CN103367090A - An ion analyzer and an ion analysis method - Google Patents
An ion analyzer and an ion analysis method Download PDFInfo
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- CN103367090A CN103367090A CN2012100908756A CN201210090875A CN103367090A CN 103367090 A CN103367090 A CN 103367090A CN 2012100908756 A CN2012100908756 A CN 2012100908756A CN 201210090875 A CN201210090875 A CN 201210090875A CN 103367090 A CN103367090 A CN 103367090A
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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
- G01N27/624—Differential mobility spectrometry [DMS]; Field asymmetric-waveform ion mobility spectrometry [FAIMS]
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- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
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- H01J49/009—Spectrometers having multiple channels, parallel analysis
Abstract
The invention relates to an ion analyzer and an ion analysis method using a differential mobility analyzer array and a mass spectrum analyzer array. The ion analyzer comprises an ion source or ion source array, a differential mobility analyzer array, an ion transfer passage array, a mass spectrum analyzer array, and an ion detector or ion detector array which are connected successively. The differential mobility analyzer array, the ion transfer passage array, and the mass spectrum analyzer array respectively comprise two or more channels with same amount and one-to-one correspondence. In the ion analysis method, ions generated by the ion source or ion source array are introduced into the various channels of the differential mobility analyzer array. Selected by the channels based on ion mobility, the ions enter mass spectrum analyzer array via the ion transfer passage array and finally are detected by the ion detector or ion detector array.
Description
Technical field
The present invention relates to the device and method of ion isolation and detection, relate in particular to ion analyzer and the ion analysis method of using difference ion mobility spectrometry analyzer array and mass spectrometer array that the complex sample from chromatographic isolation or Direct Sampling process is efficiently separated and detects.
Background technology
Along with the attention of countries in the world to public safety and anti-terrorism ability, has the object that the analytical instrument that can quick and precisely identify target compound and method more and more become each research institution and instrument company's research and development.Ionic migration spectrometer is as a kind of relative structure is simple, cost is lower but speed is higher and the ion analysis method of wide spectrum, has played the part of important role in the anti-terrorism work of various countries.Instrument based on ionic migration spectrometer has been widely used in the place that the crowd is dense and the mechanisms such as airport, station, Large conference center at present, also comprises explosive, drugs and other contraband for the target determinand.
Meanwhile, gas phase and liquid chromatogram be in each analysis field status that still takes advantage, and based on the ion analyzer of ion mobility spectrometry as chromatographic detector also with its comparatively faster speed and relatively independent separation principle and be subject to increasing attention.Certainly, the ion analyzer based on ion mobility spectrometry can also be contained between chromatograph and the mass spectrometer, the peak capacity with further raising system alleviates the mass spectrometric burden of rear class.
The ion mobility spectrometry quasi-instrument is divided three classes on structure and operating principle usually, be ionic migration spectrometer (Ion Mobility Spectrometer, IMS), difference ion mobility spectrometry analyzer (Differential Mobility Analyzer, DMA), and difference ionic migration spectrometer (Differential Mobility Spectrometer, DMS) or claim High-Field asymmetric waveform ion mobility spectrometer (High Field Asymmetric Waveform Ion Mobility Spectrometer, FAIMS).Wherein, IMS and DMA two class ionic migration spectrometers all are take the different mobilities of ion as according to ion is carried out separation and detection, and DMS/FAIMS carries out separating and detection of ion in the difference (difference is moved the spectrum rate) of mobility difference under the high electric field and under the low electric field with different ions.
Detecting instrument take IMS as principle is usually operated under the pulse mode, namely introduces the ion that enters simultaneously on a small quantity the drift region by the high-speed switch of ion gate, and then judges its Ion configuration by detecting these ions through the time of drift tube.This class detector can be referring to paper: Eiceman, G.A.and Karpas, Z., Ion Mobility Spectrometry, CRC Press, 2005,119pp..This class detector usually both can have been worked and under atmospheric pressure also can be operated under the low vacuum, and it is simple in structure, and the data of acquisition relatively directly and be easy to explain.Yet, ion source all is operated under the continuous mode when chromatogram etc. is separated the instrument coupling (especially with) under most atmospheric pressure/low vacuum, therefore use the input mode of pulse mode can make the duty ratio of instrument very low for IMS, this greatly reduces the utilization ratio to sample.
Compare with IMS, the mode of operation of DMA is different.The relative theory of DMA can be referring to paper: Panich Intra et al., Songklanakarin J.Sci.Technol.30 (2), 243-256, Mar.-Apr.2008.In DMA, with the channel flow of even high velocity air along the formation of pair of parallel battery lead plate; The ion current that produces continuously is positioned at this by one the slit on the electrode of parallel electrode plate is entered flow area and mobile downstream with air current flow.Because this is to being added with an electric field force perpendicular direction in the direct voltage (migration voltage) of airflow direction on the parallel electrode plate, ion is also moving under the condition of same air velocity and electric field force intensity to the opposite electrode under the effect of electric field force in air current flow, the size of ionic mobility has determined that this ion takes time in the uprush direction, has also determined this kind ion final mobile distance on airflow direction simultaneously.Draw from the slit that is positioned at the airflow downstream somewhere by regulating the size of electric field force between two battery lead plates, can make the ion with a certain ionic mobility, thereby realization is to the detection of this ion.For DMA, sampling process is continuous, this for various atmospheric pressure under the ion source with continuous mode work mate very large advantage arranged.Yet, also needing scan the migration voltage on the analyzer when obtaining a full spectrum, this can make the duty ratio when analyzing greatly reduce.But it should be noted that, for some online detections or monitor procedure, target compound may only have several or tens kinds, one of potential method that addresses this problem in this field can be after for the first time scanned, between several or tens different migration voltages, switch, thereby improve to a certain extent the detection efficiency of DMA.
Although DMA compares in the ion utilization ratio with IMS certain advantage is arranged, it is in resolution advantage not, especially for little molecule, strong diffusion effect so that its resolution usually all below tens, and difficult the raising.Therefore as an on-line monitoring equipment, producing false positive results also is a challenge that DMA faces.For addressing this problem, can with DMA and with its mass spectrometer coupling that detection character is relatively independent and resolution is higher.
From with the matching degree of difference ion mobility spectrometry analyzer prime, need part extremely step-scan cycle of several seconds owing to will obtain a complete ion mobility spectrometry, this, scope pair was with direct analysis (under the atmospheric pressure directly with the sample desorption ionization) or carry out coupling with chromatogram and all seem slightly slow running time, especially for the liquid chromatogram of speed or very high desorption temperature, the sample appearance time also just within several seconds, therefore misses preferably sampled point easily.
An important way that addresses this problem and improve the ion utilization ratio is by using frequency multiplexing technique, namely detecting simultaneously with a plurality of ion mobility spectrometry passages and corresponding mass spectrometer passage.The a plurality of IMS passages of use of in US Patent No. 7482582 B2, mentioning such as Ionwerks company and the method for ion trap and time-of-flight mass spectrometer coupling.In the method, a plurality of passages receive behind the ion of ion trap injection, and synchronous working is depressed in same electrical, and the ion of each passage outflow is detected by the respective channel in the multianode detector of a flight time afterwards.This patent has been used the multichannel detection technique, but owing to each passage is operated under the synchronous pulse mode, and the low problem of unresolved whole testing process duty ratio, so the utilization ratio of ion still can not be largely increased.
The people such as Chen mention in the article of multi-stage DMA and use same DMA passage, but detect synchronously (Aerosol Science and Technology, 41:217-230,2007) at the different channel position of DMA.Similarly method is also described (J.Aerosol Res., 21 (4), 329-340 (2006)) to some extent in the people's such as Intra article.The advantage of these class methods is that the analysis efficiency of system is very high, can both continuously detect ion on the detector everywhere.But shortcoming is, in case the electric field of whole passage is determined the ion that each detector can only corresponding a certain fixedly mobility.Especially when the mobility of the various ions that need to detect not during even variation, the relative position of detector is difficult to be determined.For different analytic samples, whole instrument will lack flexibility simultaneously.
Another example that uses frequency multiplexing technique is the ion transfer arrangement of being made by microelectromechanical-systems that Owlstone company uses FAIMS technology (US7714277 B2).In this technology, multichannel FAIMS analyzer is comprised of the unit that two microelectromechanical-systems processing obtain.Ion enters analyzer from a multichannel end, and is regional by multichannel under the driving of axial electric field.Owing on each passage, all be applied with same radio frequency and the direct voltage that carries out the selection of difference ionic mobility, therefore only have the ion of suitable difference mobility to pass through, thereby reach the purpose of ion isolation and detection simultaneously.Similar with US7482582 B2 patent, using multichannel purpose in the US7714277 B2 patent also is in order to increase the flux of whole system.For the ionic mobility that detects in the certain limit, the voltage on the FAIMS still needs scanning, and the duty ratio of whole instrument is still not high.
Another piece about the U.S. Patent application that uses multichannel FAIMS technology in (US2008/0067350 A1), Li Gangqiang has proposed to use simultaneously multichannel FAIMS to carry out sample analysis, but the bucking voltage of each paths (CV) can be different, therefore can improve the analysis speed of whole instrument.But this document is not discussed multichannel DMA technology.
It is worthy of note simultaneously, when using multichannel ion analyser to carry out ion detection, if each passage needs independently detector and follow-up amplification Acquisition Circuit to carry out ion detection, will greatly increase the cost of analytical instrument.For this class problem, in the United States Patent (USP) 7157699 of Ou Yangzheng, also mentioned use array mass spectrometer especially the array ion trap ion is carried out quality analysis, and the ion detection method that a plurality of discrete ion detectors are used in combination.The limitation of this method is, has reduced the quantitative requirement that rear class is gathered amplifying circuit although use by the combination to a plurality of ion detectors, and the number of ion detector can not reduce.For another example, the equality people of fourth army has proposed to use an ion detector and the scheme of follow-up amplification Acquisition Circuit to detecting by the ion behind the array of a plurality of level Four bars compositions at " mass spectrum journal, Vol22, No.3,29-35. ".Yet this scheme can only be used each mass spectrometer Channel Synchronous, and therefore when adding the ion mobility spectrometry choice device that can work alone separately before this mass spectrometer array, the latter's function just can not embody fully.
Summary of the invention
Technical problem to be solved by this invention provides a kind of ion analyzer that uses difference ion mobility spectrometry analyzer array and the coupling of mass spectrometer array, and a kind of this ion detection device that uses carries out the quick and precisely ion analysis method of sample analysis, the shortcoming that efficient is low when detecting in order to solve present use ion mobility spectrometry quasi-instrument, false positive is high.
The present invention is that to solve the problems of the technologies described above the technical scheme that adopts be to propose a kind of ion analyzer, comprise the ion source or the ion source array that link to each other successively, difference ion mobility spectrometry analyzer array, ion transfer passage array, the mass spectrometer array, and ion detector or ion detector array, wherein said difference ion mobility spectrometry analyzer array, described ion transfer passage array, each self-contained two or more passage of described mass spectrometer array, and a passage of the corresponding at least described mass spectrometer array of a passage of each described difference ion mobility spectrometry analyzer array.
In one embodiment of this invention, described mass spectrometer array is level Four bar array or ion trap array.
In one embodiment of this invention, ion analyzer also can comprise the ionic dissociation device, is located between described ion transfer passage array and the described mass spectrometer array.
In one embodiment of this invention, described ionic dissociation device is gas collisions chamber or photodissociation chamber or electron capture dissociation chamber.
In one embodiment of this invention, described difference ion mobility spectrometry analyzer array is planar structure, and the ion entrance is positioned at the relative same position of each passage, and the relative position of each channel ions exit slit is identical.
In one embodiment of this invention, described each passage of difference ion mobility spectrometry analyzer array structure that is centrosymmetric, the corresponding center line of each passage distributes in radial symmetric.
In one embodiment of this invention, each unit of described mass spectrometer array is equipped with independently ion detector and data acquisition amplification system.
In one embodiment of this invention, be centrosymmetric structure and ion detector of each units shared and data acquisition system of each unit of described mass spectrometer array.
In one embodiment of this invention, described difference ionic migration spectrometer array is to be operated under synchronous mode or the asynchronous mode, and described mass spectrometer array is to be operated under synchronous mode or the asynchronous mode.
In one embodiment of this invention, the work of described difference ion mobility spectrometry analyzer array under atmospheric pressure.
In one embodiment of this invention, described difference ion mobility spectrometry analyzer array is operated under the environment that is lower than atmospheric pressure but is not less than 0.1torr.
In one embodiment of this invention, the airflow direction in the described difference migration spectralyzer array and described ion transfer passage array is axial vertical.
In one embodiment of this invention, each feeder connection place of described difference migration spectralyzer array is provided with an ion current detector, and described ion current detector links to each other with the current sensing means of outside.
In one embodiment of this invention, described ion source comprises an isotopic ion source, and described isotopic ion source can optionally be opened or close by mechanical device according to the experiment needs.
In one embodiment of this invention, described ion analysis method comprises each passage of the ion of ion source or the generation of ion source array being introduced difference ion mobility spectrometry analyzer array, after each passage carries out selection based on ionic mobility, through entering the mass spectrometer array behind the ion transfer passage array and finally being detected by ion detector or ion detector array.
In one embodiment of this invention, described method also comprises makes ion before entering each passage of described mass spectrometer array, is introduced into an ionic dissociation device, so that ion can describedly dissociate in the ionic dissociation device.
In one embodiment of this invention, described difference ionic migration spectrometer array is to be operated under synchronous mode or the asynchronous mode, described mass spectrometer array is to be operated under synchronous mode or the asynchronous mode, and described method comprises with the variation of signal in the sampling process to be switched the mode of operation of described difference ionic migration spectrometer array and/or described mass spectrometer array.
In one embodiment of this invention, described method comprises and uses level Four bar array or ion trap array as described mass spectrometer array.
In one embodiment of this invention, when using a described ion detector, described method comprises that the mode that adopts Time share scanning to evict from surveys the ion information of each passage.
In one embodiment of this invention, described method also comprises uses an ion current detector that is positioned at each feeder connection place of difference ion mobility spectrometry analyzer array, ion introducing amount to each passage is monitored, after the described ion strength of flow normalization of resulting each passage, be used for calibrating the object ion intensity that finally records in each passage.
In one embodiment of this invention, described method comprises the isotopic ion source that is arranged in described ion source of using, and by using each passage of described ion analyzer respectively certain specific ion that described isotopic ion source produces regularly to be detected, final each passage is used for calibrating the object ion intensity that finally records in each passage after resulting ionic strength normalization on the described ion detector.
Ion analyzer proposed by the invention and ion analysis method are owing to use multichannel difference ion mobility spectrometry and multichannel mass spectrometer and single or multiple ion detector coupling, thus detection efficiency and the accuracy of raising instrument; The simultaneously coupling of difference ion mobility spectrometry array and mass spectrometer array can be operated under the different mode, thereby has improved the application power of this device in fields such as public safety and environmental monitorings.
Description of drawings
For above-mentioned purpose of the present invention, feature and advantage can be become apparent, below in conjunction with accompanying drawing the specific embodiment of the present invention is elaborated, wherein:
Figure 1A illustrates the structure that ion source and plate difference ion mobility spectrometry analyzer array, plate ion guides array, plate ion trap analyzer array are contacted mutually.
Figure 1B illustrates the basic structure of a unit in the difference migration spectralyzer array.
Fig. 2 A illustrates the structure that ion source and axisymmetricly difference ion mobility spectrometry analyzer array, quadrupole rod ion guides array, ion trap analyzer are contacted mutually.
Fig. 2 B illustrates the cross-section structure of the ion trap analysis array among Fig. 2 A.
Fig. 3 illustrates the structure that ion source and plate difference ion mobility spectrometry analyzer array, plate ion guides array, quadrupole rod mass analyzer array are contacted mutually.
Fig. 4 A illustrates the structure that ion source links to each other with difference ion mobility spectrometry analyzer array axisymmetricly, and its intermediate ion is evicted from through the backward ion detector array of quadrupole rod mass analyzer array, to reach the purpose of multichannel quality analysis.
Fig. 4 B illustrates the structure that ion source links to each other with difference ion mobility spectrometry analyzer array axisymmetricly, its intermediate ion is evicted from through the backward same ion detector of quadrupole rod mass analyzer array quality analysis, to reach the purpose of enrichment quality analysis or the quality analysis of timesharing shunting.
Fig. 5 A illustrates a kind of difference migration spectralyzer and the mutually perpendicular instrument configuration of next stage ion conveying device, and ion upwards distributes at one-dimensional square at the entrance of difference migration spectralyzer.
Fig. 5 B illustrates a kind of difference migration spectralyzer and the mutually perpendicular instrument configuration of next stage ion conveying device, and its intermediate ion distributes at two-dimensional direction at the entrance of difference migration spectralyzer.
Fig. 5 C illustrates the sectional view of the ion trap array with central ion detector.
Fig. 5 D illustrates the sectional view of the ion trap array with shunting ion detector.
Fig. 6 illustrates the structure that ion source and axisymmetricly difference ion mobility spectrometry analyzer array, ion guides array, ion trap analyzer array are contacted mutually, wherein pass through ion radially outgoing in the ion trap analyzer in each array channel, be positioned at this ion trap and analyze the detector array shunting of array periphery and detect.
Fig. 7 illustrates the structure of ion detection device of the present invention and the coupling of desorb corona beam ion source.
Fig. 8 illustrates according to an embodiment of the invention synchronously (DMAA)-asynchronous (ITA) pattern diagram.
Fig. 9 illustrates asynchronous according to an embodiment of the invention (DMAA)-asynchronous (ITA) pattern diagram.
Figure 10 illustrates the according to an embodiment of the invention ion analysis of ion trap array and the schematic diagram of timesharing outgoing.
Embodiment
Summarily say, embodiments of the invention relate to a kind of with difference ion mobility spectrometry analyzer array (Differential Mobility Analyzer Array, DMAA) with mass spectrometer array (Mass Spectrometer Array, MSA) thus the device that improves ion analyzer global analysis efficient of coupling and in order to improve the method for ion analysis efficient.
Embodiment one
As previously mentioned, when using the difference ion mobility spectrometry analyzer to carry out ion detection, the ion with different ionic mobilities is selected by changing difference ion mobility spectrometry analyzer migration voltage.When going for a spectrogram in the whole ionic mobility scope, just need carry out stepping scanning to the migration voltage of this analyzer.This process is usually very consuming time, and in order to reach balance when the each time stepping, the single pass time is usually time of several seconds to tens seconds.In order to increase the efficient of this analytic process, the method that can adopt multichannel to detect.Figure 1A illustrates the structure that ion source links to each other with plate difference ion mobility spectrometry analyzer array.Shown in Figure 1A, one ion source array 1 links to each other with a plate difference ion mobility spectrometry analyzer array (F-DMAA) 2, the ion of drawing from F-DMAA 2 can enter the plate ion trap array of next stage (F-ITA) 4 by an ion transfer passage array 3, evict from through the backward ion detector array 5 of quality analysis, to reach the purpose of quality analysis.
In the present embodiment, each unit among the F-DMAA 2, namely the structure of each passage is identical, and its cross section is as shown in Figure 1B.Ion entrance 2a is positioned at the relative same position of each passage, and the relative position of each channel ions exit slit is identical.Ion enters via the bottom slit 6 of F-DMAA passage, moves to the passage downstream with an air-flow that is parallel to channel direction.Simultaneously, ion one perpendicular to the effect of the DC electric field of airflow direction under to the top motion of parallel plate electrode.Because the movement velocity of the ion of different ions mobility under same electric field action is different, the stack of ion both direction speed is rear so that only have those ions with specific ion mobility to leave the migration area from top slit 7.
Above ion migration area both may operate under the atmospheric pressure, also may operate in background gas pressure is low to moderate under the low vacuum about 0.1torr (≈ 13.3322Pa) most, but the resolution capability for the ion migration analysis considers that the average gas pressure of ion migration area is not less than 0.1Torr usually.Therefore need through an ion transfer passage array 3 before entering F-ITA 4 after ion leaves F-DMAA 2, its effect provides a difference extraction zone that pressure is placed in the middle, improves the efficient of passing through of ion.Such ion transfer passage array can be a multistage bar array, an ion funnel array, or the array by a plurality of electrode slices or the formed multipole fields of wire electrode.By the ion of ion transfer passage array 3, can enter vertically the F-ITA 4 of next stage.Enter ion behind the F-ITA 4 after supercooling and scanning are evicted from, the corresponding unit that enters the ion detector array 5 that is positioned at side surface direction detects.
For this structure, multiple-working mode can be arranged.For example, each passage of F-DMAA 2 can be operated in synchronous mode, and namely institute's making alive equates on each passage, so the mobility of the ion that passes through of the selected property of each passage equates.Under this pattern, F-DMAA 2 only monitors a kind of ion of ionic mobility at synchronization.Monitor different kinds of ions such as need, this array need be operated under the step mode, namely changes between different migration voltage; Meanwhile, the F-ITA 4 that is attached thereto also can be operated under the synchronous mode, and namely the quality that detects of each ion trap unit or mass range equate.This pattern is quite all done as a whole analyzer use separately with F-DMAA 2 and F-ITA 4.Thereby the main purpose of this kind pattern is to improve the overall sensitivity of analyzer, but can not improve the speed of analysis.
Certainly, ion trap array also can be operated under the asynchronous mode, and namely the quality or the mass range that detect of each unit do not wait; Perhaps, several unit can form one group, detect identical quality or mass range.The main purpose of common this pattern is to detect the component with several different karyoplasmic ratios that comprises in the same ionic mobility ion.This screens the different component with analog structure compound in situation faster fast for F-DMAA 2 sweep speeds Special Significance.The pattern of this synchronously (F-DMAA 2)-asynchronous (F-ITA 4) as shown in Figure 8.The migration voltage that V1 to V5 representative is applied simultaneously at difference moment F-DMAA 2 each passage among Fig. 8, m1, m2, m3, m4 philosophy represent between the quality area of each passage scanning of mass spectrometer.For the mass spectrum asynchronous mode, these intervals are different, even can make each passage lock a certain special quality monitoring.When F-DMAA 2 sweep speed when very fast, complete mass range of scanning becomes very difficult for ion trap or quadrupole rod, above subchannel segmentation scans and just highlights its advantage.
For the synchronous mode of F-DMAA 2, it is more suitable in some sample concentration temporal evolution of monitoring is not very fast sampling process.Yet, when the prime analyzer (such as liquid phase or gas-chromatography) of F-DMAA 2 goes out the peak when very fast, use also difficult of scanning that F-DMAA 2 carries out complete spectrogram.At this moment can the mode of operation of F-DMAA 2 is asynchronous by changing into synchronously, the passage of each F-DMAA 2 is operated under different migration voltage or the migration voltage range, thereby monitors simultaneously multiple determinand, greatly reduce the time of the full spectrum of scanning.Certainly, for 2 each channel selecting of F-DMAA under asynchronous mode ion with different ions mobility out, when using follow-up F-ITA 4 to carry out the karyoplasmic ratio analysis, for F-ITA 4, both synchronous mode can be taked, also asynchronous mode can be taked.For the synchronous mode of F-ITA 4, the analyst is concerned about that more monitoring may have the same class ion of different spaces geometric configuration; And for the asynchronous mode of F-ITA 4, the analyst then more is concerned about each ion use karyoplasmic ratio with special ion mobility is confirmed, to reduce false-positive appearance.The latter is more suitable for replacing the present public safety field ionic migration spectrometer that only comes qualitative ion with ionic mobility commonly used.This process such as meaningful needs satisfy the requirement of two aspects, and at first, the interested ionic species of this testing process is not a lot (being no more than the overall channel number), and detect the before mobility known (to the monitoring of known sample) of all kinds of ions.Therefore, this process is more suitable for process conventional for some and the certain detection speed of needs, uses such as fields such as on-line monitoring and airport securitys.Fig. 9 has described the process of asynchronous (F-DMAA)-asynchronous (F-ITA) mode of operation.F-DMAA 2 each passage are within 0 to t1 sweep time, and each passage correspondence of the mass spectrometer array that it is corresponding is operated in m1 to m2, and m3 to m4 waits in the different working ranges.Under this pattern, F-DMAA 2 can monitor the ion of multiple different ions mobility at synchronization; Monitor that the ionic species number is determined by passage number in the described array; This moment, the migration voltage of F-DMAA 2 each passage can remain on a fixed value (V1, V2, V3, and V4) as shown in Figure 9, with a certain ion of persistent surveillance.The migration voltage of each passage of F-DMAA2 also can be a different narrow range interscan, with the ion information in the whole mobility scope of quick acquisition.
In addition, the ion source in the present embodiment also can be the isotopic ion source, and this isotopic ion source can optionally be opened or close by mechanical device according to the experiment needs.Like this, by using each passage of ion analyzer respectively certain specific ion that the isotopic ion source produces regularly to be detected, final each passage can be used for calibrating the object ion intensity that finally records in each passage after resulting ionic strength normalization on the described ion detector.
Embodiment two
The basic principle of the ion analyzer in the present embodiment is similar to embodiment one, but difference is that difference ion mobility spectrometry analyzer array (DMAA) and ion trap array (ITA) all adopt drum type brake in the present embodiment, be called for short respectively C-DMAA 11 and C-ITA 13, connect by cylindric ion transfer passage array 12 between the two, shown in Fig. 2 A.In this embodiment, each passage of C-DMAA 11 structure that is centrosymmetric, the corresponding center line of each passage distributes in radial symmetric.Fig. 2 B further illustrates the cross-section structure of C-ITA 13, each analytic unit is a complete circumference type and distributes in the array around same axis, and this can be so that the ion of a plurality of analytic unit institute outgoing further focuses on outgoing on the axis of device from array.
In addition, outlet that can be on C-ITA 13 end caps etc. locates to set up respectively axial outgoing ion detector etc., detects respectively the ion that evict from each ion analysis unit, or comes all ions of same detection with the detector of a large receptor area.
The structure of present embodiment has been compared some advantages with the slab construction among the upper embodiment.For example, because cylindrical structure is symmetrical for the axis, therefore ion source array and ion detector array can be reduced to independent ion source 10 and ion detector 14, guarantee that simultaneously each passage has relatively uniformly response.Moreover, can further reduce the quantity of follow-up signal amplifier and data acquisition channel for the simplification of ion detector 14, so that whole instrument cost reduces.
Under this instrument configuration structure, the various work among the upper embodiment reach synchronously asynchronous pattern and all are suitable for.Certainly, ion detector quantity is being reduced in one, the sequential that comprises asynchronous mode (DMAA and ITA are at least a to be asynchronous mode) in the ion detection process is also needed to adjust to some extent.Figure 10 has expressed under asynchronous (DMAA)-asynchronous (ITA) pattern when using an independent ion detector the special sequencing control to ITA.As shown in figure 10, each passage of DMAA is operated under the different migration voltage (V1 to V4), and the ITA unit of corresponding each DMAA passage can roughly switch between 3 working stages, and ion trap empties-ion introducing and enrichment-Ion Extraction.In this three phases, ion introduce and enrichment stage required time the longest, usually can continue tens to the hundreds of millisecond, and that ion trap empties required time is very short, common tens microseconds are just enough.And for time in Ion Extraction stage, need to determine according to the scope of concrete quality of scanning, if the scanning of carrying out in the total quality scope is evicted from, need at least tens milliseconds.But because each passage of DMAA has carried out certain differentiation with ion according to different mobilities, therefore, ion and certain mass scope that can each DMAA passage is selected combine, even the only corresponding special karyoplasmic ratio of each passage.The time of each the ion trap unit scan among the C-ITA 13 can foreshorten to a hundreds of microsecond like this, only accounts for ion trap very little share in analysis time, and this has just created condition for ion detector of each ion trap units shared.Therefore as long as the scanning time of evicting from of each ion trap unit is staggered, just can take full advantage of the service time of ion detector, thereby be more or less the same when making the duty ratio of whole system and using the ion detector array as ion detector.
Certainly, for C-ITA 13, also can an ion detector be installed for each ion trap passage, and be equipped with independently amplifier and data acquisition system.At this moment the operation of each passage will be fully independently, and this pattern that is combined in the running with F-DMAA and F-ITA is duplicate.This pattern is more suitable in each ion trap being carried out total quality scanning.
Embodiment three
The basic principle of the ion analyzer in the present embodiment and embodiment one are quite similar, but difference is that the mass analyzer array adopts the level Four bar array in the present embodiment.As shown in Figure 3, a F-DMAA unit among each the root level Four bar in the plane level Four bar array (F-QA) 15 and the F-DMAA 2 links to each other by a plate ion transfer passage array 3.Similar to precedent, the unit of F-QA 15 can be operated under the different mode according to circumstances, makes up with the different working modes with F-DMAA 2, thereby adapts to different application demands.For example, when each passage of F-DMAA 2 is operated in synchronous mode lower time, all unit of F-QA 15 also are operated under the synchronous mode, to increase a certain ion are monitored and sensitivity when confirming.Perhaps, the different units of F-QA 15 also can be divided into several groups, thereby the ion of analog structure is monitored in different possible mass ranges.When F-DMAA 2 each passage are operated in asynchronous mode lower time, then to be operated in the purpose under the synchronous mode be that multiple isomer is monitored to F-QA 15, obtains it relatively and absolute content information.At last, when F-DMAA 2 and F-QA 15 were operated in asynchronous mode, different passages will be for different, proprietary ionic mobility-ion karyoplasmic ratio pair, thereby effectively screens different types of ion.
Shown in Fig. 4 A, also can use the combination of the level Four bar array (C-QA) 16 of difference ion mobility spectrometry analyzer array (C-DMAA) 11 of similar embodiment two cylindrical structures and cylindric distribution to carry out ion analysis.The ion of drawing from C-DMAA 11 can enter next stage C-QA 16 by an ion transfer passage array 12 cylindraceous, evicts from through the backward ion detector array 17 of quality analysis, to reach the purpose of quality analysis.The advantage of using this structure is that total is symmetrical with the cylinder axle center, therefore is suitable for the generation ion of independent ion source 10 is imported.At this moment, the operational mode of whole ion analyzer is identical with the operational mode of aforementioned slab construction.
Furthermore, shown in Fig. 4 B, each unit of the level Four bar array 16 of cylindric distribution also can be mutually close, by exporting by a cylinder conversion dynode 18.Then the ion detector array with the rear portion further is reduced to an independent ion detector 14, to reduce the cost of detector and rear class Signal Collection and amplify.But, because level Four bar mass spectrum is usually operated under the continuous mode, use the difference of level Four bar array and ion trap array to be that ion can not carry out enrichment (by contrast in testing process, the time that the ion of each unit is evicted time relative ion cooling enrichment etc. from the ion trap array is wanted much shorter), therefore use independent ion detector that each passage of level Four bar array is carried out the greatly analysis efficiency of lowering apparatus of timesharing detection meeting.So at this moment whole ion detector preferably is operated under the full synchronous mode.
It is worthy of note, even whole ion analyzer is operated under the full synchronous mode (no matter be difference ion mobility spectrometry analyzer and ion trap array or with the combination of quadrupole rod array), adopt multichannel mode that its advantage is also arranged.Reason is, the amount of ions of generally ion source generation can be far longer than the amount of ions that ion analyzer can be introduced and utilize, especially for the difference ion mobility spectrometry analyzer, increase ion intake size and can increase the degree that stream field destroys, thereby affect resolution and the stability of instrument.And for the mass analyzer of rear class, for identical ionic flux, multi-channel structure can reduce the size of every channel quality analyzer, thereby reduces the voltage request of mass analyzer, and this also provides prerequisite for miniaturization, the portability of ion analyzer.
Embodiment four
For the combination of F-DMAA and F-ITA or F-QA among embodiment one and three, other geometry can also be arranged.Shown in Fig. 5 A, can allow the plate ion transfer passage array 3 vertical placements of F-DMAA 2 (i.e. airflow direction shown in the figure) and next stage, so that importing and exporting, the air-flow of front and back is easier to place.
Such displacement structure can also have a kind of variant, and the intake 2a with each passage of F-DMAA 2 shown in Fig. 5 B arranges according to centrosymmetric mode, and corresponding Ion Extraction mouth 2b is also by identical structural arrangement therewith.The periphery of C-ITA 13 arranges shunting ion detector 19 radially simultaneously.The benefit of this arrangement mode be such F-DMAA 2 just can with embodiment two in ion source 10 and C-ITA 13 couplings, reduce the quantity of desired ion source and detector and subsequent acquisition amplifying device.
Fig. 5 C, 5D illustrate the profile of ion trap array.Shown in Fig. 5 C, can a common ion detector 14 of evicting total ion current for detection of each passage from be set at the place, axis of ion trap array, this detector 14 also available first dynode that passes through on this axis replaces, so that detector body can be arranged into other correct positions, so the central ion detection system of design can be used for the collectiong focusing outgoing on the axis of device ion current and delivering to the enhancing that takes a step forward of analog-to-digital conversion harvester.When ion trap array is longer, draws ion from the axis and can be subject to the shielding of ion trap array body electrode and difficult because ion detector is drawn electric field.Can shown in Fig. 5 D, arrange a plurality of shuntings ion detector 19 or their a plurality of the first dynodes at axis in this case, wherein the corresponding ion of radially being evicted from by each analytic unit in the axial certain limit that detects of each ion detector.
Embodiment five
In the various embodiments described above for the combination of difference ion mobility spectrometry analyzer array and mass spectrometer array, thereby the ion that all is based on obtaining after selecting according to ionic mobility directly carries out the concept that quality analysis obtains the ion qualitative information.Yet for most of isomers, the difference of its molecular structure probably is not so large as to be enough to be separated by the difference ion mobility spectrometry analyzer.Therefore, between difference ion mobility spectrometry analyzer and mass spectrometer, increase an ionic dissociation device, be necessary thereby can make ion analyzer monitor to become for a certain daughter ion of the ion with a certain ionic mobility.The ion that this process is similar in the triple quadrupole mass spectrum is selected reaction monitoring (SRM) pattern.Under this pattern, coming from the chemical noises that the weakness of the lack of resolution of difference ion mobility spectrometry analyzer causes can be suppressed greatly by the peculiar daughter ion of monitoring certain isomer.Each cell operation of the segregant of being on duty migration spectralyzer array is in asynchronous mode lower time, and this ion analyzer can be operated in and be similar under the mass spectral:mass spectrographic ion multiple-reaction monitoring of triple quadrupole (MRM) pattern.Because under asynchronous mode, each passage is independent and works simultaneously separately, therefore can accomplish to monitor simultaneously to each reaction monitoring passage, has avoided the process that need to switch one by one at each interchannel, can greatly improve the detection efficiency of whole instrument.
A simple case of ionic dissociation device is a collision cell that is filled with the certain pressure collision gas.As shown in Figure 6, the collision cell array 21 with cylindric distribution is placed between C-DMAA 11 and the C-ITA 13, and it can under lower vacuum degree, will dissociate by colliding with neutral gas from the ion that each passage of C-DMAA is introduced.The mother who obtains after dissociating, daughter ion can carry out the karyoplasmic ratio analysis at the auxiliary lower mass spectrometer array that is focused on and finally enter rear class of alternating electric field.Mass spectrometer described here both can be that quadrupole rod array 16 (C-QA) also can be ion trap array 13 (C-ITA).
In other embodiments, the ionic dissociation device can also be a photodissociation chamber, in the collision of the laser of this ion and high energy and dissociate.The ionic dissociation device can also be an electron capture dissociation chamber, interacts and is dissociated at this ion and electron beam.
Embodiment six
For aforementioned each structure, its purpose all is to carry out effective separation and detection for the complicated ions mixture that will come from after liquid chromatogram is separated.Because difference ion mobility spectrometry analyzer itself just has certain separating power to complex sample, therefore also can adopt a kind of atmospheric pressure Direct Analysis ion source and the direct coupling of described ion analyzer, reach slowly the numerous and diverse shortcoming of sample preparation to exempt the analysis speed that uses liquid chromatogram to bring.
Fig. 7 has showed and has a kind ofly carried out the direct desorption ionization of sample with Chinese patent application 200810188989.8 disclosed desorb corona beam, then uses above-mentioned ion analyzer to carry out the device of ion analysis.In this device, to electrode 33, high voltage source 34, heating power supply 35, and the desorb corona beam that produces forms desorb corona beam ion source by gas-heated pipe 31, spray point 32, ground connection.The ion 36 that is desorbed corona beam ion source desorption ionization is introduced in each passage of C-DMAA 11 by further separation and detection as far as possible equably.The detection signal of channel ions detector 19 is sent into collecting device 23 after amplifying through channel amplifier 22.
Embodiment seven
For aforementioned each structure, because each entrance present position of difference ion mobility spectrometry analyzer array is different, the population of ions amount that therefore may cause each passage to enter is different, thereby causes the signal proportion distortion of ion measured in each passage.In order to address this problem, can form array at ion current detector of connection of each ion intake rear end, and the ion current detector array links to each other with the current sensing means of outside, and the current signal of the ion introducing amount of each passage of sign that will record in real time importing data acquisition system compares.The simple structure of this ion current detector can realize with the little metallic plate array of an additional bias voltage.When the ion current source was chromatogram isopulse form ion source, can make bias voltage was the top crown voltage of difference ion mobility spectrometry analyzer, detects this total ion current situation of change with the image current method.When the strong variation of ion current is slow or constant, also can adopt the method for this ion current detector and rear class mass detector time-sharing multiplex, for example in every 20ms, take the 0.5ms time wherein, during this period of time the current potential of each the discrete Detection electrode in the array 20 is drawn negative to electronegative potential such as-200V, so that all cation stream is directed on this pole plate, and the current potential of the discrete Detection electrode of other times can return to the required normal value of difference ion mobility spectrometry analyzer.Change slowly because ion current is strong, always detect electric weight with each unit inspection pole plate gained in this 0.5ms and do the curent change data that a simple transformation of scale and polynomial interopolation can represent this passage of inflow.
No matter be to use the alternating current impression method or the time-sharing multiplex method obtains ion current signal before the integral array analytical equipment, because this current signal has reflected the total amount of ion before separating that will enter in each passage, this value should be independent of employed channel position in the ideal case.According to the measured current value of different passage front ends, can carry out normalization to the final measured ionic strength of each passage, be used for calibrating the object ion intensity that finally records in each passage, consistent with actual each component ion concentration ratio with the proportionate relationship that guarantees each ion channel object ion intensity.
Further, each passage in the combination of aforesaid any DMAA and MSA regularly can also be detected respectively the same material that comes from a stabilizing ion source, in order to revise the difference of each channel transfer ion efficiency.
As the summary for the mode of operation of the described ion detector array of above each embodiment, following table 1 illustrates the according to an embodiment of the invention combination of DMAA and the various mode of operations of ITA and sums up chart, makes embodiments of the invention more clear.
Table 1
Because difference ionic migration spectrometer array can be operated under synchronous mode or the asynchronous mode, the mass spectrometer array also can be operated under synchronous mode or the asynchronous mode.Ion analysis method of the present invention comprises with the variation of signal in the sampling process to be switched the mode of operation of difference ionic migration spectrometer array and/or mass spectrometer array, to obtain desired performance, such as high-resolution, high sensitivity, high efficiency etc.
It is worthy of note that in addition except the disclosed structure of above-described embodiment, the present invention can also use existing ion trap analyzer array and use with the coupling of ion mobility spectrometry array.For example, Fudan University's fourth passes ion storage and the analytical equipment array that all people of grade propose in Chinese patent application 200610001017.4 and U.S. Patent application 2009/0294655 A1.And for example, the column type ion trap array that Purdue University RG Cook seminar proposes in the US Patent No. 6762406 and after the column type ion trap array mass analyzer chip based on micromechanics and micro-processing technology (MEMS) made of the people such as Ramsy.Or in Chinese patent application 200910054963.9, the Pan Xin of Fudan University waits in the deep pool people further to simplify the designed PCB electrode parallel array structure ion trap of all people of grade of above-mentioned fourth biography from electrode structure.
The present invention also can come to use with the coupling of ion mobility spectrometry array with other quadrupole rod analyzer arrays.For example, the people such as Ferran are at United States Patent (USP) 5401962 and J.Vac.Sci.Technol.A, and 1996, Vol 14 (3), describes among the p1258, and the equality people of fourth army (mass spectrum journal, Vol22, No.3,29-35.) the ten sextupole mass spectrograph arrays that develop on this basis.Relatively common quadrupole rod analyzer, such mass spectrometer array has the characteristics such as volume is little, quality is clear, low in energy consumption.
Although the present invention discloses as above with preferred embodiment; so it is not to limit the present invention, any those skilled in the art, without departing from the spirit and scope of the present invention; when can doing a little modification and perfect, so protection scope of the present invention is when with being as the criterion that claims were defined.For example, used ion source is not electron spray, but the Atmosphere Pressure Chemical Ionization (APCI) source; Not desorb corona beam ion source, but desorption electrospray source (DESI) or direct real-time analysis ion source (DART).For another example, described ion analyzer not only can with liquid chromatogram or direct analyzing method coupling, also can with Capillary Electrophoresis or gas-chromatography coupling.
Claims (21)
1. an ion analyzer comprises the ion source or ion source array, difference ion mobility spectrometry analyzer array, ion transfer passage array, mass spectrometer array and ion detector or the ion detector array that link to each other successively, wherein:
Described difference ion mobility spectrometry analyzer array, described ion transfer passage array, each self-contained two or more passage of described mass spectrometer array, and a passage of the corresponding at least described mass spectrometer array of a passage of each described difference ion mobility spectrometry analyzer array.
2. ion analyzer according to claim 1 is characterized in that, described mass spectrometer array is level Four bar array or ion trap array.
3. ion analyzer according to claim 1 is characterized in that, also comprises the ionic dissociation device, is located between described ion transfer passage array and the described mass spectrometer array.
4. ion analyzer according to claim 3 is characterized in that, described ionic dissociation device is gas collisions chamber or photodissociation chamber or electron capture dissociation chamber.
5. ion analyzer according to claim 1 is characterized in that, described difference ion mobility spectrometry analyzer array is planar structure, and the ion entrance is positioned at the relative same position of each passage, and the relative position of each channel ions exit slit is identical.
6. ion analyzer according to claim 1 is characterized in that, described each passage of difference ion mobility spectrometry analyzer array structure that is centrosymmetric, and the corresponding center line of each passage distributes in radial symmetric.
7. ion analyzer according to claim 1 is characterized in that, each unit of described mass spectrometer array is equipped with independently ion detector and data acquisition amplification system.
8. ion analyzer according to claim 1 is characterized in that, each unit of described mass spectrometer array be centrosymmetric structure and ion detector of each units shared and data acquisition system.
9. ion analyzer according to claim 1 is characterized in that, described difference ionic migration spectrometer array is to be operated under synchronous mode or the asynchronous mode, and described mass spectrometer array is to be operated under synchronous mode or the asynchronous mode.
10. ion analyzer according to claim 1 is characterized in that, the work of described difference ion mobility spectrometry analyzer array under atmospheric pressure.
11. ion analyzer according to claim 1 is characterized in that, described difference ion mobility spectrometry analyzer array is operated under the environment that is lower than atmospheric pressure but is not less than 0.1torr.
12. ion analyzer according to claim 1 is characterized in that, the airflow direction in the described difference migration spectralyzer array is axial vertical with described ion transfer passage array.
13. ion analyzer according to claim 1 is characterized in that, each feeder connection place of described difference migration spectralyzer array is provided with an ion current detector, and described ion current detector links to each other with the current sensing means of outside.
14. ion analyzer according to claim 1 is characterized in that, described ion source comprises an isotopic ion source, and described isotopic ion source can optionally be opened or close by mechanical device according to the experiment needs.
15. the ion analysis method of the ion analyzer of a right to use requirement 1, comprise each passage of the ion of ion source or the generation of ion source array being introduced difference ion mobility spectrometry analyzer array, after each passage carries out selection based on ionic mobility, through entering the mass spectrometer array behind the ion transfer passage array and finally being detected by ion detector or ion detector array.
16. method according to claim 15 is characterized in that, also comprises making ion before entering each passage of described mass spectrometer array, is introduced into an ionic dissociation device, so that ion can describedly dissociate in the ionic dissociation device.
17. method according to claim 15, it is characterized in that, described difference ionic migration spectrometer array is to be operated under synchronous mode or the asynchronous mode, described mass spectrometer array is to be operated under synchronous mode or the asynchronous mode, and described method comprises with the variation of signal in the sampling process to be switched the mode of operation of described difference ionic migration spectrometer array and/or described mass spectrometer array.
18. method according to claim 15 is characterized in that, comprises to use level Four bar array or ion trap array as described mass spectrometer array.
19. method according to claim 15 is characterized in that, when using a described ion detector, described method comprises that the mode that adopts Time share scanning to evict from surveys the ion information of each passage.
20. method according to claim 15, it is characterized in that, also comprise and use an ion current detector that is positioned at each feeder connection place of difference ion mobility spectrometry analyzer array, ion introducing amount to each passage is monitored, after the described ion strength of flow normalization of resulting each passage, be used for calibrating the object ion intensity that finally records in each passage.
21. method according to claim 15, it is characterized in that, comprise the isotopic ion source that is arranged in described ion source of using, and by using each passage of described ion analyzer respectively certain specific ion that described isotopic ion source produces regularly to be detected, final each passage is used for calibrating the object ion intensity that finally records in each passage after resulting ionic strength normalization on the described ion detector.
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| CN104716006A (en) * | 2013-12-13 | 2015-06-17 | 中国科学院大连化学物理研究所 | Connector shared by ion migration spectrum and mass spectrum |
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