The method that ionization is realized using flame assisted electrospray ionization apparatus of the present invention, including walk as follows
It is rapid:
A) testing sample solution is introduced into electron spray channel 1；
B) so that flame generating device 3 is generated flame 4, so that flame 4 is in contact with the port of mass spectrum sample intake passage 2 or positioned at matter
Around the port for composing sample intake passage 2, the port of mass spectrum sample intake passage 2 is burnt to red heat state by flame 4；
C) electron spray channel 1 carries out electron spray to testing sample solution, and the sample for the atomization that electron spray is formed is transferred to
The port of mass spectrum sample intake passage 2 and desolventizing formation sample ions under the action of flame 4.
The flow velocity of testing sample solution is 3~7 mul/min；Flame and mass ions transmission pipe port distance for 0~
8mm；The ionization voltage for carrying out electron spray is 2000~3800V.
Technical effect achieved by the present invention is further illustrated below with reference to concrete application embodiment.
Embodiment 1
Using flame assisted electrospray ionization apparatus of the present invention with mass spectrograph, (mass analyzer is triple quadrupole
Bar) to amino acid L-threonine (L-Thr)It is analyzed by mass spectrometry:
The sample to be tested that L-Thr is configured to 170ug/mL using the mixed solvent of methanol and water that volume ratio is 1:1 is molten
Liquid；Testing sample solution is introduced into electron spray channel 1 with the flow velocity of 3uL/min by peristaltic pump；Fuel (hydrogen) passes through fuel
Introduction passage is introduced in flame ignition end 31, lights, and generates flame 4, flame 4 is connected with the port of mass spectrum sample intake passage 2
It is located at around the port of mass spectrum sample intake passage 2 by touching, is burnt the port of mass spectrum sample intake passage 2 to red heat by flame 4
State；Electron spray channel 1 is powered on, voltage is made to be gradually increased to about 3000V, then the introducing of 1 pair of electron spray channel is to be measured
Sample solution carries out electron spray, and the sample for the atomization that electron spray is formed is transferred to the port of mass spectrum sample intake passage 2 and in port
Desolventizing forms sample ions under the action of the flame 4 at place；The sample ions of formation enter mass spectrum through mass spectrum sample intake passage 2
Subsequent mass spectral analysis is carried out, analysis result is as shown in Figure 2.In addition, at identical conditions, using traditional electron spray ion
Makeup is set (ESI) and is analyzed by mass spectrometry with mass spectrograph (mass analyzer is triple quadrupole bar) to L-threonine, and analysis result is such as
Shown in Fig. 3.
Fig. 2 is the matter of the L-threonine obtained in the present embodiment using flame assisted electrospray ionization apparatus of the invention
Spectrum analysis figure；Fig. 3 is in the present embodiment using the mass spectral analysis figure of the obtained L-threonine of traditional ESI；As it is clear from fig. 2 that spectrum
In figure other than quasi-molecular ions (m/z) 120 relevant to the compound, without the interference of other impurities quasi-molecular ions, and in spectrogram
Do not occur it is as shown in Figure 3 under the conditions of common ESI measure when the higher concentration amino acid sample will appear it is significant
Dimer, the quasi-molecular ions of polymer illustrate that small molecule can be effectively reduced using ionization apparatus of the present invention and method
The poly phenomenon for closing object amino acid realizes good ionising effect to the small molecule compound easily polymerizeing.
Embodiment 2
Using flame assisted electrospray ionization apparatus of the present invention with mass spectrograph, (mass analyzer is triple quadrupole
Bar) to the cumarin (Coumarin) for being added with sodium ionIt is analyzed by mass spectrometry:
Cumarin is configured to the solution of about 0.1ug/mL using the mixed solvent of methanol and water that volume ratio is 1:1, to
NaOH is wherein added, making the concentration of NaOH is about 0.05mmol/L, forms testing sample solution；By peristaltic pump by sample to be tested
Solution introduces electron spray channel 1 with the flow velocity of 3uL/min；Fuel (hydrogen) is introduced in flame ignition by fuel introduction passage
End 31, is lighted, and generates flame 4, flame 4 is in contact with the port of mass spectrum sample intake passage 2 or it is located at mass spectrum sample intake passage 2
Port around, the port of mass spectrum sample intake passage 2 is burnt to red heat state by flame 4；Electricity is connected into electron spray channel 1
Source makes voltage be gradually increased to about 3000V, and then the testing sample solution of the 1 pair of introducing in electron spray channel carries out electron spray, electron spray
Precipitation dosage form under the action of the sample of the atomization of formation is transferred to the port of mass spectrum sample intake passage 2 and flame 4 at port
At sample ions；The sample ions of formation can carry out subsequent mass spectral analysis, analysis knot into mass spectrum through mass spectrum sample intake passage 2
Fruit is as shown in Figure 4.In addition, at identical conditions, using traditional electro-spray ionization device (ESI) and mass spectrograph (quality
Analyzer is triple quadrupole bar) cumarin added with sodium ion is analyzed by mass spectrometry, analysis result is as shown in Figure 5.
Fig. 4 is to be added with sodium ion using what flame assisted electrospray ionization apparatus of the invention obtained in the present embodiment
Cumarin mass spectral analysis figure；Fig. 5 is in the present embodiment using the obtained cumarin added with sodium ion of traditional ESI
Mass spectral analysis figure；As seen from Figure 4, miscellaneous without other in spectrogram other than quasi-molecular ions (m/z) 147 relevant to the compound
The interference of matter quasi-molecular ions, and do not occur in spectrogram it is as shown in Figure 5 under the conditions of common ESI measure when sample molecule with added
The sodium salt added is formed plus sodium peak illustrates the presence that salt can be effectively reduced using ionization apparatus of the present invention and method
The phenomenon for adding alkali metal ion phenomenon serious is caused, matrix effect can be effectively reduced, the compound of matrix complexity is realized good
Ionising effect.
Embodiment 3
Using flame assisted electrospray ionization apparatus of the present invention with mass spectrograph, (mass analyzer is triple quadrupole
Bar) to the l-Alanine (L-Ala) for being added with potassium ionIt is analyzed by mass spectrometry:
L-Ala is configured to the solution of about 28ug/mL using the methanol of 1:1 and the mixed solvent of water, is added thereto
KH2PO4 makes salinity 0.07mmol/L, forms testing sample solution；By peristaltic pump by testing sample solution with 3uL/min
Flow velocity introduce electron spray channel 1；Fuel (hydrogen) is introduced in flame ignition end 31 by fuel introduction passage, lights, and produces
It lights a fire flame 4, flame 4 is in contact with the port of mass spectrum sample intake passage 2 or by the week of its port for being located at mass spectrum sample intake passage 2
It encloses, is burnt the port of mass spectrum sample intake passage 2 to red heat state by flame 4；Electron spray channel 1 is powered on, make voltage by
It edges up to about 3000V, then the testing sample solution of the 1 pair of introducing in electron spray channel carries out electron spray, the atomization that electron spray is formed
Sample under the action of be transferred to the port of mass spectrum sample intake passage 2 and flame 4 at port desolventizing form sample ions；
The sample ions of formation can carry out subsequent mass spectral analysis into mass spectrum through mass spectrum sample intake passage 2, analyze result such as Fig. 6 institute
Show.In addition, at identical conditions, using traditional electro-spray ionization device (ESI) and mass spectrograph (mass analyzer three
Weight quadrupole rod) l-Alanine added with potassium ion is analyzed by mass spectrometry, analysis result is as shown in Figure 7.
Fig. 6 is to be added with potassium ion using what flame assisted electrospray ionization apparatus of the invention obtained in the present embodiment
L-Alanine mass spectral analysis figure；Fig. 7 is the third ammonia of L- added with potassium ion obtained in the present embodiment using traditional ESI
The mass spectral analysis figure of acid；As seen from Figure 6, in spectrogram other than quasi-molecular ions (m/z) 90 relevant to the compound, without other
The interference at foreign ion peak, and do not occur in spectrogram it is as shown in Figure 7 under the conditions of common ESI measure when l-Alanine sample
The quasi-molecular ions for the significant dimer that will appear, at the same do not occur yet it is as shown in Figure 7 under the conditions of common ESI measure when sample
Product molecule and added sylvite are formed plus potassium peak, illustrating can be effective using ionization apparatus of the present invention and method
The poly phenomenon of small molecule compound amino acid is reduced, and the presence that can effectively reduce salt causes plus alkali metal ion is serious existing
As matrix effect can be effectively reduced, realize good ionising effect to the small molecule compound of easy polymerization and matrix complexity.
Embodiment 4
Using flame assisted electrospray ionization apparatus of the present invention with mass spectrograph, (mass analyzer is triple quadrupole
Bar) to Quercetin (Quercetin) standard solutionIt is analyzed by mass spectrometry:
Quercetin is configured to the testing sample solution of about 150ug/mL using the methanol of 1:1 and the mixed solvent of water；It is logical
It crosses peristaltic pump and testing sample solution is introduced into electron spray channel 1 with the flow velocity of 3uL/min；Fuel (hydrogen) is introduced logical by fuel
Road is introduced in flame ignition end 31, lights, and generates flame 4, and flame 4 is in contact or is incited somebody to action with the port of mass spectrum sample intake passage 2
Around its port for being located at mass spectrum sample intake passage 2, the port of mass spectrum sample intake passage 2 is burnt to red heat state by flame 4；It will
Electron spray channel 1 powers on, and voltage is made to be gradually increased to about 3000V, then the testing sample solution of the 1 pair of introducing in electron spray channel
Electron spray is carried out, the sample for the atomization that electron spray is formed is transferred to the port of mass spectrum sample intake passage 2 and the flame 4 at port
Under the action of desolventizing formed sample ions；The sample ions of formation can carry out through mass spectrum sample intake passage 2 into mass spectrum subsequent
Mass spectral analysis, analysis result it is as shown in Figure 8.In addition, at identical conditions, using traditional electro-spray ionization device
(ESI) Quercetin (Quercetin) standard solution is analyzed by mass spectrometry with mass spectrograph (mass analyzer is triple quadrupole bar),
It is as shown in Figure 9 to analyze result.
Fig. 8 is the Quercetin obtained in the present embodiment using flame assisted electrospray ionization apparatus of the invention
(Quercetin) mass spectral analysis figure；Fig. 9 is in the present embodiment using the obtained Quercetin (Quercetin) of traditional ESI
Mass spectral analysis figure；As seen from Figure 8, miscellaneous without other in spectrogram other than quasi-molecular ions (m/z) 301 relevant to the compound
The interference of matter quasi-molecular ions, and do not occur in spectrogram it is as shown in Figure 9 under the conditions of common ESI measure when low molecular weight region by
The interference for the cluster ion (m/z 60,75,92) that small molecule solvent generates illustrates to use device and method of the present invention can be with
The generation of solvent cluster ion in measurement system is effectively reduced.
In summary: using ionization apparatus and method of the invention, small molecule can not only be effectively reduced in when ionization
The poly phenomenon of object is closed, and the interference of matrix reasons for its use signal can be effectively reduced, moreover it is possible to solvent molecule generation be effectively reduced
Cluster ion signal interference, to the compound of the small molecule compound, matrix complexity that easily polymerize in traditional ESI measurement with good
Good ionising effect, has a wide range of application, and universality is strong, compared with the existing technology, has conspicuousness progress and practical value.
It is last it is necessarily pointed out that: the foregoing is merely the preferable specific embodiment of the present invention, but the present invention
Protection scope be not limited thereto, anyone skilled in the art in the technical scope disclosed by the present invention,
Any changes or substitutions that can be easily thought of, should be covered by the protection scope of the present invention.
Claims (10)
1. a kind of flame assisted electrospray ionization apparatus, the electron spray channel including sample to be tested can be introduced, the electron spray
The outlet ends in channel are located in front of the port of mass spectrum sample intake passage, it is characterised in that: electron spray channel outlet ends and
Flame generating device is equipped between the port of mass spectrum sample intake passage, the flame and mass spectrum sample introduction that the flame generating device generates are logical
The port in road is in contact or around the port of mass spectrum sample intake passage.
2. flame assisted electrospray ionization apparatus according to claim 1, it is characterised in that: the axis in electron spray channel
Angle between the axis of mass spectrum sample intake passage is obtuse angle or 180 degree.
3. flame assisted electrospray ionization apparatus according to claim 1, it is characterised in that: the outlet in electron spray channel
The distance between end and the port of mass spectrum sample intake passage are 3~15mm.
4. flame assisted electrospray ionization apparatus according to claim 1, it is characterised in that: electron spray channel is applied with
The voltage of 2000~3800V.
5. flame assisted electrospray ionization apparatus according to claim 1, it is characterised in that: flame and mass spectrum sample introduction are logical
The distance between the port in road is 0~8mm.
6. flame assisted electrospray ionization apparatus according to claim 1, it is characterised in that: the flame generating device
Including fuel introduction passage, the outlet ends of fuel introduction passage are flame ignition end, and flame ignition end is located at electron spray channel
Outlet ends and mass spectrum sample intake passage port between.
7. a kind of method for realizing ionization using flame assisted electrospray ionization apparatus described in claim 1, feature
It is, includes the following steps:
A) testing sample solution is introduced into electron spray channel；
B) so that flame generating device is generated flame, flame is made to be in contact with the port of mass spectrum sample intake passage or lead to positioned at mass spectrum sample introduction
Around the port in road, the port of mass spectrum sample intake passage is burnt to red heat state by flame；
C) electron spray channel to testing sample solution carry out electron spray, electron spray formed atomization sample be transferred to mass spectrum into
The port in sample channel and desolventizing formation sample ions under the action of flame.
8. according to the method described in claim 7, it is characterized by: the flow velocity of testing sample solution is 3~7 mul/min.
9. according to the method described in claim 7, it is characterized by: flame and mass ions transmission pipe port distance for 0~
8mm。
10. according to the method described in claim 7, it is characterized by: the ionization voltage for carrying out electron spray is 2000~3800V.
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