CN206116347U - Reduce cross interference's mass spectrum collision reaction tank - Google Patents
Reduce cross interference's mass spectrum collision reaction tank Download PDFInfo
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- CN206116347U CN206116347U CN201621061259.8U CN201621061259U CN206116347U CN 206116347 U CN206116347 U CN 206116347U CN 201621061259 U CN201621061259 U CN 201621061259U CN 206116347 U CN206116347 U CN 206116347U
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- ion
- reaction tank
- electrode slice
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Abstract
The utility model discloses a reduce cross interference's mass spectrum collision reaction tank. Particularly, the utility model discloses a neotype collision reaction tank, the accelerating electrode piece of major structure between by one set of hexapole pole and hexapole pole of collision reaction tank constitutes to it make pointed references from subscanner to utilize controls the monitoring ion. Have a same daughter ion when different parent ions, and the scanning of adjacent stage, voltage control system applys an optimum voltage by oneself on the electrode slice to the axial motion of daughter ion accelerates. The utility model discloses both guarantee multiple reaction monitoring's sensitivity, reduced crosstalk's emergence again.
Description
Technical field
This utility model belongs to chemical analysis instrument field, in particular it relates to a kind of MS/MS collision for reducing cross interference
Reaction tank.
Background technology
Triple quadrupole bar mass spectrum has various scan patterns, and wherein multiple-reaction monitoring pattern (MRM) is wherein to apply most
A kind of extensive pattern, it have sensitivity it is high, it is quantitative accurately the characteristics of.As a example by monitoring ion pair A-B, multiple-reaction monitoring mould
Formula requires that the RF amplitudes of the first pole level Four bar Q1 are fixed on certain certain value, and the definite value uniquely can ensure that mother with the ratio of the DC for applying
Ion A passes through level Four bar, and other ions exclude first order quadrupole rod due to unsteady motion, and parent ion A leaves
After first order quadrupole rod, into collision cell Q-cell, in the presence of collision gas and collision voltage, parent ion A is collided
Induced fragmentation, all fragment ions are transmitted to second level quadrupole rod Q3, the scan mode and Q1 of Q3 in the presence of rf electric field
Equally, only allow fragment ion B to leave quadrupole rod, reach detector.
The ion pair quantity that triple quadrupole bar (such as 1s) within the unit interval can be scanned is the key of MRM scan patterns
Performance indications, at present many commercialization mass spectrometers be claimed to reach 1s and scan to the ion pair of more than 500.In practical application
In, in the unit interval, the number of ions of scanning is more, while bringing two after the object species of detection also can be more, but scanning number is improved
Individual problem：(1) residence time of parent ion and daughter ion declines, parent ion in the collision cell fragmentation it is not abundant enough.(2) when
When two parent ions of appearance obtain an identical daughter ion scanning, the ion pair continuous detecting of such as A-B, C-B then occurs
The situation of cross interference, the daughter ion B that parent ion A is produced in upper ion pair A-B also do not leave collision cell completely, then can be by
Mass spectrum is recorded as the signal of next ion pair C-B, it is thus possible to cause false positive or detection signal to raise to testing result.
For this phenomenon, current mass spectrometer company employs the mode for increasing gradient DC electric field in collision cell,
Accelerate colliding in collision cell inner utilization using the quadrupole rod in irregular alignment by, for example, AB Sciex companies for daughter ion
Voltage manufactures gradient electric field, and all acceleration of ions in collision cell can be made to leave collision cell.But this accelerated mode to it is all from
Son is respectively provided with same effect, when ion pair quantity is a lot, it is also possible to the phenomenon of cross interference occurs.
In order to reduce the cross interference phenomenon of monitoring objective ion pair, it is auxiliary that this utility model devises a kind of new collision cell
Structure is helped, while coupled computer program arranges a kind of new control method, the identical daughter ion to the same time is capable of achieving
Ion pair accelerates to pass through, to other ions, it can be ensured that its abundant fragmentation, it is ensured that optimum detection sensitivity.
The content of the invention
First aspect of the present utility model provides a kind of MS/MS collision reaction tank, and the crash response pond is collided for n levels
Reaction tank, described n level crash responses pond are provided with the n pole bar being arranged in parallel, and wherein n is positive integer 4,6 or 8；And it is described
Crash response pond be additionally provided with for accelerating the acceleration electrode slice of mass ions.
In another preference, described mass ions are confusing mass ions.
In another preference, described mass ions are the mass ions of adjacent sweep phase.
In another preference, described arrival end and the crash response pond for accelerating electrode slice in the crash response pond
One produced between the port of export expels potential, and described expels potential for accelerating described mass ions to leave described mass spectrum
Crash response pond.
In another preference, when described mass ions are positive charge ion, described acceleration electrode slice is described
The arrival end in crash response pond produces high potential, and the low potential produced between the port of export in crash response pond, so as to be formed
Drive the mass ions acceleration MS/MS collision reaction tank expels potential.
In another preference, when described mass ions are negatively charged ions, described acceleration electrode slice is described
The arrival end in crash response pond produces low potential, and the high potential produced between the port of export in crash response pond, so as to be formed
Drive the mass ions acceleration MS/MS collision reaction tank expels potential.
In another preference, the arrival end by the crash response pond to exporting extreme direction, the acceleration electrode slice
Sectional area diminishes.
In another preference, described acceleration electrode slice is symmetrically arranged, so as to described acceleration electrode slice is to institute
The mass ions stated are produced or are substantially produced and expel power along MS/MS collision reaction tank axial direction.
In another preference, the quantity of described acceleration electrode slice is m, and wherein m is 2,3,4,6, or 8.
In another preference, m=n.
In another preference, m=n=6.
In another preference, the described electrode slice that accelerates is be arranged in parallel with n described pole bar.
In another preference, described electrode slice is located at pole bar between any two.
In another preference, the n pole bar length range is 50mm-500mm, it is preferred that being 100mm-150mm.
In another preference, the acceleration electrode slice length range is 50mm-500mm, it is preferred that being 100mm-
150mm。
In another preference, n described pole bar and the length ratio for accelerating electrode slice are 0.8-1.2；It is preferred that being
0.9-1.1。
In another preference, the acceleration electrode slice material is selected from the group：Rustless steel, alloy, molybdenum, copper or ferrum.
In another preference, the shape of the first type surface for accelerating electrode slice is selected from the group：It is trapezoidal, triangle, rectangular
Shape.
In another preference, the described DC voltage for accelerating to apply on electrode slice is -100V～+100V, it is preferred that
For -10V～+10V.
Second aspect of the present utility model provides a kind of mass spectrograph, and the mass spectrograph is furnished with or is provided with such as this utility model
First aspect described in crash response pond.
In another preference, the mass spectrograph is additionally provided with voltage control system, and the voltage control system is used to control
Put on the voltage Vjs for accelerating electrode slice.
In another preference, described control includes：Change the positive negative direction of the voltage Vjs, change the voltage
The positive negative direction of Vjs or its combination.
In another preference, described voltage control system is based on ion scan result, to putting on the acceleration electricity
The voltage Vjs of pole piece is controlled.
In another preference, described ion scan program can recognize the adjacent mother with same daughter ion from
Son.
In another preference, described ion scan program can apply an acceleration DC voltage automatically in acceleration electrode
Piece.
Second aspect of the present utility model provides a kind of analysis method for reducing MS/MS collision reaction cross interference, described
Analysis method include step：
I () provides a mass spectrograph, for detecting the first parent ion to be measured and the second parent ion, wherein the mass spectrograph
The MS/MS collision reaction tank being provided with as described in this utility model first aspect；
(ii) the first parent ion to be measured and the second parent ion are successively sent into into MS/MS collision reaction tank, is collided respectively
Reaction, so as to produce the first daughter ion collection from the first parent ion and the second daughter ion collection from the second parent ion；
Wherein, when the first described parent ion and the second described parent ion can produce one or more identical daughter ion
When, then carry out the first parent ion carry out crash response among or afterwards, to it is described acceleration electrode slice apply accelerating potential, so as to
Produce one and expel potential, it is described expel potential for accelerate from identical daughter ion (or the mass spectrum described in the first parent ion
Ion) leave described MS/MS collision reaction tank；And when from described in the first parent ion identical daughter ion (or mass spectrum from
Son) leave described MS/MS collision reaction tank after, will second parent ion feeding MS/MS collision reaction tank, so as to reduce mass spectrum
Crash response cross interference.
In another preference, methods described also includes step (iii)：Based on MS/MS collision reaction tank produce son from
Son, differentiates to first parent ion and the second parent ion.
In another preference, described putting on accelerates the accelerating potential of electrode slice to come from mass spectrograph storage inside
Device.
In another preference, described method includes step：To mass spectrograph internal storage one voltage of setting, and
When first parent ion and the second described parent ion can produce one or more identical daughter ion, the acceleration electrode slice is applied
Plus accelerating potential, potential is expelled so as to produce one.
In another preference, there is provided a kind of mass spectrometric analysis method, including step：
A () provides mass spectrograph of the present utility model；
B () arranges ion scan program；
Apply the rf electric field and assisted bias direct current DC of alternation in (c) pole bar
D () parent ion is cracked in the crash response pond as described in this utility model first aspect, so as to produce son from
Son；
(e) ion scan program performing flow process set in advance；With
F () daughter ion leaves crash response pond, reach detector, be analyzed detection.
In another preference, the ion scan program circuit in the step (b) also includes：
(e1) judge the scan type of user input for MRM patterns；
(e2) recognize that adjacent scanning fragment has the parent ion of identical daughter ion in arranging；
(e3), during the adjacent parent ion with identical daughter ion, a direct current accelerating potential is set on electrode slice is accelerated；
With
(e4) start scanning.
In another preference, described direct current accelerating potential is carried out according to the ion pair that user pre-sets by computer
Algorithm is calculated.
In another preference, described direct current accelerating potential changes with the daughter ion change of monitoring ion.
In another preference, described direct current accelerating potential scope is -10V～+10V.
It should be understood that in the range of this utility model, above-mentioned each technical characteristic of the present utility model and below (as implemented
Example) in can be combined with each other between each technical characteristic for specifically describing, so as to constitute new or preferred technical scheme.It is limited to
Length, here is no longer tired one by one to be stated.
Description of the drawings
The new collision cell structural representations of Fig. 1.
The new collision cell front views of Fig. 2.
The new collision cell rear views of Fig. 3.
Fig. 4 trapezoidal auxilliary electrode piece schematic diagrams.
Specific embodiment
The present inventor has invented a kind of analysis for reducing MS/MS collision reaction cross interference through extensively and in depth studying
Devices and methods therefor.The method is based on a kind of new crash response pond and matched voltage control system, main thought
It is the increase auxiliary electrode piece on six types of severe debility disease transmission pole collision cell, and is targetedly entered to monitoring ion using ion scan program
Row control.When different parent ions have identical daughter ion, and adjacent phases scanning, voltage control system is voluntarily applied on electrode slice
Plus an optimum voltage, so as to accelerate the axially-movable of daughter ion, reduce multiple-reaction monitoring crosstalk phenomenon and occur.Here basis
On, complete this utility model.
Term
As used herein, term " multiple reaction monitors (MRM) " technology is a kind of based on reactive ion that is known or assuming
Information, targetedly selects data to carry out mass signal collection, carries out signal record to legal ion, and removal is not inconsistent
The normally interference of ion signal, by the statistical analysiss to data so as to obtaining the mass-spectrometric technique of mass spectrum quantitative information.Specifically
Process is as follows：Parent ions of the first order quadrupole rod Q1 according to needed for the mass charge ratio range scanning and selection of setting；Collision cell Q2 (Q-
Cell), in the flight way of selected ion, neutral collision gas is introduced, Jing collision-induced makes parent ion produce fragment ion；
Second level quadrupole rod Q3 is used for the fragment ion that analysis is produced in collision cell.Q1 selects the parent ion of a certain quality, and collision is single
Unit produces fragment ion.Q3 is used for the daughter ion for searching parent ion generation, and feeds them into detector and be monitored, here it is many
Weight reaction monitoring (MRM).
As used herein, term " acceleration electrode slice " or " auxiliary electrode piece " are used interchangeably.
As used herein, term " mass ions " is including daughter ion and parent ion.
As used herein, term " crosstalk ", " interference " or " cross interference " is used interchangeably.Crosstalk refer to carry out it is multiple
During reaction detection, if adjacent sweep phase has two but there are identical m/z fragment ions from different parent ions, and scan
Time is very short, then when the daughter ion that a upper parent ion is produced also does not leave collision cell completely, will be registered as the next one
The signal of the daughter ion that parent ion is produced, causes the false positive or detection signal of testing result to raise.
As used herein, term " the first parent ion " and " the second parent ion ", refer in this utility model, when successively or first
After detect i, during i+n parent ion of i+1, i+2 ... ..., wherein i is positive integer, and n is >=1 positive integer, then for wantonly two phases
For adjacent parent ion, posterior parent ion is the second parent ion for the first parent ion for first parent ion, such as i parent ions
For the first parent ion, i+1 parent ions are the second parent ion；I+5 parent ions be the first parent ion, i+6 parent ions be the second mother from
Son.
As used herein, " the first described parent ion and the second described parent ion can produce one or more phase to term
Same daughter ion ", refers to that the first daughter ion collection from the first parent ion is concentrated with the second daughter ion from the second parent ion
One or more daughter ion is identical (occuring simultaneously not for sky).
Crash response pond
Crash response pool technology is also referred to as chemical identification.Chemical identification is that one kind passes through gaseous ion-molecular action, will
Ion carries out the process of collision induced dissociation.Crash response pond is just provided between ion lens and multi-pole mass analyzer
, for carrying out the device of this chemical identification process.A kind of neutral collision gas is introduced in the cell body of closing, in particle beam
Ion through with neutral molecule collide and induce dissociation after, by only plus radio frequency multistage bar transfer element ion beam is effective
Be transferred to mass analyzer and be measured.
If crash response pond described in the utility model is n level crash responses pond, described n level crash responses pond is provided with n
The pole bar being arranged in parallel, wherein n are positive integer 4,6 or 8；And described crash response pond is additionally provided with for accelerating mass ions
Acceleration electrode slice.In preferred implementation of the present utility model, n is positive integer 6.Crash response pond master of the present utility model
Body structure is made up of auxiliary electrode piece between a set of six types of severe debility disease bar and six types of severe debility disease bar.Apply the rf electric field and auxiliary of alternation on six types of severe debility disease bar
Bias direct current DC, rf electric field be used for fetter ion, prevent ion from suffering a loss in transmitting procedure, bias direct current DC give from
The kinetic energy of son motion, makes ion collide with buffering gas, and momentum transfer to ionic bond makes ion that cracking to occur, and this process is referred to as
Collision induced dissociation.
Additionally, for the collision pool structure of non-directional bending, multi-pole can also be in warp architecture with acceleration electrode slice.
Reduce the analysis method that MS/MS collision reacts cross interference
In this utility model, when i is detected successively or successively, during i+n parent ion of i+1, i+2 ... ..., wherein i is for just
Integer, n is >=1 positive integer, then for wantonly two adjacent parent ions, first parent ion for the first parent ion
Parent ion afterwards is the second parent ion, and such as i parent ions are the first parent ion, and i+1 parent ions are the second parent ion；I+5 it is female from
Son is the first parent ion, and i+6 parent ions are the second parent ion.
When the first and second parent ions produce identical daughter ion, analysis method of the present utility model can accelerate first female
The daughter ion of ion leaves, and reduces MS/MS collision reaction cross interference phenomenon.
Concrete mechanism is as follows：First parent ion to be measured and the second parent ion are successively sent into into MS/MS collision reaction tank, point
Crash response is not carried out, so as to produce the first daughter ion collection from the first parent ion and second sub from the second parent ion
Ion collection；Wherein, when the first described parent ion and the second described parent ion can produce one or more identical daughter ion
When, then carry out the first parent ion carry out crash response among or afterwards, to it is described acceleration electrode slice apply accelerating potential, so as to
Produce one and expel potential, it is described expel potential for accelerate from identical daughter ion (or the mass spectrum described in the first parent ion
Ion) leave described MS/MS collision reaction tank；And when from described in the first parent ion identical daughter ion (or mass spectrum from
Son) leave described MS/MS collision reaction tank after, will second parent ion feeding MS/MS collision reaction tank, so as to reduce mass spectrum
Crash response cross interference.
Ion scan program
This utility model is provided with a set of ion scan program, for being targetedly controlled to monitoring ion, reduces
Multiple-reaction monitoring crosstalk phenomenon occurs.The ion scan program can according in same section sweep time monitor ion son from
Son is judged, if different parent ions have identical daughter ion, and adjacent phases scanning, then software is being scanned to these sections
When, automatically apply one and accelerate DC voltage to auxiliary electrode piece, the voltage according to scan type be cation scanning or bear from
Son scanning, setting voltage range is between (such as -5V～+5V).
One preferred program execution flow is as follows：
Voltage control system
Voltage control system of the present utility model includes above-mentioned ion scan program.Voltage control system identification it is adjacent from
Sub- centering is it may happen that the ion pair of crosstalk, the mass ions pre-set according to user by computer program, calculate which
Without the optimal applied voltage that crosstalk occurs, put on accessory.The voltage changes with monitoring objective ion pair and changes.
Major advantage of the present utility model includes：
1st, new crash response pond can accelerate passing through for ion.
2nd, by software according to ion pair type is monitored, targetedly the ion pair to being susceptible to crosstalk phenomenon carries out adding
Other ion pairs are reduced and are accelerated by speed, while ensure that detection sensitivity and reduce crosstalk phenomenon occur.
With reference to specific embodiment, this utility model is expanded on further.It should be understood that these embodiments are merely to illustrate this
Utility model rather than restriction scope of the present utility model.The experimental technique of unreceipted actual conditions in the following example, leads to
Often according to normal condition, or according to the condition proposed by manufacturer.
Embodiment 1
MS/MS collision reaction tank No.1 and mass spectrograph No.1
The MS/MS collision reaction pool structure of the present embodiment is as shown in figure 1, wherein described crash response pond is 6 grades of crash responses
Pond, 6 grades of described crash response ponds are provided with 6 level bars being arranged in parallel；And described crash response pond is additionally provided with for adding
6 acceleration electrode slices of fast mass ions, arrange an acceleration electrode slice between the adjacent pole bar of two of which.Accelerate electrode slice be
Trapezoidal sheet metal, when DC voltage puts on acceleration electrode slice, accelerates electrode slice to be internally formed one in crash response pond
The electric potential field of graded, can accelerate the axially-movable of ion.Fig. 2 and Fig. 3 is that new collision cell front view and the back side regard
Figure, as illustrated, trapezoidal electrode slice is axially uniformly present in two-by-two between six grades of bars, along the crash response pond arrival end extremely
Outlet extreme direction, it is different to accelerate electrode slice that there is identical cross-sectional area, and cross-sectional area uniformly diminishes.Fig. 4 is trapezoidal
Auxiliary electrode piece schematic diagram.
Wherein, pole bar size is 120mm, accelerates electrode chip size to be 120mm.
Mass spectrometric other structures are essentially identical with conventional mass spectrometer, but are additionally provided with for controlling 6 acceleration
The voltage control system of electrode slice.When the adjacent ion pair with identical daughter ion is cation, setting accelerating potential is 3V.
Comparative example 1
MS/MS collision reaction tank No.C1 and mass spectrograph No.C1
With embodiment 1, difference only exists the structure of the MS/MS collision reaction tank No.C1 and mass spectrograph No.C1 of this comparative example
Accelerate electrode slices in eliminating 6, and for controlling the voltage control systems of 6 acceleration electrode slice.
Test case
With embodiment 1 and the mass spectrograph of comparative example 1, Mass Spectrometer Method is carried out.Parent ion to be detected is aminoacid.Various
In amino acid analysises, adjacent detectable substance proline and ornithine successively enter mass spectrum, and interval time is very of short duration, their detection
Ion pair is respectively：Proline m/z172.1->70 and ornithine m/z189.1->70, using the technology of embodiment 1, proline
Daughter ion 70 accelerate to leave collision cell, the testing result of the ornithine entered after not resulting in is in that false positive or signal increase
Plus, and adopt the technology of comparative example, then the testing result of ornithine is likely to result in false positive or signal increases.
The all documents referred in this utility model are all incorporated as reference in this application, just as each document quilt
It is individually recited such as reference.In addition, it is to be understood that after above-mentioned teachings of the present utility model have been read, this area skill
Art personnel can be made various changes or modifications to this utility model, and these equivalent form of values equally fall within the application claims
Book limited range.
Claims (5)
1. a kind of MS/MS collision reaction tank, it is characterised in that the crash response pond is n level crash responses pond, described n levels are touched
Hit reaction tank and be provided with the n pole bar being arranged in parallel, wherein n is positive integer 4,6 or 8；
And described crash response pond is additionally provided with for accelerating the acceleration electrode slice of mass ions.
2. crash response pond as claimed in claim 1, it is characterised in that by the arrival end in the crash response pond to the port of export
Direction, the sectional area of the acceleration electrode slice diminish.
3. crash response pond as claimed in claim 1, it is characterised in that described acceleration electrode slice be it is symmetrically arranged, from
And described acceleration electrode slice is produced to described mass ions or substantially produces expelling along MS/MS collision reaction tank axial direction
Power.
4. a kind of mass spectrograph, it is characterised in that the mass spectrograph is furnished with or is provided with crash response as described in claim 1
Pond.
5. mass spectrograph as described in claim 4, it is characterised in that the mass spectrograph is additionally provided with voltage control system, described
Voltage control system puts on the voltage Vjs for accelerating electrode slice for control.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201621061259.8U CN206116347U (en) | 2016-09-18 | 2016-09-18 | Reduce cross interference's mass spectrum collision reaction tank |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201621061259.8U CN206116347U (en) | 2016-09-18 | 2016-09-18 | Reduce cross interference's mass spectrum collision reaction tank |
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| Publication Number | Publication Date |
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| CN206116347U true CN206116347U (en) | 2017-04-19 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107845561A (en) * | 2016-09-18 | 2018-03-27 | 江苏可力色质医疗器械有限公司 | A kind of MS/MS collision reaction tank and analysis method for reducing cross jamming |
-
2016
- 2016-09-18 CN CN201621061259.8U patent/CN206116347U/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107845561A (en) * | 2016-09-18 | 2018-03-27 | 江苏可力色质医疗器械有限公司 | A kind of MS/MS collision reaction tank and analysis method for reducing cross jamming |
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