CN203300594U - Microwave plasma normal pressure desorption ion source and ion source device constituted thereby - Google Patents
Microwave plasma normal pressure desorption ion source and ion source device constituted thereby Download PDFInfo
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- CN203300594U CN203300594U CN2013201949486U CN201320194948U CN203300594U CN 203300594 U CN203300594 U CN 203300594U CN 2013201949486 U CN2013201949486 U CN 2013201949486U CN 201320194948 U CN201320194948 U CN 201320194948U CN 203300594 U CN203300594 U CN 203300594U
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Abstract
The utility model discloses a microwave plasma normal pressure desorption ion source and an ion source device constituted thereby. The ion source mainly includes a basic member designed with a cylindrical tube, a tubular main adjustment member arranged in the cylindrical tube of the basic member and used for adjusting microwave coupling, a gas discharge tube arranged in the cylindrical tube of the basic member, and a microwave antenna arranged outside the gas discharge tube and used for applying microwave coupling to discharging gas in the discharge tube. An ion source device of a normal pressure desorption mass spectrometer is constituted by the ion source. A sample to be tested is subjected to microwave plasma normal pressure desorption mass spectrometry analysis. The microwave plasma normal pressure desorption ion source has the advantages of small power required, small amount of gas required, no toxic reagents, relatively high plasma temperature, no pollution to environment, easiness in operation and the like.
Description
Technical field
The utility model belongs to normal pressure Ionization Techniques In Mass Spectrometry field, and particularly a kind of maldi ion source of normal pressure based on microwave plasma reaches the ion source device by its normal pressure maldi mass spectrometer analyzer that forms.
Background technology
Mass spectrum has its significant advantage as a kind of spectrum method, namely highly sensitive, analysis speed is fast, selectivity good, can be used for stoichiometry etc., thereby mass spectrometric analysis method be widely used in medicine synthetic with the fields such as analysis, forensic science, food security, petrochemical industry, environmental science.No matter molecule mass spectrum or atom mass spectrum, the basic structure of instrument all is comprised of sampling system, ion source, mass analyzer, detector, vacuum system and computer control system and data handling system.The wherein sensitivity of ion source and sample analysis, detect existence and contact directly.Traditional ion source that is used for Analysis of Organic Substances mainly contains electron bombardment ionization source, chemical ionization source, field desorption ionization source, fast atom bombardment source, laser desorption ionisation source.Utilize these traditional ion sources to carry out the sample mass spectral analysis, all need sample is carried out long preliminary treatment and strict vacuum pre-treatment condition.The deficiency that exists in order to solve conventional ion source mass spectrometric analysis method, people have developed the normal pressure Ionization Techniques In Mass Spectrometry, and normal pressure Ionization Techniques In Mass Spectrometry development in recent years rapidly.
The normal pressure Ionization Techniques In Mass Spectrometry starts from the people's such as R.G.Cooks in 2004 electron spray desorption ionization techniques (Desorption Electrospray Ionization DESI) and the people's such as R.B.Cody in 2005 direct real-time analysis ionization technique (Direct Analysis in Real Time DART).These technology need not sample treatment, can directly to sample, carry out sample analysis fast and accurately.This type of normal pressure mass ion source occurs it being a quantum leap progress of field of mass spectrometry.the normal pressure Ionization Techniques In Mass Spectrometry that occurred in recent years has desorption atmospheric chemical ionization (Desorption Atmospheric Pressure Chemical Ionization DAPCI), dielectric barrier discharge ionization (Dielectric Discharge Barrier Desorption/Ionization DBDI), extraction electron spray ionisation (Extractive Electrospray Ionization EESI), plasmaassisted laser desorption ionisation (Plasma-Assisted Desorption/Ionization PADI), electron spray laser desorption ionisation (Electrospray Laser Desorption/Ionization ELDI), laser ablation electron spray ionisation (Laser Ablation Electrospray Ionization LAESI), normal pressure solid analysis probe (Ambient Solid Analysis Probe ASAP) etc.
The DESI technology adopts corona discharge directly solid sample to be carried out desorption ionization, belongs to the soft ionization mode.Its mechanism is that specific solvent forms spraying under electric field action, and spraying is dissolved, extracted with the solid body surface, wherein relates to the processes such as momentum transfer, Coulomb repulsion.Ensuing ionization mechanism similar to the mechanism in ESI (ion evaporation mechanism or charged residue mechanism).The ionic species of observing and sample, matrix, solvent are relevant.Be mainly used in measuring the compound of middle polarity and strong polarity.Can reach optimum experiment condition by regulating solvent flux, sample panel material, capillary temperature etc. in experiment.DESI is widely used in explosive detection, metabolite analysis, medicine is synthetic and the fields such as detection, environmental science.But this technology required voltage is high, spraying reagent may be to environment, and because the generation of the generation of polymer, sample partial solvent, multiple-charged ion etc. causes its mass spectrogram complicated.
The DART technology also adopts corona discharge to carry out desorption ionization to sample, and what be different from DESI is that carrier that its utilizes is gas but not solution generally adopts helium or nitrogen.Gas produces active component by corona discharge, and the high energy metastable atom carries out desorption ionization as main active to determinand.The DART technology can detect different compounds on the surface of various detected objects, and comprising: medicine, food, spices, blood of human body, saliva, urine be some inorganic matters even.And the DART source is to the particular location of sample, and namely sample and mass spectrometric distance, angle etc. are all insensitive.Be applicable to the detection of solid-state, gaseous state, liquid sample.But need extra heater, complex structure, expensive.
, though other atmospheric pressure ionization know-whies are incomplete same with DESI, DART, also all mainly comprise desorb and two processes of ionization.Its process that produces ion roughly can be summarized as: certain energy source (electric field, heat energy, metastable particle etc.) acts on the upper electrified body with certain energy that forms of specific support (gas, reagent), and this electrified body and sample effect, make its ionization.Although these ionization techniques all have important application in every field, all there is certain limitation, therefore, develop new ion source the development of normal pressure Ionization Techniques In Mass Spectrometry is of great importance.
Summary of the invention
Present situation and deficiency for existing normal pressure Ionization Techniques In Mass Spectrometry, the purpose of this utility model aims to provide a kind of maldi ion source of normal pressure based on microwave plasma and by its ion source device that is used for mass spectrometer that forms, the problem that exists to solve prior art.
the maldi ion source of the normal pressure based on microwave plasma that the utility model provides, its formation comprises the base member that is designed with the cylinder tube chamber, be arranged on the tubular structure main regulation part that is used for regulating microwave coupling in base member cylinder tube chamber, be arranged on the intraluminal gas discharge tube of main regulation part and be arranged on gas discharge tube and be used for microwave coupling is applied to the microwave antenna of discharge gas in discharge tube outward, is designed with the installing hole that gas discharge tube therefrom passes at the bottom of the chamber of described base member cylinder tube chamber, described main regulation part is designed with the ring plug dish that is slidably matched with the base member lumen wall, be slidably mounted in the base member tube chamber by the strutting piece that is fixed on base member, be designed with adjustment structure between supporting member and main regulation part, by adjustment structure with the ring plug dish of main regulation part and base member chamber at the bottom of between be used for chamber length that ripple forms and be adjusted into the odd-multiple of 1/4 wavelength, so that microwave reflection power is minimum, described gas discharge tube is the insulated tube of inorganic, input is connected with the discharge gas source, installing hole on output passes at the bottom of the base member chamber, on the gas discharge tube of the male part of described microwave antenna between at the bottom of main regulation part ring plug dish and base member chamber, be connected with microwave generator by transmission line.
put on the microwave of discharge gas in gas discharge tube, its reflection power is subjected to the impact of a lot of structures in ion source, in order better microwave reflection to be adjusted, make microwave reflection power reach minimum, the further technical scheme of the utility model, ion source design is useful on the tubular structure fine adjustment part of microwave coupling fine adjustment, to form ionogenic gas discharge tube is arranged in fine adjustment part tube chamber, fine adjustment part two ends are arranged in main regulation part tube chamber overhangingly, the adjustment structure of distance between at the bottom of being designed with for adjustment fine adjustment part end face and base member tube chamber between main regulation part and fine adjustment part.
In technique scheme of the present utility model, adjustment structure between described main regulation part and described strutting piece, the various structures form is arranged, as long as between realizing at the bottom of the ring plug dish of adjustment main regulation part and base member chamber, the structure of distance can, pull out and draw latch structure etc. as scale, pay the utmost attention to and adopt the screw thread pair adjustment structure, by the internal thread that is positioned on strutting piece, with the external screw thread that is positioned on main regulation part body, formed.Adjustable side at the main regulation part preferably is designed with the adjustment operation handle.
In technique scheme of the present utility model, adjustment structure between described main regulation part and described fine adjustment part, the various structures form is equally also arranged, as long as between realizing at the bottom of adjustment fine adjustment part end face and base member tube chamber, the adjustment structure of distance can, pull out and draw latch structure etc. as scale, pay the utmost attention to and adopt the screw thread pair adjustment structure, by the external screw thread that is positioned on fine adjustment part body, with the internal thread that is positioned on main regulation part tube chamber, formed.Adjustable side at the fine adjustment part preferably is designed with the adjustment operation handle.
In technique scheme of the present utility model, described strutting piece is paid the utmost attention to adopt by screw and is fixed in annular endplate on the base member cavity; Pay the utmost attention at the bottom of the tube chamber of described base member and adopt dismantled and assembled structure, be fixed by screws in base member cavity end face by annular plate and form.
In technique scheme of the present utility model, the material of described gas discharge tube is preferentially selected the inorganic insulation materials such as quartz, pottery, alundum (Al2O3).The version of gas discharge tube can be the structures such as sleeve pipe, single tube, and inside diameter ranges can be 0.5-6.0mm.The material of described base member, main regulation part and fine adjustment part is preferentially selected the metal materials such as copper, aluminium, gold.Discharge gas can be He, Ar, N
2, air etc.
The ion source that the utility model provides, the lumen diameter of its base member is generally 25-100mm, and pipe range is generally 10-100mm, and the tube chamber wall thickness is generally 1-5mm; The lumen diameter of fine adjustment part is generally 1-10mm, and pipe range is generally 10-200mm, and pipe thickness is generally 0.1-4mm; The pipe range of main regulation part is generally 10-70mm, and thickness is 1-4mm.
The ion source that the utility model provides, coupling puts on the microwave of discharge gas in gas discharge tube, the microwave source of its microwave generator is paid the utmost attention to the solid state microwave sources that adopts 2450MHZ, and the power output of microwave and reflection power can be read by the display of generator front end.
By the above-mentioned normal pressure maldi mass spectrometer analyzer ion source device that forms based on microwave plasma normal pressure maldi ion source, its formation can be designed to: above-mentioned ion source is placed on the vertical rotary platform that can rotate in 0-90 ° of scopes of vertical plane, described vertical rotary platform is placed in again on 3 dimension (3D) translation stages,, so that from the plasma torch of ion source discharge pipe outlet ejection, aim at testing sample, make sample ionization under plasma desorption ionization.
Microwave plasma normal pressure maldi mass spectrometer analytical method based on above-mentioned ion source device: will be adjusted into for the chamber length that ripple forms the odd-multiple of 1/4 wavelength, as 1/4,3/4,5/4 wavelength, flow of discharge gas speed in gas discharge tube is adjusted into 0.1～5.0L/min, with the microwave coupling of power 10～150W to the discharge gas in gas discharge tube, make the plasma torch aligning testing sample that ejects from discharge tube, make the sample surfaces desorption ionization, sample plasma enters mass spectrometer by the mass spectrometer entrance, analyzes the sample material composition.
Employing is equipped with the ionogenic mass spectrometer of the utility model to analyze sample, the microwave that puts on discharge gas in gas discharge tube makes the discharge gas ionization, plasma produces in the gas discharge tube of insulation, the shape of plasma torch, length change with discharge gas type, discharge gas flow velocity, microwave source power, therefore can regulate by regulating discharge gas flow velocity and microwave power plasma torch.In addition, the microwave power that puts on discharge gas is low, the ion that the sample surfaces desorption ionization obtains more mostly is molecular ion, the high ion that obtains of power more mostly is fragment ion, so people can control by regulating electric rate of flow of fluid and microwave power the ionic species that testing sample produces according to actual needs.
The ionization desorb of the disclosed Microwave Induced Plasma normal pressure of the utility model maldi ion source is the physical and chemical process of a complexity, comprising electric charge transfer, proton translocation, Penning ionization, thermal desorption etc.When Microwave Induced Plasma normal pressure maldi ion source of the present utility model is used for analyte analysis,, take Ar or He as the ionization discharge gas, can be observed [M+H]
+, [2M+H]
+, [M+O+H]
+, [M+2O+H]
+, [M+OH+H]
+Collect with optical fiber the light that Microwave Induced Plasma is launched in order to study its reaction mechanism, detect in 200-1100nm with the optical spectra instrument system, its emission spectrum is analyzed discovery: the OI spectral line at obvious ArI characteristic spectral line, 777.15nm place and H I, N are arranged in 696-965nm scope
2, N
2 +Deng characteristic spectral line.Referring to Fig. 5.During with this ion source test sample, when the proton affinity of determinand is higher than water cluster ion, determinand may with water cluster ion generation Proton-Transfer Reactions, produce protonated ion.Protonated ion and neutral particle OH, M, O generates [M+OH+H]
+, [2M+H]
+, [M+O+H]
+, [M+2O+H]
+The contingent reaction of the utility model Microwave Induced Plasma and determinand has:
M+H
3O
+(H
2O)n→[M+H]
++(n+1)H
2O (1)
[M+H]
2+M→[2M+H]
+ (2)
[M+H]
++OH·→[M+OH+H]
+ (3)
M+H]
++nO·→[M+nO+H]
+ (4)
The maldi ion source of the normal pressure based on microwave plasma that the utility model provides, compare with the ion source of prior art, has following very outstanding technique effect and advantage:
1, the ion source that provides of the utility model is connected with the mass spectrometer with atmospheric pressure interface, can realize the detection to gas, solid, fluid sample, and dismounting is very easy.
2, adopt and be equipped with the ionogenic mass spectrometer of the utility model to detect analysis to sample, do not need sample is carried out complicated pre-treatment, and analysis speed is fast, simple to operate.
3, in to the sample analysis testing process, the plasma temperature that produces due to ion source is higher, does not therefore need to be equipped with the extra device that heats.
3, adopt and be equipped with the ionogenic mass spectrometer of the utility model to detect analysis to sample, need not built-in electrode, do not have high-tension electricity danger and electrode corrosion to pollute; Do not need reagent, can be to environment.
4, in ion source of the present utility model, the plasma that produces is the Microwave Exposure cavity not, and ion source forms the device long service life.
Ion source of the present utility model is applied to mass spectral analysis, and its advantage sums up as having power demand little, and the desired gas amount is few, without the need for malicious reagent, plasma temperature is relatively high, can be to environment, and the very outstanding advantage of many-side that waits easy and simple to handle.
Description of drawings
Accompanying drawing 1 is the structural representation of an embodiment of Microwave Induced Plasma normal pressure maldi ion source.
Accompanying drawing 2 is structural representations of another embodiment of Microwave Induced Plasma normal pressure maldi ion source.
Accompanying drawing 3 is to be equipped with the utility model ion source to detect to analyze mode schematic diagram solid-state, liquid sample.
Accompanying drawing 4 is to be equipped with the utility model ion source to detect the mode schematic diagram of analyzing gaseous sample.
Accompanying drawing 5 is spectrograms of microwave induced argon plasma emission.
Accompanying drawing 6 is mass spectrograms that microwave induced helium plasma is analyzed pure polyethylene glycol, and wherein (a) is the mass spectrogram of pure PEG400, is (b) mass spectrogram of pure polyethylene glycol 800.
Accompanying drawing 7 is mass spectrograms that Microwave Induced Plasma is analyzed L-phenylalanine.
Accompanying drawing 8 is mass spectrograms that paracetamol is analyzed in the Microwave Induced Plasma source.
Accompanying drawing 9 is mass spectrograms that active component in Clarityne is analyzed in the Microwave Induced Plasma source, and wherein (a) is the mass spectrogram of active component in solid-state Clarityne, is (b) mass spectrogram of active component in liquid Clarityne.
In above-mentioned accompanying drawing, the object of each shown by reference numeral sign, 1-gas discharge tube; 2-microwave coupling fine adjustment part; 3--microwave coupling main regulation part; The 4-base member; The 5-mouthpiece; 6-microwave antenna connector; 7-microwave antenna male part; 21-fine adjustment part release handle; 22-fine adjustment part body; 31-main regulation part release handle; 32-main regulation part body; 33-homophony part strutting piece; 34-homophony part ring plug dish; 41-base member cavity; At the bottom of 42-base member chamber, l-is the distance between at the bottom of ring plug dish and base member chamber; G-is the distance between at the bottom of fine adjustment part end face and base member tube chamber.
Embodiment
Below in conjunction with embodiment, the utility model is described in further detail; it is important to point out; following embodiment only is described further invention; and scope of the present utility model is not subjected to the restriction of illustrated embodiment; affiliated art skilled staff is according to the foregoing invention content; the utility model is made some nonessential improvement and adjustment is specifically implemented, should still belong to protection range of the present utility model.
The present embodiment is based on the normal pressure maldi ion source of microwave plasma, as shown in Figure 1, its formation comprises the base member 4 that is designed with the cylinder tube chamber to its structure, be arranged on the main regulation part 3 that is used for the tubular construction of microwave coupling main regulation in base member cylinder tube chamber, be arranged on the fine adjustment part 2 that is used for the tubular construction of microwave coupling fine adjustment in main regulation part tube chamber, be arranged on the intraluminal gas discharge tube 1 of fine adjustment part and be arranged on gas discharge tube and be used for microwave coupling is applied to the microwave antenna of discharge gas in discharge tube outward.At the bottom of the tube chamber chamber of described base member, 42 are fixed by screws in base member cavity 41 end faces by annular plate and form, and are designed with the installing hole that the supplied gas discharge tube passes at the bottom of chamber.Described main regulation part is designed with the ring plug dish 34 that is slidably matched with the base member lumen wall, its adjustable side is designed with release handle 31, be slidably mounted in the base member tube chamber by the strutting piece 33 that is fixed on base member, external screw thread on internal thread on supporting member and main regulation part body 32 forms the adjustment structure of main regulation part, regulate main regulation part ring plug dish 34 by adjustment structure and be positioned at the intraluminal position of base member cylinder, distance (l) between making at the bottom of ring plug dish and base member chamber is adjusted into 1/4 wavelength, so that microwave reflection power is minimum.Described strutting piece is fixed by screws on base member.Described fine adjustment part 2 two ends are arranged in main regulation part tube chamber overhangingly, the adjustment structure of distance (g) between at the bottom of external screw thread formation adjustment fine adjustment part end face on internal thread on main regulation part tube chamber and fine adjustment part body 22 and base member tube chamber, its adjustable side is designed with release handle 21.Described gas discharge tube 1 is the insulated tube of quartzy material, and input is connected with the discharge gas source, the installing hole on output passes at the bottom of the base member chamber.Described microwave antenna consists of male part 7 and the connector 6 of the laminated structure of filling the span of a man's arms on gas discharge tube between at the bottom of main regulation part ring plug dish and base member chamber, connector one end is connected with male part, and the solid state microwave sources that the other end is 2450MHZ by the standard N-type interface 5 and the model that are arranged on base member 4 is connected.
The present embodiment is based on the normal pressure maldi ion source of microwave plasma, as shown in Figure 2, its formation comprises the base member 4 that is designed with the cylinder tube chamber to its structure, be arranged on the main regulation part 3 that is used for the tubular construction of microwave coupling main regulation in base member cylinder tube chamber, be arranged on the intraluminal gas discharge tube 1 of main regulation part and be arranged on gas discharge tube and be used for microwave coupling is applied to the microwave antenna of discharge gas in discharge tube outward.At the bottom of the tube chamber chamber of described base member, 42 are fixed by screws in base member cavity 41 end faces by annular plate and form, and are designed with the installing hole that the supplied gas discharge tube passes at the bottom of chamber.Described main regulation part is designed with the ring plug dish 34 that is slidably matched with the base member lumen wall, its adjustable side is designed with release handle 31, be slidably mounted in the base member tube chamber by the strutting piece 33 that is fixed on base member, external screw thread on internal thread on supporting member and main regulation part body 32 forms the adjustment structure of main regulation part, regulate main regulation part ring plug dish 34 by adjustment structure and be positioned at the intraluminal position of base member cylinder, distance (l) between making at the bottom of ring plug dish and base member chamber is adjusted into 1/4 wavelength, so that microwave reflection power is minimum.Described gas discharge tube 1 is the insulated tube of quartzy material, and input is connected with the discharge gas source, the installing hole on output passes at the bottom of the base member chamber.Described microwave antenna consists of male part 7 and the connector 6 of the laminated structure of filling the span of a man's arms on gas discharge tube between at the bottom of main regulation part ring plug dish and base member chamber, connector one end is connected with male part, and the solid state microwave sources that the other end is 2450MHZ by the standard N-type interface 5 and the model that are arranged on base member 4 is connected.
Embodiment 3:
Apply Microwave Induced Plasma normal pressure maldi ion source of the present utility model and analyze solid-state, liquid sample, can adopt mode shown in Figure 3, the ripple induced plasma normal pressure maldi ion source that embodiment 2 is disclosed is placed on the vertical rotary platform that can rotate in 0-90 ° of scopes of vertical plane, described vertical rotary platform is placed in again on 3D (dimension) translation stage, solid-state or liquid sample are placed on carrier, and the carrier material of carrying sample can be quartz plate, the quartz plate through the HF corrosion, potsherd, stainless steel substrates etc.Liquid sample also can directly be contained in vessel.Sample and mass spectrometer entrance horizontal range are 5-20mm, and vertical range is 1-5mm, and plasma and sample surfaces angle can be 0-90 °,, so that more testing sample ion enters mass spectrometer, improve detection sensitivity, measure the mass spectrum of testing sample.
Embodiment 4:
apply Microwave Induced Plasma normal pressure maldi ion source of the present utility model and analyze gaseous sample, can adopt mode shown in Figure 4, the ripple induced plasma normal pressure maldi ion source that embodiment 1 is disclosed is placed on the vertical rotary platform that can rotate in 0-90 ° of scopes of vertical plane, described vertical rotary platform is placed in again on 3D (dimension) translation stage, gaseous sample is by the conduit introducing or by the sample introduction needle sample introduction, regulate the outlet of Microwave Induced Plasma normal pressure maldi ion source gas discharge tube, the position of conduit outlet, change ion source, conduit, and the distance between the mass spectrometer ion and angle, so that more testing sample ion enters mass spectrometer, improve detection sensitivity, measure the mass spectrum of gaseous sample to be measured.
Embodiment 5:
Polyethylene glycol is widely used in the fields such as cosmetics, medicine, chemical fibre as lubricant, NMF, softening agent.With the utility model Microwave Induced Plasma atmospheric pressure ion source, the polyethylene glycol of different polymerization degree is analyzed.Discharge gas detects PEG400 and polyethylene glycol 800 while adopting helium under positive ion mode, observe the spectrogram (see figure 6) take 44 mean molecule quantities as increment as 400,800, its spectrogram is relevant with holding time of He plasma, along with the growth of holding time of plasma, the protonated molecule of observing is shifted to lower molecular weight.This may be because the reason that long He plasma of life-span and protonated molecule bump.When discharge gas adopts argon gas, the spectrogram of observing is different, when microwave power is 40W, PEG400 can only observe the peak of molecular weight 300 left and right, but along with the increase of microwave power can be observed the larger quasi-molecular ions of molecular weight gradually, but after being increased to a certain degree, can not produce the more peak of HMW.
Adopt Microwave Induced Plasma normal pressure maldi ion source of the present utility model to measure the amino acid of various opposed polarities, can observe obvious molecular ion peak [M+H]
+In addition, also there will be [2M+H]
+, [M+H-HCOOH]
+, and [M+H-H
2O]
+Deng., take L-phenylalanine as example, can observe 166 ([M+H] in spectrogram
+, 100%), 331 ([2M+H]
+, 40%), 120 ([M-HCOOH+H]
+, 5%).See Fig. 7.And in spectrogram, 268 background peaks does not affect determinand and measures.The fragment ion that measures in the utility model Microwave Induced Plasma source only accounts for minimum ratio, and visible Microwave Induced Plasma source is a kind of softer ion source.
Adopt Microwave Induced Plasma normal pressure maldi ion source of the present utility model directly to sample, to analyze, do not need testing sample is carried out pre-treatment.Below with paracetamol, be determined as example explanation.
Paracetamol as anodyne, antipyretic is comprised of Multiple components, as the paracetamol of 500mg, comprises 125mg paracetamol, 230mg aspirin, 30mg caffeine.In experiment, paracetamol directly is put under plasma and analyzes, obtain paracetamol spectrogram shown in Figure 8.152,194,211,303,345 [M+H] that correspond respectively to paracetamol in figure
+, [M+CH
2CO+H]
+, [M+CH
2CO+OH+H]
+, [2M+H]
+, [2M+CH
2CO+H]
+Do not observe the molecular ion peak of aspirin in spectrogram, 163 and 240 peak corresponds respectively to its [M-H
2O+H]
+, [M+CH
3COO+H]
+Aspirin loses the peak of a part water at DESI(desorption electrospray ionization source) with the real-time ionization source of DART(Direct Analysis) report is arranged in document.In document, report is with PADI(plasmaassisted desorption ionization source) 121 peaks that lose a molecular acid of generation do not find at this ionogenic spectrogram.195 and 388 peaks of the protonated molecular ion corresponding to caffeine and dimer quasi-molecular ions [M+H] in spectrogram
+, [2M]
+
Embodiment 8
Adopt the utility model Microwave Induced Plasma normal pressure maldi ion source can directly be used for analyzing liquid sample.Hold solution with 25mL glass culture dish or surface plate, be placed under Microwave Induced Plasma, sample ionization under plasma desorption ionization, sample ions directly enters in mass spectrometer and analyzes.Respectively the solid-state and liquid state of antihistaminic Clarityne is analyzed and found (see figure 9), solid-state and liquid sample can be observed the protonated molecular ion peak at 383 places and chlorine isotope at the peak at 385 places, but the background peaks that liquid sample is observed will be lacked.There is more intense signal at the peak at 224 places at solid-state middle ratio in liquid state, may be because its corresponding composition solubility in solvent is less, is deposited to the solution bottom.And plasma can only the desorption ionization solution surface.This can illustrate that the peak at 224 places is cleaning agents of reporting in the main component of Clarityne rather than air background or DESI.
Claims (9)
1. microwave plasma normal pressure maldi ion source, it is characterized in that, comprise the base member (4) that is designed with the cylinder tube chamber, be arranged on the tubular structure main regulation part (3) that is used for regulating microwave coupling in base member cylinder tube chamber, be arranged on the intraluminal gas discharge tube of main regulation part (1) and be arranged on gas discharge tube and be used for microwave coupling is applied to the microwave antenna of discharge gas in discharge tube outward, at the bottom of the chamber of described base member cylinder tube chamber, (42) are designed with the installing hole that gas discharge tube therefrom passes, described main regulation part is designed with the ring plug dish (34) that is slidably matched with the base member lumen wall, be slidably mounted in the base member tube chamber by the strutting piece (33) that is fixed on base member, be designed with adjustment structure between supporting member (33) and main regulation part, by adjustment structure with the ring plug dish of main regulation part and base member chamber at the bottom of between be used for chamber length that ripple forms and be adjusted into the odd-multiple of 1/4 wavelength, so that microwave reflection power is minimum, described gas discharge tube is the insulated tube of inorganic, input is connected with the discharge gas source, installing hole on output passes at the bottom of the base member chamber, on the gas discharge tube of the male part of described microwave antenna between at the bottom of main regulation part ring plug dish and base member chamber, be connected with microwave generator by transmission line.
2. microwave plasma normal pressure maldi ion source according to claim 1, it is characterized in that, ion source design is used for the tubular structure fine adjustment part (2) of microwave coupling fine adjustment, gas discharge tube (1) is arranged in fine adjustment part tube chamber, fine adjustment part two ends are arranged in main regulation part tube chamber overhangingly, the adjustment structure of distance between (42) at the bottom of being designed with for adjustment fine adjustment part body end face and base member chamber between main regulation part and fine adjustment part.
3. microwave plasma normal pressure maldi ion source according to claim 1 and 2, it is characterized in that, adjustment structure between described main regulation part and described strutting piece is the screw thread pair adjustment structure, consist of with the external screw thread that is positioned on main regulation part body (32) the internal thread that is positioned on strutting piece, the adjustable side of main regulation part is designed with adjustment operation handle (31).
4. microwave plasma normal pressure maldi ion source according to claim 1 and 2, it is characterized in that, adjustment structure between described main regulation part and described fine adjustment part spare is the screw thread pair adjustment structure, consist of with the internal thread that is positioned on main regulation part tube chamber the external screw thread that is positioned on fine adjustment part body (22), the adjustable side of fine adjustment part is designed with adjustment operation handle (21).
5. microwave plasma normal pressure maldi ion source according to claim 1 and 2, is characterized in that, described strutting piece is for being fixed in the annular endplate on base member cavity end face by screw.
6. microwave plasma normal pressure maldi ion source according to claim 1 and 2, is characterized in that, is dismantled and assembled structure at the bottom of the chamber of described base member, is fixed by screws in base member cavity (41) end face by annular plate and forms.
7. microwave plasma normal pressure maldi ion source according to claim 1 and 2, is characterized in that, the material of described gas discharge tube is quartz, pottery or alundum (Al2O3).
8. microwave plasma normal pressure maldi ion source according to claim 1 and 2, is characterized in that, the material of described base member (4), main regulation part (3) and fine adjustment part (2) is copper, aluminium or gold.
9. the ion source device of the normal pressure maldi mass spectrometer analyzer that is formed by the described microwave plasma normal pressure of one of claim 1 to 8 maldi ion source, it is characterized in that, described ion source is placed on the vertical rotary platform that can rotate in 0-90 ° of scopes of vertical plane, described vertical rotary platform is placed in again on 3 dimension translation stages, so that aim at testing sample from the plasma torch of ion source discharge pipe outlet ejection, sample ionization under plasma desorption ionization.
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| CN (1) | CN203300594U (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103236394A (en) * | 2013-04-17 | 2013-08-07 | 四川大学 | Microwave plasma based atmospheric pressure desorption ion source and application thereof |
| CN113727508A (en) * | 2020-05-26 | 2021-11-30 | 上海大学 | Novel vacuum microwave plasma ion source |
-
2013
- 2013-04-17 CN CN2013201949486U patent/CN203300594U/en not_active Expired - Lifetime
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103236394A (en) * | 2013-04-17 | 2013-08-07 | 四川大学 | Microwave plasma based atmospheric pressure desorption ion source and application thereof |
| CN103236394B (en) * | 2013-04-17 | 2015-12-09 | 四川大学 | Based on atmospheric pressure desorption ion source and the application thereof of microwave plasma |
| CN113727508A (en) * | 2020-05-26 | 2021-11-30 | 上海大学 | Novel vacuum microwave plasma ion source |
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