CN105355536A - Ionization method and ionization device - Google Patents
Ionization method and ionization device Download PDFInfo
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- CN105355536A CN105355536A CN201510730846.5A CN201510730846A CN105355536A CN 105355536 A CN105355536 A CN 105355536A CN 201510730846 A CN201510730846 A CN 201510730846A CN 105355536 A CN105355536 A CN 105355536A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
- G01N27/622—Ion mobility spectrometry
- G01N27/623—Ion mobility spectrometry combined with mass spectrometry
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- 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
- H01J49/18—Ion sources; Ion guns using spark ionisation
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/26—Mass spectrometers or separator tubes
Abstract
The invention discloses an ionization method and an ionization device. The ionization method comprises an ion source, a sample, and a mass spectrum feeding channel, and is characterized in that the ion source is a flame. By using a flame as an ion source, the ionization technology is easy to implement and simple in operation, the analysis cost is reduced greatly, the ionization technology is of high compatibility and can meet the ionization resolution temperature requirement of compounds of different molecular sizes, the ionization efficiency is high for gaseous, liquid and solid samples and actual samples, the ionization technology is of high sensitivity, actual samples can be analyzed directly, substances such as polar, highly polar, non-polar and metal organic compounds can be well ionized, and the ionization technology has a wide application range, can be used together with a portable mass spectrometry to make natural in-situ analysis more convenient and is of significant practical value.
Description
Technical field
The present invention relates to a kind of ioning method and device, belong to analytical technique of mass spectrum field.
Background technology
Mass spectrum (MS) is a kind of Analysis of Complex mixture, provides the strong tools of the chemical constitution about molecular information, weight and analyte.In recent years; along with constantly bringing forth new ideas and improvement of ionization techniques and mass analyzer; mass spectrum becomes development one of analytical technology the most rapidly, and current mass-spectrometric technique is more and more extensive with the application in the field such as chemical industry, biology and life science, medical science, pharmacy, material science, environmental protection at chemistry.
Common ioning method comprises the conventional substance assistant laser desorpted ionized ionization (MALDI) of electron spray ionisation (ESI), Atmosphere Pressure Chemical Ionization (APCI) (APCI) and solid.These ionization techniques above-mentioned belong to enclosed ionization techniques, adopt above-mentioned ionization techniques carry out mass spectral analysis before usually need to carry out pre-treatment to material, the mixture that such as some compositions are comparatively complicated needed to use chromatogram to be separated, with the impurity of trying one's best in minimizing mixture to the inhibition etc. of analyte ions usually before MS measures.
In recent years, without the need to complicated pre-treatment, realize Ionized mass-spectrometric technique under opening wide condition at sample primal environment, ion source and become the forward position in mass-spectrometric technique field and received much concern.Cooks in 2004 etc. develop desorption electrospray ionization technology (DESI) on the basis of ESI, RobertB.Cody in 2005 etc. develop Direct Analysis in Real Time ionization techniques (DART) on the basis of APCI, thus open the development of open type ionization techniques.This technology makes that the complex mixture without the need to sample preparation can realize (usually only needing a few second) fast, Direct Analysis.
In open type ionization techniques at present commercialization, DART compared to DESI, DART technology commercialization comparatively early, also comparatively ripe, the industry scope of application is more extensive.Although DART has operation need the advantages such as solvent fast, not, DART itself yet also exists some defects.The temperature adjusting range of such as DART is less, and usually at 50-550 DEG C, what therefore it can detect mostly is Small molecular, and some macromolecular compounds are not easily resolved; Meanwhile, DART adopts helium as ionized gas usually, and the cost of helium is very high, and this just makes analytical test cost very high, and the experimental provision of DART is very complicated simultaneously, and operation is also comparatively complicated.The appearance of DART and DESI opens the development of normal pressure open type ionization techniques.In in the past 10 years, tens kinds of novel Ionized mass-spectrometric techniques of normal pressure open type are developed in succession.These technology there has been application prospect widely in fields such as national public safety, medicine and pharmacy, original position and imaging analysis.Although these atmospheric pressure ionization methods simplify analytical procedure, these ioning methods still need the auxiliary of assist gas, laser, voltage etc., the analytical procedure of sample that this is just complicated.In order to widen the mass spectrographic range of application of normal pressure further, this area Kei need develop more portable, simple ioning method and device, to realize mass spectrum in-situ study anywhere or anytime.
Summary of the invention
The problems referred to above existed for prior art and demand, the object of this invention is to provide a kind of resolution temperature wider range, structure simple, easy and simple to handle, with low cost, be easy to the ioning method that realizes.
A kind of ioning method of the present invention, comprises ion source, sample and mass spectrum sample intake passage, it is characterized in that: described ion source is flame.
As a kind of execution mode, described sample is placed near flame or flame, and described flame is positioned at the port front of mass spectrum sample intake passage.
Preferably, the angle between the center line of described flame and the axis of mass spectrum sample intake passage is 5 ~ 355 degree.
Preferably, described sample is positioned on the axis of mass spectrum sample intake passage.
As further preferred version, the distance between described sample and flame is 0 ~ 80mm, and the distance between the port of described sample and mass spectrum sample intake passage is 1 ~ 80mm.
As a kind of execution mode, described flame is burnt by inorganic fuel or organic-fuel and produces.
Preferably, described flame is produced by any one burning in hydrogen, hydrocarbon fuel, Aalcohols fuel, ketone fuel, ethers fuel or ester class A fuel A.
Preferably, described flame is produced by hydrocarbon fuel combustion, the mixture that described hydrocarbon fuel comprises saturated alkane class, unsaturated alkanes and is made up of multiple hydrocarbon.
As further preferred version, described flame is produced by any one burning in propane, normal butane, acetylene, gasoline, diesel oil.
As a kind of execution mode, described sample is directly inserted in flame or near flame, such as: can by direct for gaseous sample disperse above flame or surrounding, or liquid sample is sprayed at top or the surrounding of flame, or solid sample is dissolved into solution spray above flame or surrounding, or solid sample is directly inserted in flame or near flame.
As another kind of execution mode, described sample is introduced in flame or near flame by bearing apparatus, such as: by gas compression utensil, gaseous sample is pressed in flame or near flame, or dip liquid sample by sample rod to insert in flame or near flame, or solid sample is dissolved into solution, by dropping liquid utensil instillation flame or near flame.
A kind of ionization apparatus, comprises ion source and mass spectrum sample intake passage, it is characterized in that: described ion source is flame.
As a kind of execution mode, described flame is positioned at the port front of mass spectrum sample intake passage.
Preferably, the distance between the center line of described flame and the port of mass spectrum sample intake passage is 1 ~ 80mm.
Preferably, the angle between the center line of described flame and the axis of mass spectrum sample intake passage is 5 ~ 355 degree.
As a kind of execution mode, described flame is connected with fuel supply system.
As a kind of execution mode, described fuel supply system comprises fuel storage tank and fuel transmission pipe.
Preferably, described fuel supply system also comprises fuel flow control valve.
As further preferred version, described fuel supply system also comprises fuel flow rate micro-adjustable valve.
Compared with prior art, the present invention has following conspicuousness beneficial effect:
1, compared with Direct Analysis in Real Time technology (DART) of the prior art, ionization techniques provided by the invention, by using flame as ion source, not only be easy to realize, simple to operate, greatly reduce analysis cost, and it is compatible strong, be applicable in various mass spectral analysis, have wide range of applications;
2, compared with Direct Analysis in Real Time technology (DART) of the prior art, the present invention only just need can realize by selecting the fuel be suitable for the flame that temperature range is 50 ~ 1500 degree, thus meet the ionization resolution temperature demand of the compound of different molecular weight size, can test sample object range extensive, applicability is strong;
3, in addition, experiment proves: adopt ionization techniques provided by the invention, to gaseous state, liquid state, solid sample and actual sample, all there is good Ionization Efficiency, not only highly sensitive, and Direct Analysis can be carried out to actual sample, and the ionization of the materials such as polarity, high polarity, nonpolar, metallo-organic compound can be realized well;
4, ionization techniques provided by the invention, can also be used in conjunction with portable mass spectrum, realize the in-situ study of nature more easily, have significant practicality.
Accompanying drawing explanation
Fig. 1 is the structural representation of a kind of ionization apparatus provided by the invention;
Fig. 2 is the structural representation of a kind of fuel supply system provided by the invention;
Fig. 3 is the mass spectral analysis figure of the embodiment of the present invention 1;
Fig. 4 is the mass spectral analysis figure of the embodiment of the present invention 2;
Fig. 5 is the mass spectral analysis figure of the embodiment of the present invention 3;
Fig. 6 is the mass spectral analysis figure of the embodiment of the present invention 4;
Fig. 7 is the mass spectral analysis figure of the embodiment of the present invention 5;
Fig. 8 is the mass spectral analysis figure of the embodiment of the present invention 6;
Fig. 9 is the mass spectral analysis figure of the embodiment of the present invention 7;
Figure 10 is the mass spectral analysis figure of the embodiment of the present invention 8;
Figure 11 is the mass spectral analysis figure of the embodiment of the present invention 9;
Figure 12 is the mass spectral analysis figure of the embodiment of the present invention 10;
Figure 13 is the mass spectral analysis figure of the embodiment of the present invention 11;
Figure 14 is the mass spectral analysis figure of the embodiment of the present invention 12;
Figure 15 is the mass spectral analysis figure of the embodiment of the present invention 13;
Figure 16 is the mass spectral analysis figure of the embodiment of the present invention 14;
Figure 17 is the mass spectral analysis figure of the embodiment of the present invention 15;
Figure 18 is the mass spectral analysis figure of the embodiment of the present invention 16;
Figure 19 is the mass spectral analysis figure of the embodiment of the present invention 17;
Figure 20 is the mass spectral analysis figure of the embodiment of the present invention 18;
Figure 21 is the mass spectral analysis figure of the embodiment of the present invention 19;
Figure 22 is the mass spectral analysis figure of the embodiment of the present invention 20;
Figure 23 is the mass spectral analysis figure of the embodiment of the present invention 21;
Figure 24 is the mass spectral analysis figure of the embodiment of the present invention 22;
Figure 25 is the mass spectral analysis figure of the embodiment of the present invention 23.
Number in the figure is schematically as follows:
1-flame; 2-mass spectrum sample intake passage; 3-sample; 4-fuel supply system; 41-fuel storage tank; 42-fuel transmission pipe; 43-fuel flow control valve; 44-fuel flow rate micro-adjustable valve; 5-sample rod.
Embodiment
Below in conjunction with embodiment and accompanying drawing, technical solution of the present invention is described in further detail and completely.
As shown in Figure 1: a kind of ionization apparatus provided by the invention, comprise as ionogenic flame 1 and mass spectrum sample intake passage 2, described flame 1 is positioned at the port front of mass spectrum sample intake passage 2.
Distance d between the center line of described flame 1 and the port of mass spectrum sample intake passage 2 is preferably 1 ~ 80mm, and with 1 ~ 30mm for the best, the angle α between the center line of described flame 1 and the axis of mass spectrum sample intake passage 2 can be 0 ~ 360 degree, is preferably 5 ~ 355 degree.
As shown in Figure 2: described flame 1 can be connected with fuel supply system 4, described fuel supply system 4 can comprise fuel storage tank 41 and fuel transmission pipe 42, fuel storage tank 41 is provided with fuel flow control valve 43, fuel transmission pipe 42 is provided with fuel flow rate micro-adjustable valve 44, to facilitate the size regulating flame.
Described flame 1 can be burnt by inorganic fuel or organic-fuel and produce, such as: inorganic fuel can select hydrogen etc., organic-fuel can select in the fuel such as hydrocarbon fuel, Aalcohols fuel, ketone fuel, ethers fuel or ester class A fuel A any one.
Preferably, described flame 1 is produced by hydrocarbon fuel combustion, the mixture that described hydrocarbon fuel comprises saturated alkane class, unsaturated alkanes and is made up of multiple hydrocarbon, wherein with propane, normal butane, acetylene, gasoline, diesel oil for the best.
See Fig. 1: will the sample 3 of mass spectral analysis be needed to be placed near flame 1 or flame, the material in band analytic sample can be made to produce ionization.
Preferably, described sample 3 is positioned on the axis of mass spectrum sample intake passage 2, and the distance h between flame is 0 ~ 80mm, and the distance L between the port of mass spectrum sample intake passage is 1 ~ 80mm.
Described sample 3 can directly be inserted in flame 1 or near flame 1, such as: can by direct for gaseous sample disperse above flame or surrounding, or liquid sample is sprayed at top or the surrounding of flame, or solid sample is dissolved into solution spray above flame or surrounding, or solid sample is directly inserted in flame or near flame; Described sample 3 also can be introduced in flame 1 or near flame 1 by bearing apparatus, such as: by gas compression utensil, gaseous sample is pressed in flame or near flame, or dip liquid sample by sample rod to insert in flame or near flame, or solid sample is dissolved into solution, by dropping liquid utensil instillation flame or near flame.
Core of the present invention is using flame as ion source, as long as the mutual alignment between flame 1, mass spectrum sample intake passage 2, sample 3 three in above-mentioned scope and handled easily.
The technique effect achieved by the present invention is further illustrated below in conjunction with embody rule embodiment:
Embodiment 1
Flame ion gasifying device shown in Fig. 1 is combined with mass spectrometer (mass analyzer is Fourier transform ion cyclotron resonance), liquid towards sample gaultherolin (Methylsalicylate, MW=152):
carry out mass spectral analysis:
Be fuel with normal butane, make it burn and produce flame 1;
Gaultherolin sample is sprayed at top or the surrounding of flame;
Keep fire endurance period burning, mass analyzer is in acquisition state always;
Fig. 3 is the mass spectrogram obtained, and mass spectrogram is as shown in Figure 3 visible: occurred the quasi-molecular ions [M+H] relevant to gaultherolin in spectrogram
+=153, illustrate and adopt apparatus and method of the present invention can realize good Ionization Efficiency.
Embodiment 2
Ionization apparatus shown in Fig. 1 is combined with mass spectrometer (mass analyzer is Fourier transform ion cyclotron resonance), liquid towards sample dimethyl sulfoxide (DMSO) (Dimethylsulfoxide, MW=78):
carry out mass spectral analysis:
Be fuel with normal butane, make it burn and produce flame 1;
The container open depositing dimethyl sulfoxide (DMSO) is placed near flame;
Keep fire endurance period burning, mass analyzer is in acquisition state always;
Fig. 4 is the mass spectrogram obtained, and mass spectrogram is as shown in Figure 4 visible: occurred the quasi-molecular ions [2M+H] relevant to dimethyl sulfoxide (DMSO) in spectrogram
+=157, illustrate and adopt apparatus and method of the present invention can realize good Ionization Efficiency.
Embodiment 3
Ionization apparatus shown in Fig. 1 is combined with mass spectrometer (mass analyzer is Fourier transform ion cyclotron resonance), liquid towards sample diethylene glycol dimethyl ether (2-Methoxyethylether, MW=134):
carry out mass spectral analysis:
Be fuel with normal butane, make it burn and produce flame 1;
The container open depositing diethylene glycol dimethyl ether is placed near flame;
Keep fire endurance period burning, mass analyzer is in acquisition state always;
Fig. 5 is the mass spectrogram obtained, and mass spectrogram is as shown in Figure 5 visible: occurred the quasi-molecular ions [M+H] relevant to diethylene glycol dimethyl ether in spectrogram
+=135, illustrate and adopt apparatus and method of the present invention can realize good Ionization Efficiency.
Embodiment 4
Ionization apparatus shown in Fig. 1 is combined, to azithromycin (Azithromycin, MW=748) tablet with mass spectrometer (mass analyzer is Fourier transform ion cyclotron resonance):
carry out mass spectral analysis:
Be fuel with normal butane, make it burn and produce flame 1;
Use ethanol by the testing sample solution of azithromycin tablet formulation into about 0.1mg/mL, be then sprayed in the top of flame or surrounding or instillation flame to insert after dipping with sample rod in flame or near;
Keep fire endurance period burning, mass analyzer is in acquisition state always;
Fig. 6 is the mass spectrogram obtained, and mass spectrogram is as shown in Figure 6 visible: occurred the quasi-molecular ions [M+H] relevant to azithromycin in spectrogram
+=749, illustrate and adopt apparatus and method of the present invention can realize good Ionization Efficiency.
Embodiment 5
Ionization apparatus shown in Fig. 1 is combined, to metronidazole (Metronidazole, MW=171) with mass spectrometer (mass analyzer is Fourier transform ion cyclotron resonance):
tablet carries out mass spectral analysis:
Be fuel with normal butane, make it burn and produce flame 1;
Use ethanol by the testing sample solution of metronidazole tablet formulation into about 0.1mg/mL, be then sprayed in the top of flame or surrounding or instillation flame to insert after dipping with sample rod in flame or near;
Keep fire endurance period burning, mass analyzer is in acquisition state always;
Fig. 7 is the mass spectrogram obtained, and mass spectrogram is as shown in Figure 6 visible: occurred the quasi-molecular ions [M+H] relevant to metronidazole in spectrogram
+=172, illustrate and adopt apparatus and method of the present invention can realize good Ionization Efficiency.
Embodiment 6
Combined with mass spectrometer (mass analyzer is Fourier transform ion cyclotron resonance) by ionization apparatus shown in Fig. 1, dialogue adds black powder and carries out mass spectral analysis:
Be fuel with normal butane, make it burn and produce flame 1;
Use ethanol by the testing sample solution of morning-night tablet formulation into about 0.1mg/mL, be then sprayed in the top of flame or surrounding or instillation flame to insert after dipping with sample rod in flame or near;
Keep fire endurance period burning, mass analyzer is in acquisition state always;
Fig. 8 is the mass spectrogram obtained, and mass spectrogram is as shown in Figure 8 visible: occurred the main component in morning-night tablet in spectrogram: the relevant ions peak [M+H] of paracetamol (A)
+=152, the relevant ions peak [M+H] of pseudoephedrine (B)
+=166, the relevant ions peak [M+H] of diphenhydramine (C)
+=256 and the relevant ions peak [M+H] of dextromethorphan (D)
+=272, illustrate and adopt apparatus and method of the present invention can realize good Ionization Efficiency.
Embodiment 7
Ionization apparatus shown in Fig. 1 is combined with mass spectrometer (mass analyzer is Fourier transform ion cyclotron resonance), mass spectral analysis is carried out to compound amino phenol tablet:
Be fuel with normal butane, make it burn and produce flame 1;
Use ethanol by the testing sample solution of compound amino phenol tablet formulation into about 0.1mg/mL, be then sprayed in the top of flame or surrounding or instillation flame to insert after dipping with sample rod in flame or near;
Keep fire endurance period burning, mass analyzer is in acquisition state always;
Fig. 9 is the mass spectrogram obtained, and mass spectrogram is as shown in Figure 9 visible: occurred the main component in compound amino phenol tablet in spectrogram: the relevant ions peak [M+H] of paracetamol (A)
+=152, the relevant ions peak [M+H] of caffeine (B)
+=195 and the relevant ions peak [M+H] of propyphenazone (C)
+=231, illustrate and adopt apparatus and method of the present invention can realize good Ionization Efficiency.
Embodiment 8
Ionization apparatus shown in Fig. 1 is combined with mass spectrometer (mass analyzer is Fourier transform ion cyclotron resonance), mass spectral analysis is carried out to apple skin:
Be fuel with normal butane, make it burn and produce flame 1;
Apple skin to be inserted in flame or near;
Keep fire endurance period burning, mass analyzer is in acquisition state always;
Figure 10 is the mass spectrogram obtained, and mass spectrogram is as shown in Figure 10 visible: occurred the main component in apple skin in spectrogram: the relevant ions peak [M+H] of imazalil
+=297, illustrate and adopt apparatus and method of the present invention can realize good Ionization Efficiency.
Embodiment 9
Ionization apparatus shown in Fig. 1 is combined with mass spectrometer (mass analyzer is Fourier transform ion cyclotron resonance), mass spectral analysis is carried out to pork:
Be fuel with normal butane, make it burn and produce flame 1;
Pork to be inserted in flame or near;
Keep fire endurance period burning, mass analyzer is in acquisition state always;
Figure 11 is the mass spectrogram obtained, and mass spectrogram is as shown in Figure 11 visible: occurred the main component in pork in spectrogram: the relevant ions peak [M+H] of diacylglycerol (A)
+=577 and the relevant ions peak [M+H] of triacylglycerol (B)
+=876, illustrate and adopt apparatus and method of the present invention can realize good Ionization Efficiency.
Embodiment 10
Ionization apparatus shown in Fig. 1 is combined with mass spectrometer (mass analyzer is Fourier transform ion cyclotron resonance), mass spectral analysis is carried out to garlic:
Be fuel with normal butane, make it burn and produce flame 1;
Garlic to be inserted in flame or near;
Keep fire endurance period burning, mass analyzer is in acquisition state always;
Figure 12 is the mass spectrogram obtained, and mass spectrogram is as shown in Figure 12 visible: occurred the main component in garlic in spectrogram: the relevant ions peak [M+H] of allicin (A)
+=163 and the relevant ions peak [M+NH of allicin ammonium salt (B)
4]
+=180, illustrate and adopt apparatus and method of the present invention can realize good Ionization Efficiency.
Embodiment 11
Ionization apparatus shown in Fig. 1 is combined, to diphenyl sulfoxide (Phenylsulfoxide, MW=202) with mass spectrometer (mass analyzer is Fourier transform ion cyclotron resonance):
carry out mass spectral analysis:
Be fuel with normal butane, make it burn and produce flame 1;
Use mixed solvent (V
h2O: V
cH3CN=1:1) by diphenyl sulfoxide preparation into about the testing sample solution of 0.1mg/mL, then drop in the top of flame or flame or to insert after dipping with sample rod in flame or near;
Keep fire endurance period burning, mass analyzer is in acquisition state always;
Figure 13 is the mass spectrogram obtained, and mass spectrogram is as shown in Figure 13 visible: occurred the quasi-molecular ions [M+H] relevant to described compound in spectrogram
+=203, illustrate and adopt apparatus and method of the present invention can realize good Ionization Efficiency.
Embodiment 12
Ionization apparatus shown in Fig. 1 is combined, to H-PHE-PHE-OH (MW=312) with mass spectrometer (mass analyzer is Fourier transform ion cyclotron resonance):
carry out mass spectral analysis:
Be fuel with normal butane, make it burn and produce flame 1;
Use mixed solvent (V
h2O: V
cH3CN=1:1) by the testing sample solution of sample preparation into about 0.1mg/mL, then drop in the top of flame or flame or to insert after dipping with sample rod in flame or near;
Keep fire endurance period burning, mass analyzer is in acquisition state always;
Figure 14 is the mass spectrogram obtained, and mass spectrogram is as shown in Figure 14 visible: occurred the quasi-molecular ions [M+H] relevant to described compound in spectrogram
+=313, illustrate and adopt apparatus and method of the present invention can realize good Ionization Efficiency.
Embodiment 13
Ionization apparatus shown in Fig. 1 is combined, to ferrocene (Ferrocene, MW=186) with mass spectrometer (mass analyzer is Fourier transform ion cyclotron resonance):
carry out mass spectral analysis:
Be fuel with normal butane, make it burn and produce flame 1;
Use mixed solvent (V
h2O: V
cH3CN=1:1) by the testing sample solution of sample preparation into about 0.1mg/mL, then drop in the top of flame or flame or to insert after dipping with sample rod in flame or near;
Keep fire endurance period burning, mass analyzer is in acquisition state always;
Figure 15 is the mass spectrogram obtained, and mass spectrogram is as shown in Figure 15 visible: occurred the quasi-molecular ions M relevant to described compound in spectrogram
+=186, illustrate and adopt apparatus and method of the present invention can realize good Ionization Efficiency.
Embodiment 14
Ionization apparatus shown in Fig. 1 is combined, to glycylalanine (H-ALA-GLY-OH, MW=146) with mass spectrometer (mass analyzer is Fourier transform ion cyclotron resonance):
carry out mass spectral analysis:
Be fuel with normal butane, make it burn and produce flame 1;
Use mixed solvent (V
h2O: V
cH3CN=1:1) by the testing sample solution of sample preparation into about 0.1mg/mL, then drop in the top of flame or flame or to insert after dipping with sample rod in flame or near;
Keep fire endurance period burning, mass analyzer is in acquisition state always;
Figure 16 is the mass spectrogram obtained, and mass spectrogram is as shown in Figure 16 visible: occurred the quasi-molecular ions [M+H] relevant to described compound in spectrogram
+=147, illustrate and adopt apparatus and method of the present invention can realize good Ionization Efficiency.
Embodiment 15
Ionization apparatus shown in Fig. 1 is combined, to anthracene (Anthracene, MW=178) with mass spectrometer (mass analyzer is Fourier transform ion cyclotron resonance):
carry out mass spectral analysis:
Be fuel with normal butane, make it burn and produce flame 1;
Use mixed solvent (V
h2O: V
cH3CN=1:1) by the testing sample solution of sample preparation into about 0.1mg/mL, then drop in the top of flame or flame or to insert after dipping with sample rod in flame or near;
Keep fire endurance period burning, mass analyzer is in acquisition state always;
Figure 17 is the mass spectrogram obtained, and mass spectrogram is as shown in Figure 17 visible: occurred the quasi-molecular ions M relevant to described compound in spectrogram
+=178, illustrate and adopt apparatus and method of the present invention can realize good Ionization Efficiency.
Embodiment 16
Ionization apparatus shown in Fig. 1 is combined with mass spectrometer (mass analyzer is Fourier transform ion cyclotron resonance), to the chloro-2-aminopurine (6-Chloroguanine, MW=169) of 6-:
carry out mass spectral analysis:
Be fuel with normal butane, make it burn and produce flame 1;
Use mixed solvent (V
h2O: V
cH3CN=1:1) by the testing sample solution of sample preparation into about 0.1mg/mL, then drop in the top of flame or flame or to insert after dipping with sample rod in flame or near;
Keep fire endurance period burning, mass analyzer is in acquisition state always;
Figure 18 is the mass spectrogram obtained, and mass spectrogram is as shown in Figure 18 visible: occurred the quasi-molecular ions [M+H] relevant to described compound in spectrogram
+=170, illustrate and adopt apparatus and method of the present invention can realize good Ionization Efficiency.
Embodiment 17
Ionization apparatus shown in Fig. 1 is combined, to Sudan red 1 (SudanI, MW=248) with mass spectrometer (mass analyzer is Fourier transform ion cyclotron resonance):
carry out mass spectral analysis:
Be fuel with normal butane, make it burn and produce flame 1;
Use mixed solvent (V
h2O: V
cH3CN=1:1) by the testing sample solution of sample preparation into about 0.1mg/mL, then drop in the top of flame or flame or to insert after dipping with sample rod in flame or near;
Keep fire endurance period burning, mass analyzer is in acquisition state always;
Figure 19 is the mass spectrogram obtained, and mass spectrogram is as shown in Figure 19 visible: occurred the quasi-molecular ions [M+H] relevant to described compound in spectrogram
+=249, illustrate and adopt apparatus and method of the present invention can realize good Ionization Efficiency.
Embodiment 18
Ionization apparatus shown in Fig. 1 is combined, to 5,6-dimethylbenzimidazole (5,6-Dimethylbenzimidazole, MW=146) with mass spectrometer (mass analyzer is Fourier transform ion cyclotron resonance):
carry out mass spectral analysis:
Be fuel with normal butane, make it burn and produce flame 1;
With sample rod directly pick sample to insert in flame or near;
Keep fire endurance period burning, mass analyzer is in acquisition state always;
Figure 20 is the mass spectrogram obtained, and mass spectrogram is as shown in Figure 20 visible: occurred the quasi-molecular ions [M+H] relevant to described compound in spectrogram
+=147, illustrate and adopt apparatus and method of the present invention can realize good Ionization Efficiency.
Embodiment 19
Ionization apparatus shown in Fig. 1 is combined with mass spectrometer (mass analyzer is Fourier transform ion cyclotron resonance), to the chloro-2-aminopurine (6-Chloroguanine, MW=169) of 6-:
carry out mass spectral analysis:
Be fuel with ether, make it burn and produce flame 1;
Use mixed solvent (V
h2O: V
cH3CN=1:1) by the testing sample solution of sample preparation into about 0.1mg/mL, then drop in the top of flame or flame or to insert after dipping with sample rod in flame or near;
Keep fire endurance period burning, mass analyzer is in acquisition state always;
Figure 21 is the mass spectrogram obtained, the mass spectrogram from shown in Figure 21: occurred the quasi-molecular ions [M+H] relevant to described compound in spectrogram
+=170, illustrate and adopt apparatus and method of the present invention can realize good Ionization Efficiency.
Embodiment 20
Ionization apparatus shown in Fig. 1 is combined with mass spectrometer (mass analyzer is Fourier transform ion cyclotron resonance) ,-6-ether is preced with to 18-:
(m/z=264) mass spectral analysis is carried out:
Be fuel with hydrogen, make it burn and produce flame 1;
Use mixed solvent (V
h2O: V
cH3CN=1:1) by the testing sample solution of sample preparation into about 0.1mg/mL, then drop in the top of flame or flame or to insert after dipping with sample rod in flame or near;
Keep fire endurance period burning, mass analyzer is in acquisition state always;
Figure 22 is the mass spectrogram obtained, the mass spectrogram from shown in Figure 22: occurred the quasi-molecular ions [M+Na] relevant to described compound in spectrogram
+=287 and [M+K]
+=303, illustrate and adopt apparatus and method of the present invention can realize good Ionization Efficiency.
Embodiment 21
Ionization apparatus shown in Fig. 1 is combined, to diphenyl sulfoxide with mass spectrometer (mass analyzer is Fourier transform ion cyclotron resonance):
(m/z=202) mass spectral analysis is carried out:
Be fuel with ethanol, make it burn and produce flame 1;
Use mixed solvent (V
h2O: V
cH3CN=1:1) by the testing sample solution of sample preparation into about 0.1mg/mL, then drop in the top of flame or flame or to insert after dipping with sample rod in flame or near;
Keep fire endurance period burning, mass analyzer is in acquisition state always;
Figure 23 is the mass spectrogram obtained, the mass spectrogram from shown in Figure 23: occurred the quasi-molecular ions [M+H] relevant to described compound in spectrogram
+=203, illustrate and adopt apparatus and method of the present invention can realize good Ionization Efficiency.
Embodiment 22
Ionization apparatus shown in Fig. 1 is combined, to 3-aminoquinoline with mass spectrometer (mass analyzer is Fourier transform ion cyclotron resonance):
(m/z=144) mass spectral analysis is carried out:
Be fuel with acetone, make it burn and produce flame 1;
Use mixed solvent (V
h2O: V
cH3CN=1:1) by the testing sample solution of sample preparation into about 0.1mg/mL, then drop in the top of flame or flame or to insert after dipping with sample rod in flame or near;
Keep fire endurance period burning, mass analyzer is in acquisition state always;
Figure 24 is the mass spectrogram obtained, the mass spectrogram from shown in Figure 24: occurred the quasi-molecular ions [M+H] relevant to described compound in spectrogram
+=145, illustrate and adopt apparatus and method of the present invention can realize good Ionization Efficiency.
Embodiment 23
Ionization apparatus shown in Fig. 1 is combined, to melamine with mass spectrometer (mass analyzer is Fourier transform ion cyclotron resonance):
(m/z=126) mass spectral analysis is carried out:
Be fuel with ethyl acetate, make it burn and produce flame 1;
Use mixed solvent (V
h2O: V
cH3CN=1:1) by the testing sample solution of sample preparation into about 0.1mg/mL, then drop in the top of flame or flame or to insert after dipping with sample rod in flame or near;
Keep fire endurance period burning, mass analyzer is in acquisition state always;
Figure 25 is the mass spectrogram obtained, the mass spectrogram from shown in Figure 25: occurred the quasi-molecular ions [M+H] relevant to described compound in spectrogram
+=127, illustrate and adopt apparatus and method of the present invention can realize good Ionization Efficiency.
To sum up experiment is visible: ionization techniques of the present invention, by using flame as ion source, be not only easy to realize, simple to operate, greatly reduce analysis cost, and compatible by force, be applicable in various mass spectral analysis, have wide range of applications, compared with Direct Analysis in Real Time technology (DART) of the prior art, the present invention only just need can realize by selecting the fuel be suitable for the flame that temperature range is 50 ~ 1500 degree, thus meet the ionization resolution temperature demand of the compound of different molecular weight size, can to gaseous state, liquid, solid sample and actual sample all have good Ionization Efficiency, not only highly sensitive, and Direct Analysis can be carried out to actual sample, and polarity can be realized well, high polarity, nonpolar, the ionization of the materials such as metallo-organic compound, not only there is test sample object range extensive, and can be used in conjunction with portable mass spectrum, realize the in-situ study of nature more easily, there is conspicuousness progress and practicality.
Finally need described herein: above content is only for being described in more detail technical scheme of the present invention; can not be interpreted as limiting the scope of the invention, some nonessential improvement that those skilled in the art's foregoing according to the present invention is made and adjustment all belong to protection scope of the present invention.
Claims (18)
1. an ioning method, comprises ion source, sample and mass spectrum sample intake passage, it is characterized in that: described ion source is flame.
2. ioning method according to claim 1, is characterized in that: described flame is burnt by inorganic fuel or organic-fuel and produces.
3. ioning method according to claim 2, is characterized in that: described flame is produced by any one burning in hydrogen, hydrocarbon fuel, Aalcohols fuel, ketone fuel, ethers fuel or ester class A fuel A.
4. ioning method according to claim 3, is characterized in that: described flame is produced by hydrocarbon fuel combustion, the mixture that described hydrocarbon fuel comprises saturated alkane class, unsaturated alkanes and is made up of multiple hydrocarbon.
5. ioning method according to claim 1, is characterized in that: described sample is placed near flame or flame, and described flame is positioned at the port front of mass spectrum sample intake passage.
6. ioning method according to claim 5, is characterized in that: described sample is positioned on the axis of mass spectrum sample intake passage.
7. ioning method according to claim 6, is characterized in that: the distance between described sample and flame is 0 ~ 80mm, and the distance between the port of described sample and mass spectrum sample intake passage is 1 ~ 80mm.
8. the ioning method according to claim 5 or 7, is characterized in that: the angle between the center line of described flame and the axis of mass spectrum sample intake passage is 5 ~ 355 degree.
9. ioning method according to claim 5, is characterized in that: described sample is directly inserted in flame or near flame.
10. ioning method according to claim 5, is characterized in that: described sample is introduced in flame or near flame by bearing apparatus.
11. 1 kinds of ionization apparatus, comprise ion source and mass spectrum sample intake passage, it is characterized in that: described ion source is flame.
12. ionization apparatus according to claim 11, is characterized in that: described flame is positioned at the port front of mass spectrum sample intake passage.
13. ionization apparatus according to claim 12, is characterized in that: the distance between the center line of described flame and the port of mass spectrum sample intake passage is 1 ~ 80mm.
14. ionization apparatus according to claim 12 or 13, is characterized in that: the angle between the center line of described flame and the axis of mass spectrum sample intake passage is 5 ~ 355 degree.
15. ionization apparatus according to claim 11, is characterized in that: described flame is connected with fuel supply system.
16. ionization apparatus according to claim 15, is characterized in that: described fuel supply system comprises fuel storage tank and fuel transmission pipe.
17. ionization apparatus according to claim 16, is characterized in that: described fuel supply system also comprises fuel flow control valve.
18. ionization apparatus according to claim 17, is characterized in that: described fuel supply system also comprises fuel flow rate micro-adjustable valve.
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| PCT/CN2015/094079 WO2017016099A1 (en) | 2015-07-24 | 2015-11-08 | Ionization method and device |
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|---|---|---|---|---|
| CN105845540A (en) * | 2016-03-28 | 2016-08-10 | 复旦大学 | Desolvation and ionizationoun method through heating and apparatus |
| CN106680361A (en) * | 2017-03-28 | 2017-05-17 | 中国科学院上海有机化学研究所 | Temperature-adjustable opening type flame ionizing device |
| CN110364412A (en) * | 2019-07-23 | 2019-10-22 | 中国科学院上海有机化学研究所 | A kind of flame assisted electrospray ionization apparatus and the method using device realization ionization |
| CN110400740A (en) * | 2019-07-23 | 2019-11-01 | 中国科学院上海有机化学研究所 | A kind of method and apparatus using solvent and gas double auxiliary flame direct ion sample |
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| CN105355536B (en) * | 2015-07-24 | 2017-12-19 | 中国科学院上海有机化学研究所 | A kind of ioning method and device |
| CN113514529B (en) * | 2020-04-09 | 2022-11-11 | 湖南中烟工业有限责任公司 | Method for rapidly detecting photoinitiator in cigarette paper |
| CN112730574B (en) * | 2020-12-15 | 2024-03-29 | 兰州海关技术中心 | Method for rapidly and high-throughput detecting aldicarb, aldicarb sulfoxide and aldicarb sulfone in environmental water body |
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| CN106680361A (en) * | 2017-03-28 | 2017-05-17 | 中国科学院上海有机化学研究所 | Temperature-adjustable opening type flame ionizing device |
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| CN110364412A (en) * | 2019-07-23 | 2019-10-22 | 中国科学院上海有机化学研究所 | A kind of flame assisted electrospray ionization apparatus and the method using device realization ionization |
| CN110400740A (en) * | 2019-07-23 | 2019-11-01 | 中国科学院上海有机化学研究所 | A kind of method and apparatus using solvent and gas double auxiliary flame direct ion sample |
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| CN105355536B (en) | 2017-12-19 |
| CN205122534U (en) | 2016-03-30 |
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