CN202339901U - High voltage assisted laser desorption ionization mass spectrometric analysis ion source - Google Patents
High voltage assisted laser desorption ionization mass spectrometric analysis ion source Download PDFInfo
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- CN202339901U CN202339901U CN2011204989217U CN201120498921U CN202339901U CN 202339901 U CN202339901 U CN 202339901U CN 2011204989217 U CN2011204989217 U CN 2011204989217U CN 201120498921 U CN201120498921 U CN 201120498921U CN 202339901 U CN202339901 U CN 202339901U
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- temperature control
- ion source
- laser desorption
- desorption ionization
- control plate
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Abstract
The utility model discloses a high voltage assisted laser desorption ionization mass spectrometric analysis ion source, which comprises a laser, a support, a temperature control plate, a high-voltage power supply and sample surfaces with at least one surface conducting, wherein the temperature control plate is horizontally fixed on the support, the sample surfaces are flatwise placed on the temperature control plate and insulated from the temperature control plate, the high-voltage power supply is electrically connected with the sample surfaces, and the laser is located above the sample surfaces. The high voltage assisted laser desorption ionization mass spectrometric analysis ion source is easy, fast and convenient to operate, can obtain good sample signals in positive ion analysis mode and negative ion analysis mode, and can continuously analyze a plurality of samples; and can further inspect signal responses of the samples at different temperatures, obtain thermodynamic data and dynamic data of reactions and the like through temperature control on the sample surfaces.
Description
Technical field
The utility model relates to chemical analysis field, relates in particular to a kind of high pressure assisted laser desorption ionization massspectrum and analyzes ion source.
Background technology
Ion source is one of mass spectrometric core component, and its effect is the ion that sample is transformed into gas phase.At present, common mass ion source mainly contains: electron impact ionization source (EI), chemical ionization source (CI), fast atom bombardment source (FAB), electron spray ionisation source (ESI), APCI source (APCI), substance assistant laser desorpted ionized source (MALDI) etc.These ionogenic ionization mechanisms are different, are applicable to the compound that ionization is dissimilar respectively, obtain the molecular ion and the fragment ion thereof of respective compound.These ion sources need use under vacuum condition mostly or before mensuration, need loaded down with trivial details preprocessing process, can not be under the original state of sample to its carry out continuously, real-time, high throughput analysis.In recent years; Having occurred with desorption electrospray ionization (DESI) and real time direct analysis (DART) technology is the multiple novel normal pressure open type ion source of representative; They combine the normal pressure desorption technology of sample with its ioning method; Thereby do not need the sample pretreatment of any (or seldom), just can carry out direct rapid analysis sample.
In various novel normal pressure open type ion sources, attach the ion source of technology based on laser desorption and pay close attention to because of its unique advantage has received widely.Laser can instantaneously provide higher energy to sample surfaces on the one hand, helps the desorption of macromolecular substances such as protein, DNA; Laser has higher spatial resolution on the other hand, is suitable for the imaging analysis of material or biological tissue.
These comprise based on the normal pressure open type ion source that laser desorption attaches technology: the electron spray assisted laser desorption attaches ionization (ELDI); Laser lift-off electro-spray ionization (LAESI), substance assistant laser desorpted attach electro-spray ionization (MALDESI) and laser desorption and attach spraying back ionization (LDSPI) etc.Their common feature is the lagging ionization technology that can electron spray (ESI) ioning method be attached the gas phase sample of generation as laser desorption, therefore has similar working principle.With LDSPI is example: laser radiation places the solid-state or liquid sample on sample target surface; Make the sample molecule desorption come out to get into gas phase; And merge mutually with charged spray droplet in electron spray zone, after obtain gaseous ion with one or more electric charges with the similar desolvation process of ESI.LDSPI can obtain ionization effect preferably under the cation analytical model; But under the anion analytical model, be difficult to obtain good sample ions signal; This is because the normally used spraying solvent of LDSPI (methanol or acetonitrile/water) is difficult to the stable spraying of formation under the anion analytical model, causes that Ionization Efficiency is lower thereafter.
People such as Muddiman once carried out improvement to their MALDESI ion source; They are Ionized electron spray afterwards; But voltage directly is added on the metal surface of carrying sample; Promptly on the substance assistant laser desorpted sample surfaces that attaches ioning method, increase high voltage, made the Ionization Efficiency of sample make moderate progress.But this method needs in sample, to sneak into matrix, has not only increased the complexity of analytic process, has also destroyed original state of sample simultaneously, and the existence of matrix has limited this The Application of Technology easily to the analysis generation interference of micromolecular compound.
In addition, the serviceability temperature control system not only can cause reaction, the conditioned reaction speed of sample through heating in novel normal pressure open type ion source, and can be to optionally ionization of sample.For example, people such as Nilles through the temperature of Control work gas, have realized containing the separation and the detection of mixture of three kinds of molecules of identical nominal molecular weight in the real time direct analytical technology.Yet, in the ionogenic report of various normal pressure open types that attaches based on laser desorption, also do not see with the utility model in the application of similar temperature control equipment.
The utility model content
The technical problem that the utility model solves is to provide a kind of and need add matrix, analyzes easy, ion source fast.
In order to overcome the above problems; The utility model provides a kind of high pressure assisted laser desorption ionization massspectrum to analyze ion source; Comprise the sample surfaces of laser, support, temperature control plate, high voltage source and at least one surface conductance, the temperature control plate level is fixed on the support, and sample surfaces lies on the temperature control plate and with the temperature control plate and insulate; High voltage source is electrically connected with sample surfaces, and laser is positioned at the sample surfaces top.
Since when being employed in laser desorption and attaching on the metal sample surface on-load voltage, guaranteed under the positive and negative ion analytical model, all can obtain sample signal intensity and signal to noise ratio preferably; Owing to matrix need in determinand, do not added or carry out other sample pretreatments, simplified operation again, the possibility of having avoided matrix to disturb simultaneously for sample.
Description of drawings
When combining accompanying drawing to consider; Through with reference to following detailed, can more completely understand the utility model better and learn wherein many attendant advantages easily, accompanying drawing described herein is used to provide the further understanding to the utility model; Constitute the part of the utility model; Illustrative examples of the utility model and explanation thereof are used to explain the utility model, do not constitute the improper qualification to the utility model, wherein:
Fig. 1 is that the utility model high pressure assisted laser desorption ionization massspectrum is analyzed ionogenic structural representation Fig. 1;
Fig. 2 is that the utility model high pressure assisted laser desorption ionization massspectrum is analyzed ionogenic structural representation Fig. 2;
Fig. 3 is that the utility model high pressure assisted laser desorption ionization massspectrum is analyzed ionogenic structural representation Fig. 3;
Fig. 4 is the structural representation of the utility model support;
Fig. 5 is the structural representation of the utility model conductive metal sheet;
Fig. 6 is the structural representation of the utility model fixed part.
Embodiment
Following embodiment with reference to Fig. 1-6 pair the utility model describes.
For make above-mentioned purpose, feature and advantage can be more obviously understandable, below in conjunction with accompanying drawing and embodiment the utility model done further detailed explanation.
The utility model provides a kind of high pressure assisted laser desorption ionization (HALDI, High Voltage Assisted Laser Desorption Ionization) mass spectral analysis ion source.In the HALDI mass spectral analysis; Fluid sample directly is added on the metal sample surface; Dependence loads on the external voltage of sample surfaces and is charged; Under laser radiation, go out tiny charged drop, obtain sample ions, and under effect of electric field, get into the mass spectrum injection port with one or more electric charges through the desolvation process from the sample surfaces desorption.Though; The sample ions process of HALDI and the ionization process of LDSPI have similarity; Under the cation analytical model, all can produce sample ions signal preferably, still visibly different with LDSPI is that HALDI also can obtain stable ion signal under the anion analytical model; And need not add matrix with improved MALDESI compared with techniques, analyze easy, quick.In addition,, can also investigate the signal response of sample under different temperatures through the sample surfaces temperature control, and the thermodynamics and kinetics data of acquisition reaction etc.On the temperature control plate, place sample surfaces a plurality of and the external voltage conducting, can realize the continuous analysis of a plurality of samples through the control motorized precision translation stage.
Embodiment
High pressure assisted laser desorption ionization massspectrum that the utility model provides is analyzed ion source structure shown in Fig. 1-3, comprises 1, support, and 2, conductive metal sheet, 3, the temperature control plate, 4, fixed part, 5, sample surfaces, laser.Its medium-height trestle 1 can be fixedly connected with the D translation platform, with the package unit support fixation.Conductive metal sheet 2 is fixed through the metal screw with support 1, and external voltage can be transmitted on the conductive metal sheet 2 through the metal screw.Temperature control plate 3 can be buy or homemade electric hot plate, electric heating piece or cooling piece etc.Sample surfaces 5 is coated with the other materials thin slice of metal level for sheet metal or surface.Fixed part 4 can be installed in support 1 lower end and vertically be slidingly connected with support 1.The laser emitted laser is a pulse laser, is radiated on the sample of sample surfaces 5 carryings.
Fixed part 4 is by the insulation heat proof material; Like phenolic plastics etc.; Be processed into; The lower end is passed the groove of support 1 and vertically is slidingly connected with support 1, can regulate the position of fixed part 4 through regulating the middle screw in support 1 lower end, and fix the temperature control plate 3 between fixed part 4 and the support 1.
Laser for buy or the pulse laser built of design voluntarily.The wavelength of the pulse laser that laser is launched is 1064nm.The frequency adjustable of pulse laser is generally 20Hz.The energy of pulse laser is adjustable, is generally 1.1mJ/pulse.When fluid sample and external voltage conducting, the pulsed laser irradiation that laser is launched is on the fluid sample that sample surfaces 5 carries, and desorption goes out tiny charged drop, perhaps directly goes out sample ions from the sample surfaces desorption.
The rapidoprint of support 1 and fixed part 4 is guaranteeing under the firm prerequisite it can is phenolic plastics, pottery, also can make other insulation heat proof materials.
Screw through regulating support 1 lower end can be fixed on temperature control plate 3 between support 1 and the fixed part 4, also can adopt fixedly temperature control plate 3 of other modes.
Between support 1 and the fixed part 4 certain adjustable range is arranged, when the size of temperature control plate 3 exceeds existing adjustable range, but support 1 and fixed part 4 that processing dimension matches.
Fixed part 4 lower ends embed the groove of support 1 and are slidingly connected with support 1, and the position of regulating fixed part 4 through support 1 lower end screw is temperature control plate 3 fixedly, also can adopt fixedly temperature control plate 3 of other modes.
High pressure assisted laser desorption ionization massspectrum is analyzed ion source, direct analyzing liquid sample, and the solvent of liquid sample can be methanol, acetonitrile/water etc.During laser radiation, should be taken into account sample solvent contingent reaction even burning under laser radiation, and carry out corresponding safety prevention measure.When heat on the surface, should be taken into account the at high temperature contingent variation of sample and solvent thereof and carry out corresponding safety prevention measure.
When temperature control plate 3 outer surfaces are electric conducting material, should coat one deck heat-conducting insulation material, avoid applied voltage to damage the electric elements in the temperature control plate 3., ion source should avoid directly contacting the parts of on-load voltage when working.
Should wear lasering protective eyeglass when opening laser.
The optical maser wavelength that laser is selected for use can be at infrared, visible or ultraviolet band.
All screw threads, screw and nut in the present embodiment also can be English system guaranteeing both can be metric system under the prerequisite that matches each other.
The ionogenic package unit of the above mass spectrum high pressure assisted laser desorption can place on the adjustable translation stage of three-dimensional.
Ion source analytic sample method is following:
As stated, the embodiment of the utility model has been carried out explanation at length, but as long as break away from the inventive point and the effect of the utility model in fact a lot of distortion can not arranged, this will be readily apparent to persons skilled in the art.Therefore, such variation also all is included within the protection range of the utility model.
Claims (10)
1. a high pressure assisted laser desorption ionization massspectrum is analyzed ion source; It is characterized in that; Comprise the sample surfaces of laser, support, temperature control plate, high voltage source and at least one surface conductance, the temperature control plate level is fixed on the support, and sample surfaces lies on the temperature control plate and with the temperature control plate and insulate; High voltage source is electrically connected with sample surfaces, and laser is positioned at the sample surfaces top.
2. a kind of according to claim 1 high pressure assisted laser desorption ionization massspectrum is analyzed ion source, and it is characterized in that: said laser is a pulse laser.
3. a kind of according to claim 1 high pressure assisted laser desorption ionization massspectrum is analyzed ion source, and it is characterized in that: said support is processed by the High-Voltage Insulation heat proof material.
4. analyze ion source like the said a kind of high pressure assisted laser desorption ionization massspectrum of claim 3, it is characterized in that: said High-Voltage Insulation heat proof material is phenolic plastics.
5. a kind of according to claim 1 high pressure assisted laser desorption ionization massspectrum is analyzed ion source, and it is characterized in that: said sample surfaces is the gold-plated silicon chip of upper surface.
6. a kind of according to claim 1 high pressure assisted laser desorption ionization massspectrum is analyzed ion source, and it is characterized in that: also comprise the electric three-dimensional translation stage, support is fixed on the electric three-dimensional translation stage.
7. analyze ion source like the said a kind of high pressure assisted laser desorption ionization massspectrum of one of claim 1 to 6; It is characterized in that: also comprise conductive metal sheet; Conductive metal sheet is fixed on the support, and high voltage source is electrically connected with conductive metal sheet earlier, and conductive metal sheet is electrically connected with sample surfaces again.
8. analyze ion source like the said a kind of high pressure assisted laser desorption ionization massspectrum of claim 7, it is characterized in that: said conductive metal sheet is processed by the other materials that gold, silver or alloy or surface are coated with metal level or alloy-layer.
9. analyze ion source like the said a kind of high pressure assisted laser desorption ionization massspectrum of one of claim 1 to 6; It is characterized in that: also comprise the fixed part that an insulation heat proof material is processed; The temperature control plate holder is fixed between support and fixed part and by fixed part, and fixed part is installed in the support lower end and vertically is slidingly connected with support.
10. analyze ion source like the said a kind of high pressure assisted laser desorption ionization massspectrum of one of claim 1 to 6, it is characterized in that: heater or refrigerating plant that said temperature control plate is plate or sheet.
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CN2011204989217U CN202339901U (en) | 2011-12-02 | 2011-12-02 | High voltage assisted laser desorption ionization mass spectrometric analysis ion source |
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CN2011204989217U CN202339901U (en) | 2011-12-02 | 2011-12-02 | High voltage assisted laser desorption ionization mass spectrometric analysis ion source |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104616961A (en) * | 2015-02-16 | 2015-05-13 | 江苏天瑞仪器股份有限公司 | Ion source three-dimensional linkage mechanism |
CN111684271A (en) * | 2018-02-09 | 2020-09-18 | 浜松光子学株式会社 | Sample support and method for producing sample support |
-
2011
- 2011-12-02 CN CN2011204989217U patent/CN202339901U/en not_active Expired - Fee Related
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104616961A (en) * | 2015-02-16 | 2015-05-13 | 江苏天瑞仪器股份有限公司 | Ion source three-dimensional linkage mechanism |
CN111684271A (en) * | 2018-02-09 | 2020-09-18 | 浜松光子学株式会社 | Sample support and method for producing sample support |
US11948787B2 (en) | 2018-02-09 | 2024-04-02 | Hamamatsu Photonics K.K. | Sample support, and manufacturing method of sample support |
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C14 | Grant of patent or utility model | ||
GR01 | Patent grant | ||
CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20120718 Termination date: 20141202 |
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EXPY | Termination of patent right or utility model |