CN205122534U - Ionizationoun device - Google Patents
Ionizationoun device Download PDFInfo
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- CN205122534U CN205122534U CN201520861732.XU CN201520861732U CN205122534U CN 205122534 U CN205122534 U CN 205122534U CN 201520861732 U CN201520861732 U CN 201520861732U CN 205122534 U CN205122534 U CN 205122534U
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- XSUVPVMIJYRTKI-IPYMFYIGSA-N C/C(/NC=C)=C(\C(\Cl)=N/C(N)=C)/N Chemical compound C/C(/NC=C)=C(\C(\Cl)=N/C(N)=C)/N XSUVPVMIJYRTKI-IPYMFYIGSA-N 0.000 description 1
- CRMOZBYBHBKJJM-UHFFFAOYSA-N COC(C1=CC=CCC1O)=O Chemical compound COC(C1=CC=CCC1O)=O CRMOZBYBHBKJJM-UHFFFAOYSA-N 0.000 description 1
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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
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Abstract
The utility model discloses an ionizationoun device, the device advances a kind passageway including ion source and mass spectrum, its characterized in that: the ion source is flame. Ionizationoun device, through using flame as the ion source, not only easily realize, the operation is thus simple, the the analysis cost is greatly reduced, and it is compatible strong, can satisfy the analytic temperature demand of ionizationoun of the compound of different molecular weight size, and can be to the gaseous state, it is liquid, gu aspect article and actual sample standard deviation have good ionizationoun efficiency, not only sensitivity is high, and can carry out the direct analysis to actual sample, and can realize polarity well, high polarity, it is nonpolar, the ionizationoun of materials such as metal organic compound, wide range of application, and can use together with portable mass spectrum, realize more convenient natural state's normal position analysis, apparent practical value has.
Description
Technical field
The utility model relates to a kind of ionization apparatus, belongs 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 ionization techniques, to realize mass spectrum in-situ study anywhere or anytime.
Utility model content
The problems referred to above existed for prior art and demand, the purpose of this utility model be to provide a kind of resolution temperature wider range, structure simple, easy and simple to handle, with low cost, be easy to the ionization apparatus that realizes.
A kind of ionization apparatus described in the utility model, 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 flow control valve is arranged on fuel storage tank.
As further preferred version, described fuel supply system also comprises fuel flow rate micro-adjustable valve.
As further preferred version, described fuel flow rate micro-adjustable valve is arranged on fuel transmission pipe.
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.
By directly being inserted by sample to be analyzed in flame or near flame or by bearing apparatus introducing flame or near flame, in the burning of maintenance fire endurance period, under mass analyzer is in acquisition state always, ionization and the mass spectral analysis of material to be analyzed can be realized.
Compared with prior art, the utility model has following conspicuousness beneficial effect:
1, compared with Direct Analysis in Real Time technology (DART) of the prior art, the ionization apparatus that the utility model provides, 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 utility model 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 the ionization apparatus that the utility model provides, 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, the ionization apparatus that provides of the utility model, 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
The structural representation of a kind of ionization apparatus that Fig. 1 provides for the utility model;
The structural representation of a kind of fuel supply system that Fig. 2 provides for the utility model;
Fig. 3 is the mass spectral analysis figure of the utility model embodiment 1;
Fig. 4 is the mass spectral analysis figure of the utility model embodiment 2;
Fig. 5 is the mass spectral analysis figure of the utility model embodiment 3;
Fig. 6 is the mass spectral analysis figure of the utility model embodiment 4;
Fig. 7 is the mass spectral analysis figure of the utility model embodiment 5;
Fig. 8 is the mass spectral analysis figure of the utility model embodiment 6;
Fig. 9 is the mass spectral analysis figure of the utility model embodiment 7;
Figure 10 is the mass spectral analysis figure of the utility model embodiment 8;
Figure 11 is the mass spectral analysis figure of the utility model embodiment 9;
Figure 12 is the mass spectral analysis figure of the utility model embodiment 10;
Figure 13 is the mass spectral analysis figure of the utility model embodiment 11;
Figure 14 is the mass spectral analysis figure of the utility model embodiment 12;
Figure 15 is the mass spectral analysis figure of the utility model embodiment 13;
Figure 16 is the mass spectral analysis figure of the utility model embodiment 14;
Figure 17 is the mass spectral analysis figure of the utility model embodiment 15;
Figure 18 is the mass spectral analysis figure of the utility model embodiment 16;
Figure 19 is the mass spectral analysis figure of the utility model embodiment 17;
Figure 20 is the mass spectral analysis figure of the utility model embodiment 18;
Figure 21 is the mass spectral analysis figure of the utility model embodiment 19;
Figure 22 is the mass spectral analysis figure of the utility model embodiment 20;
Figure 23 is the mass spectral analysis figure of the utility model embodiment 21;
Figure 24 is the mass spectral analysis figure of the utility model embodiment 22;
Figure 25 is the mass spectral analysis figure of the utility model embodiment 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 solutions of the utility model are described in further detail and completely.
As shown in Figure 1: a kind of ionization apparatus that the utility model provides, 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 utility model 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 utility model is further illustrated below in conjunction with embody rule embodiment:
Embodiment 1
Ionization apparatus 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 described in the utility model 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 described in the utility model 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 described in the utility model 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 described in the utility model 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 described in the utility model 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 described in the utility model 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 described in the utility model 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 described in the utility model 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 described in the utility model 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 described in the utility model 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 described in the utility model 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 described in the utility model 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 described in the utility model 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 described in the utility model 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 described in the utility model 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 described in the utility model 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 described in the utility model 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 described in the utility model 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 described in the utility model 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 described in the utility model 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 described in the utility model 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 described in the utility model 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):
carry out mass spectral analysis:
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 described in the utility model can realize good Ionization Efficiency.
To sum up experiment is visible: ionization apparatus described in the utility model, 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 utility model 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 the technical solution of the utility model; can not be interpreted as the restriction to the utility model protection range, some nonessential improvement that those skilled in the art makes according to foregoing of the present utility model and adjustment all belong to protection range of the present utility model.
Claims (7)
1. an ionization apparatus, comprise ion source and mass spectrum sample intake passage, it is characterized in that: described ion source is flame, described flame is positioned at the port front of mass spectrum sample intake passage, distance between the center line of described flame and the port of mass spectrum sample intake passage is 1 ~ 80mm, and the angle between the center line of described flame and the axis of mass spectrum sample intake passage is 5 ~ 355 degree.
2. ionization apparatus according to claim 1, is characterized in that: described flame is connected with fuel supply system.
3. ionization apparatus according to claim 2, is characterized in that: described fuel supply system comprises fuel storage tank and fuel transmission pipe.
4. ionization apparatus according to claim 3, is characterized in that: described fuel supply system also comprises fuel flow control valve.
5. ionization apparatus according to claim 4, is characterized in that: described fuel flow control valve is arranged on fuel storage tank.
6. ionization apparatus according to claim 3, is characterized in that: described fuel supply system also comprises fuel flow rate micro-adjustable valve.
7. ionization apparatus according to claim 6, is characterized in that: described fuel flow rate micro-adjustable valve is arranged on fuel transmission pipe.
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CN105355536A (en) * | 2015-07-24 | 2016-02-24 | 中国科学院上海有机化学研究所 | Ionization method and ionization device |
CN113514529A (en) * | 2020-04-09 | 2021-10-19 | 湖南中烟工业有限责任公司 | Method for rapidly detecting photoinitiator in cigarette paper |
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CN106680361B (en) * | 2017-03-28 | 2023-05-12 | 中国科学院上海有机化学研究所 | Temperature-adjustable open flame ionization 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 |
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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CN101587038B (en) * | 2009-06-26 | 2011-07-20 | 中国科学院合肥物质科学研究院 | Liquid sample desorption ionization method under atmospheric pressure |
CN202256256U (en) * | 2011-09-20 | 2012-05-30 | 卓东玲 | Novel flame ionization detector |
CN203882953U (en) * | 2014-01-28 | 2014-10-15 | 北京普析通用仪器有限责任公司 | Mass spectrometer and ionization device thereof |
CN204789463U (en) * | 2015-07-24 | 2015-11-18 | 中国科学院上海有机化学研究所 | Open -type flame ionizationoun device |
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CN105355536A (en) * | 2015-07-24 | 2016-02-24 | 中国科学院上海有机化学研究所 | Ionization method and ionization device |
CN113514529A (en) * | 2020-04-09 | 2021-10-19 | 湖南中烟工业有限责任公司 | Method for rapidly detecting photoinitiator in cigarette paper |
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 |
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