EP1271610A2 - Spectromètre de masse - Google Patents

Spectromètre de masse Download PDF

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Publication number
EP1271610A2
EP1271610A2 EP02254394A EP02254394A EP1271610A2 EP 1271610 A2 EP1271610 A2 EP 1271610A2 EP 02254394 A EP02254394 A EP 02254394A EP 02254394 A EP02254394 A EP 02254394A EP 1271610 A2 EP1271610 A2 EP 1271610A2
Authority
EP
European Patent Office
Prior art keywords
fragmentation cell
electrodes
ions
mass spectrometer
voltage
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
EP02254394A
Other languages
German (de)
English (en)
Other versions
EP1271610A3 (fr
EP1271610B1 (fr
Inventor
Robert Harold Bateman
Kevin Giles
Steve Pringle
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Micromass UK Ltd
Original Assignee
Micromass UK Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from GB0115429A external-priority patent/GB0115429D0/en
Priority claimed from GB0120122A external-priority patent/GB0120122D0/en
Priority claimed from GB0206164A external-priority patent/GB0206164D0/en
Application filed by Micromass UK Ltd filed Critical Micromass UK Ltd
Priority to EP04026519A priority Critical patent/EP1505634B1/fr
Publication of EP1271610A2 publication Critical patent/EP1271610A2/fr
Publication of EP1271610A3 publication Critical patent/EP1271610A3/fr
Application granted granted Critical
Publication of EP1271610B1 publication Critical patent/EP1271610B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/02—Details
    • H01J49/06—Electron- or ion-optical arrangements
    • H01J49/062—Ion guides
    • H01J49/065—Ion guides having stacked electrodes, e.g. ring stack, plate stack
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/004—Combinations of spectrometers, tandem spectrometers, e.g. MS/MS, MSn
    • H01J49/0045—Combinations of spectrometers, tandem spectrometers, e.g. MS/MS, MSn characterised by the fragmentation or other specific reaction
    • H01J49/005—Combinations of spectrometers, tandem spectrometers, e.g. MS/MS, MSn characterised by the fragmentation or other specific reaction by collision with gas, e.g. by introducing gas or by accelerating ions with an electric field

Definitions

  • the present invention relates to mass spectrometers.
  • a known fragmentation cell comprises a multipole (e.g. a quadrupole or hexapole) rod set wherein adjacent rods are connected to opposite phases of an RF voltage supply.
  • the quadrupole or hexapole collision cell is housed in a cylindrical housing which is open at an upstream end and at a downstream end to allow ions to enter and exit the collision cell.
  • the housing includes a gas inlet port through which a collision or buffer gas, typically nitrogen or argon, is introduced into the collision cell.
  • the collision cell is maintained at a pressure of 10 -3 -10 -2 mbar.
  • Ions entering the collision cell are arranged to be sufficiently energetic so that when they collide with the collision or buffer gas at least some of the ions will fragment into daughter or fragment ions by means of Collisional Induced Dissociation/Decomposition ("CID"). Ions in the collision cell will also become thermalised after they have undergone a few collisions i.e. their kinetic energy will be considerably reduced, and this leads to greater radial confinement of the ions in the presence of the RF electric field. In order to ensure that ions are sufficiently energetic so as to fragment when entering the collision cell, the collision cell is typically maintained at a DC potential which is offset from that of the ion source by approximately -30V DC or more (for positive ions).
  • ions Once ions have fragmented and have been thermalised within the collision cell, their low kinetic energy is such that they will tend to remain within the collision cell. In practice, ions are observed to exit the collision cell after a relatively long period of time, and this is believed to be due to the effects of diffusion and the repulsive effect of further ions being admitted into the collision cell.
  • ions tend to have a relatively long residence time within the collision cell. This is problematic for certain types of mass spectrometry methods since it is necessary to wait until ions have exited the collision cell before further ions are admitted into it.
  • MS/MS i.e. fragmentation
  • a quadrupole mass filter Q1 (MS1) upstream of a collision cell Q2 is scanned rapidly compared to the typical empty time ( ⁇ 30ms) of ions to exit the collision cell Q2
  • MS1 quadrupole mass filter
  • ⁇ 30ms typical empty time
  • the fragmentation cell according to the preferred embodiment is capable of being emptied of and filled with ions much faster than a conventional collision cell. Mass spectra obtained using the preferred fragmentation cell exhibit improved resolution and greater sensitivity.
  • the fragmentation cell may comprise 10-20, 20-30, 30-40, 40-50, 50-60, 60-70, 70-80, 80-90, 90-100, 100-110, 110-120, 120-130, 130-140, 140-150, or >150 electrodes.
  • the fragmentation cell may have a length ⁇ 5 cm, 5-10 cm, 10-15 cm, 15-20 cm, 20-25 cm, 25-30 cm, or >30 cm.
  • at least 10%, 20%, 30%, 40%, 50%, 60%, 70%, 80%, 90%, or 95% of the electrodes are connected to both a DC and an AC or RF voltage supply.
  • an axial DC voltage difference of approximately 3V may be maintained along the whole length of the fragmentation cell (i.e.
  • electrodes at the downstream end of the fragmentation cell are maintained at a DC voltage approximately 3V below electrodes at the upstream end of the fragmentation cell).
  • the axial DC voltage difference maintained along at least a portion, preferably the whole length, of the fragmentation cell is 0.1-0.5 V, 0.5-1.0 V, 1.0-1.5 V, 1.5-2.0 V, 2.0-2.5 V, 2.5-3.0 V, 3.0-3.5 V, 3.5-4.0 V, 4.0-4.5 V, 4.5-5.0 V, 5.0-5.5 V, 5.5-6.0 V, 6.0-6.5 V, 6.5-7.0 V, 7.0-7.5 V, 7.5-8.0 V, 8.0-8.5 V, 8.5-9.0 V, 9.0-9.5 V, 9.5-10.0 V or > 10V.
  • the electrodes forming the fragmentation cell are supplied with an AC or RF voltage which can be considered to be superimposed upon the DC potential supplied to the electrodes.
  • adjacent electrodes are connected to opposite phases of an AC or RF supply but according to other less preferred embodiments adjacent electrodes may be connected to different phases of the AC or RF supply i.e. voltage supplies having more than two phases are contemplated.
  • the AC or RF voltage supplied to the electrodes has a sinusoidal waveform (with a frequency 0.1-3.0 MHz, preferably 1.75 MHz), non-sinusoidal waveforms including square waves may be supplied to the electrodes.
  • ions may be trapped within the fragmentation cell in a mode of operation.
  • Embodiments are contemplated wherein ions may be trapped in a downstream portion of the fragmentation cell whilst ions may be continually admitted into an upstream portion of the fragmentation cell.
  • V-shaped axial DC potential profiles may be used to accelerate and trap ions within the collision cell.
  • the fragmentation cell is preferably maintained, in use, at a pressure > 1.0 x 10 -3 mbar, > 5.0 x 10 -3 mbar, > 1.0 x 10 -2 mbar, 10 -3 -10 -2 mbar, or 10 -4 -10 -1 mbar.
  • the mass spectrometer preferably comprises a continuous ion source, further preferably an atmospheric pressure ion source, although other ion sources are contemplated.
  • Electrospray (“ESI”), Atmospheric Pressure Chemical Ionisation (“APCI”), Atmospheric Pressure Photo Ionisation (“APPI”), Matrix Assisted Laser Desorption Ionisation (“MALDI”), non-matrix assisted Laser Desorption Ionisation, Inductively Coupled Plasma (“ICP”), Electron Impact (“EI”) and Chemical Ionisation (“CI”) ion sources may be provided.
  • a mass spectrometer comprising: an ion source; one or more ion guides; a first quadrupole mass filter; a fragmentation cell for fragmenting ions, the fragmentation cell comprising a plurality of electrodes having apertures through which ions are transmitted in use, wherein at least some of the electrodes are connected to both a DC and an AC or RF voltage supply and wherein an axial DC voltage gradient or difference is maintained in use along at least a portion of the length of the fragmentation cell; a second quadrupole mass filter; and a detector.
  • a mass spectrometer comprising: an ion source; one or more ion guides; a quadrupole mass filter; a fragmentation cell for fragmenting ions, the fragmentation cell comprising a plurality of electrodes having apertures through which ions are transmitted in use, wherein at least some of the electrodes are connected to both a DC and an AC or RF voltage supply and wherein an axial DC voltage gradient or difference is maintained in use along at least a portion of the length of the fragmentation cell; and a time of flight mass analyser.
  • the fragmentation cell comprises a plurality of segments, each segment comprising a plurality of electrodes having apertures through which ions are transmitted and wherein all the electrodes in a segment are maintained at substantially the same DC potential and wherein adjacent electrodes are supplied with different phases of an AC or RF voltage.
  • a mass spectrometer comprising: a first mass filter/analyser; a fragmentation cell for fragmenting ions, the fragmentation cell being arranged downstream of the first mass filter/analyser and comprising at least 20 electrodes having apertures through which ions are transmitted in use, wherein at least 75% of the electrodes are connected to both a DC and an AC or RF voltage supply and wherein a non-zero axial DC voltage gradient or difference is maintained in use along at least 75% of the length of the fragmentation cell; and a second mass filter/analyser arranged downstream of the fragmentation cell.
  • the first mass filter/analyser comprises a quadruople mass filter/analyser and the second mass filter comprises a quadrupole mass filter/analyser or a time of flight mass analyser.
  • a mass spectrometer comprising: a fragmentation cell comprising ⁇ 10 ring or plate electrodes having substantially similar internal apertures between 2-10 mm in diameter arranged in a housing having a buffer gas inlet port, wherein a buffer gas is introduced in use into the fragmentation cell at a pressure of 10 -4 -10 -1 mbar and wherein a DC potential gradient or difference is maintained, in use, along the length of the fragmentation cell.
  • a mass spectrometer comprising: an ion source; a fragmentation cell for fragmenting ions, the fragmentation cell comprising at least ten plate-like electrodes arranged substantially perpendicular to the longitudinal axis of the fragmentation cell, each electrode having an aperture therein through which ions are transmitted in use, the fragmentation cell being supplied in use with a collision gas at a pressure ⁇ 10 -3 mbar, wherein adjacent electrodes are connected to different phases of an AC or RF voltage supply and a DC potential gradient ⁇ 0.01 V/cm is maintained over at least 20% of the length of the fragmentation cell; and ion optics arranged between the ion source and the fragmentation cell; wherein in a mode of operation the ion source, ion optics and fragmentation cell are maintained at potentials such that singly charged ions are caused to have an energy ⁇ 10 eV upon entering the fragmentation cell so that at least some of the ions fragment into daughter ions.
  • At least some of the electrodes are also connected to a DC voltage supply and wherein an axial DC voltage gradient or difference is maintained in use along at least a portion of the length of the fragmentation cell.
  • a mass spectrometer comprising: a fragmentation cell in which ions are fragmented in use, the fragmentation cell comprising a plurality of electrodes having apertures through which ions are transmitted in use, and wherein in a mode of operation an upstream portion of the fragmentation cell continues to receive ions into the fragmentation cell whilst a downstream portion of the fragmentation cell separated from the upstream portion by a potential barrier stores and periodically releases ions.
  • the peak amplitude of the AC or RF voltage is ⁇ 200 V Pp , ⁇ 150 V Pp , ⁇ 100 V Pp , or ⁇ 60 V Pp .
  • Each ion tunnel segment 4a;4b;4c comprises two interleaved and electrically isolated sections i.e. an upper and lower section.
  • the ion tunnel segment 4a closest to the entrance aperture 2 preferably comprises ten electrodes (with five electrodes in each section) and the remaining ion tunnel segments 4b,4c preferably each comprise eight electrodes (with four electrodes in each section). All the electrodes are preferably substantially similar in that they have a central substantially circular aperture (preferably 5 mm in diameter) through which ions are transmitted.
  • All the eight (or ten) electrodes 5 in an ion tunnel segment 4a;4b;4c comprised of two separate sections are preferably maintained at substantially the same DC voltage.
  • Adjacent electrodes in an ion tunnel segment 4a;4b;4c comprised of two interleaved sections are connected to different, preferably opposite, phases of an AC or RF voltage supply i.e. one section of an ion tunnel segment 4a;4b;4c is connected to one phase (RF+) and the other section of the ion tunnel segment 4a;4b;4c is connected to another phase (RF-).
  • the fragmentation cell 1 was set to operate in a fragmentation mode with the fragmentation cell 1 being held at approx. 35V DC below the DC potential at which the ion source is held so that ions are sufficiently energetic when entering the fragmentation cell 1 that they fragment when they collide with collision gas in the fragmentation cell 1.
  • a downstream quadrupole mass filter Q3 (MS2) was set so as to transmit only daughter ions having a mass to charge ratio of 195.
  • the sample used was 50 pg/ ⁇ l reserpine (having a mass to charge ratio of 609) infused at 5 ⁇ l/min. Results are shown for applied axial DC voltage differences of 0V, 3V, 5V and 10V across the length of the whole fragmentation cell 1.
  • Fig. 12(a) shows the transmission characteristics for ions having a mass to charge ratio of 117
  • Fig. 12(b) for ions having a mass to charge ratio of 609
  • Fig. 12(c) for ions having a mass to charge ratio of 1081
  • Fig. 12(a) shows the transmission characteristics for ions having a mass to charge ratio of 117
  • Fig. 12(b) for ions having a mass to charge ratio of 609
  • Fig. 12(c) for ions having a mass to charge ratio of 1081
  • Fig. 12(a) shows the transmission characteristics for ions having a mass to charge ratio of 117
  • Fig. 12(b) for ions having a mass to charge ratio of 609
  • Fig. 12(c) for ions having a mass to charge ratio of 1081
  • Fig. 13 shows the intensity of daughter ions having a mass to charge ratio of 173 produced by fragmenting a high mass cluster from NaRbCsI (having a mass to charge ratio of 2872) in a daughter ion MS/MS experiment as a function of the amplitude of the applied RF voltage with and without a 3V DC voltage difference being maintained along the length of the fragmentation cell 1.
  • the amplitude of the RF voltage required for maximum transmission is closer to that of the higher mass to charge ratio parent ion than that of the lower mass to charge ratio daughter ion.
  • the application of an axial DC voltage gradient improves the intensity of the signal compared with no axial DC voltage gradient. Similar results were obtained using PPG 3000 and also for lower mass parent ions.

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
  • Electron Tubes For Measurement (AREA)
EP02254394.6A 2001-06-25 2002-06-24 Spectromètre de masse Expired - Lifetime EP1271610B1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP04026519A EP1505634B1 (fr) 2001-06-25 2002-06-24 Spectromètre de masse

Applications Claiming Priority (8)

Application Number Priority Date Filing Date Title
GB0115429 2001-06-25
GB0115429A GB0115429D0 (en) 2001-06-25 2001-06-25 Mass spectrometers and methods of mass spectrometry
GB0120122A GB0120122D0 (en) 2001-06-25 2001-08-17 Gas collision cell
GB0120122 2001-08-17
GB0120096 2001-08-17
GB0120096A GB0120096D0 (en) 2001-06-25 2001-08-17 Mass spectrometers and methods of mass spectrometry
GB0206164 2002-03-15
GB0206164A GB0206164D0 (en) 2001-06-25 2002-03-15 Mass spectrometer

Related Child Applications (2)

Application Number Title Priority Date Filing Date
EP04026519A Division EP1505634B1 (fr) 2001-06-25 2002-06-24 Spectromètre de masse
EP04026519A Division-Into EP1505634B1 (fr) 2001-06-25 2002-06-24 Spectromètre de masse

Publications (3)

Publication Number Publication Date
EP1271610A2 true EP1271610A2 (fr) 2003-01-02
EP1271610A3 EP1271610A3 (fr) 2004-10-13
EP1271610B1 EP1271610B1 (fr) 2017-12-27

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Family Applications (1)

Application Number Title Priority Date Filing Date
EP02254394.6A Expired - Lifetime EP1271610B1 (fr) 2001-06-25 2002-06-24 Spectromètre de masse

Country Status (3)

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EP (1) EP1271610B1 (fr)
CA (1) CA2391148C (fr)
GB (1) GB2381949C (fr)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2391698A (en) * 2002-05-30 2004-02-11 Micromass Ltd Mass spectrometer
US6800846B2 (en) 2002-05-30 2004-10-05 Micromass Uk Limited Mass spectrometer
EP2778669A1 (fr) * 2013-03-15 2014-09-17 Morpho Detection, LLC Spectromètre de mobilité à piège d'ions et son procédé d'utilisation
US9147565B1 (en) 2014-12-30 2015-09-29 Morpho Detection, Llc Ion mobility spectrometer and method of using the same
WO2023237958A1 (fr) * 2022-06-09 2023-12-14 Dh Technologies Development Pte. Ltd. Bobine d'arrêt rf destinée à être utilisée dans un spectromètre de masse et bobine d'arrêt rf

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7071467B2 (en) 2002-08-05 2006-07-04 Micromass Uk Limited Mass spectrometer
GB2394356B (en) * 2002-08-05 2005-02-16 Micromass Ltd Mass spectrometer

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2242311A (en) 1987-03-06 1991-09-25 Extrel Corp Mass spectrometry method
US5206506A (en) 1991-02-12 1993-04-27 Kirchner Nicholas J Ion processing: control and analysis
US5572035A (en) 1995-06-30 1996-11-05 Bruker-Franzen Analytik Gmbh Method and device for the reflection of charged particles on surfaces
US6107628A (en) 1998-06-03 2000-08-22 Battelle Memorial Institute Method and apparatus for directing ions and other charged particles generated at near atmospheric pressures into a region under vacuum

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AU6653296A (en) * 1995-08-11 1997-03-12 Mds Health Group Limited Spectrometer with axial field
DE19628179C2 (de) * 1996-07-12 1998-04-23 Bruker Franzen Analytik Gmbh Vorrichtung und Verfahren zum Einschuß von Ionen in eine Ionenfalle
GB2375653B (en) * 2001-02-22 2004-11-10 Bruker Daltonik Gmbh Travelling field for packaging ion beams
CA2391060C (fr) * 2001-06-21 2011-08-09 Micromass Limited Spectrometre de masse

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2242311A (en) 1987-03-06 1991-09-25 Extrel Corp Mass spectrometry method
US5206506A (en) 1991-02-12 1993-04-27 Kirchner Nicholas J Ion processing: control and analysis
US5572035A (en) 1995-06-30 1996-11-05 Bruker-Franzen Analytik Gmbh Method and device for the reflection of charged particles on surfaces
US6107628A (en) 1998-06-03 2000-08-22 Battelle Memorial Institute Method and apparatus for directing ions and other charged particles generated at near atmospheric pressures into a region under vacuum

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2391698A (en) * 2002-05-30 2004-02-11 Micromass Ltd Mass spectrometer
GB2391698B (en) * 2002-05-30 2004-07-21 Micromass Ltd Mass spectrometer
US6800846B2 (en) 2002-05-30 2004-10-05 Micromass Uk Limited Mass spectrometer
EP2778669A1 (fr) * 2013-03-15 2014-09-17 Morpho Detection, LLC Spectromètre de mobilité à piège d'ions et son procédé d'utilisation
US8866073B2 (en) 2013-03-15 2014-10-21 Morpho Detection, Llc Ion trap mobility spectrometer and method of using the same
US9147565B1 (en) 2014-12-30 2015-09-29 Morpho Detection, Llc Ion mobility spectrometer and method of using the same
WO2023237958A1 (fr) * 2022-06-09 2023-12-14 Dh Technologies Development Pte. Ltd. Bobine d'arrêt rf destinée à être utilisée dans un spectromètre de masse et bobine d'arrêt rf

Also Published As

Publication number Publication date
CA2391148C (fr) 2008-02-19
GB2381949C (en) 2006-02-06
GB2381949A (en) 2003-05-14
GB0214583D0 (en) 2002-08-07
CA2391148A1 (fr) 2002-12-25
GB2381949B (en) 2004-01-07
EP1271610A3 (fr) 2004-10-13
EP1271610B1 (fr) 2017-12-27

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