CN113725065A - Biochemical small molecule flight time mass spectrum system - Google Patents
Biochemical small molecule flight time mass spectrum system Download PDFInfo
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- CN113725065A CN113725065A CN202111080513.4A CN202111080513A CN113725065A CN 113725065 A CN113725065 A CN 113725065A CN 202111080513 A CN202111080513 A CN 202111080513A CN 113725065 A CN113725065 A CN 113725065A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
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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
- G01N27/64—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 using wave or particle radiation to ionise a gas, e.g. in an ionisation chamber
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/0027—Methods for using particle spectrometers
- H01J49/0036—Step by step routines describing the handling of the data generated during a measurement
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
- H01J49/025—Detectors specially adapted to particle spectrometers
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
- H01J49/04—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components
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- 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
- H01J49/067—Ion lenses, apertures, skimmers
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
- H01J49/24—Vacuum systems, e.g. maintaining desired pressures
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/26—Mass spectrometers or separator tubes
- H01J49/34—Dynamic spectrometers
- H01J49/40—Time-of-flight spectrometers
Abstract
The invention discloses a biochemical micromolecule flight time mass spectrum system, which comprises a sample introduction module, a vacuum module, an ion source, a flight time mass analyzer, a detector, a data acquisition card, a control panel and a power supply, wherein the sample introduction module is connected with the vacuum module; the sample introduction module comprises a sample target and a sample introduction cavity, and the sample target is arranged at the position of the sample introduction cavity; the vacuum module comprises three electromagnetic valves, a molecular pump and a backing pump; ion(s)The source comprises an XY stage, a vacuum lock, and an ion optics section comprising a laser system, a target electrode, a pulse electrode, and a grounded acceleration electrode; the flight time mass analyzer is a non-electric field flight tube; the detector is a microchannel plate detector; the data acquisition card adopts a high-performance accumulation data acquisition card. The vacuum system of the invention can lead the pressure in the vacuum area to reach 3 multiplied by 10‑4Pa below, and the sample and the matrix are effectively ionized under the irradiation of high-pulse laser light, the detection limit reaches 1fmol/ul, and the quality accuracy is as follows: the precision of the internal standard method is 150ppm, and the precision of the external standard method is 200 ppm.
Description
Technical Field
The invention relates to the technical field of small molecule mass spectra, in particular to a biochemical small molecule flight time mass spectrum system.
Background
A time-of-flight mass analyser is capable of mass analysing charged ions generated by an ion source at a flight speed. The flight time mass analyzer is a non-electric field flight tube, when an ion source ionizes a sample to become charged ions, the ions with different mass-to-charge ratios enter the flight tube at different speeds through an accelerating electric field, and the larger the mass-to-charge ratio, the smaller the speed. Ions with different flight speeds fly in the flight tubes with the same length, so the time of arriving at the detector is different, ions with small mass-to-charge ratio arrive first, and ions with large mass-to-charge ratio arrive later, thereby completing mass analysis. However, the sample target, the ion source and the flight tube are all in a vacuum environment to complete the ion flight process, and if the vacuum degree is not enough, the accuracy of the ion flight time is reduced. After the detector detects the ions, the ions are amplified and collected, and the collected signals are sent to analysis software for analysis. In the whole process, the measurement is required to be accurately and efficiently carried out, and if the error is large, the measurement accuracy is reduced.
Disclosure of Invention
The present invention is directed to solving, at least to some extent, one of the technical problems in the related art. Therefore, the invention aims to provide a biochemical small molecule flight time mass spectrum system, which solves the problems of low measurement accuracy caused by insufficient vacuum degree of a vacuum region in the mass spectrum system and large error of detection and acquisition information.
The invention provides a biochemical micromolecule flight time mass spectrum system which comprises a sample introduction module, a vacuum module, an ion source, a flight time mass analyzer, a detector, a data acquisition card, a control panel and a power supply, wherein the sample introduction module is connected with the vacuum module;
the sample introduction module comprises a sample target and a sample introduction cavity, the sample target is arranged at the position of the sample introduction cavity, and a target cabin door is arranged on the sample introduction cavity;
the vacuum module comprises three electromagnetic valves, a molecular pump and a backing pump, wherein a backing valve is arranged between the backing pump and the molecular pump, a deflation valve is arranged on the sample injection cavity, and a pre-pumping valve is arranged in a main cavity body where the ion source is positioned;
the ion source comprises an XY platform, a vacuum lock and an ion optical part, wherein the XY platform is used for moving a sample target to a corresponding position, the vacuum lock is used for isolating the atmosphere from a sample target vacuum region, the ion optical part comprises a laser system, a target electrode, a pulse electrode and a grounded accelerating electrode, and the sample target is placed on the target electrode;
the flight time mass analyzer is a non-electric field flight tube and is arranged between the ion source and the detector, and a same vacuum cavity is arranged between the flight time mass analyzer and the main cavity;
the detector is a microchannel plate detector and consists of two microchannel plates;
the data acquisition card adopts a high-performance accumulation data acquisition card, and the data acquisition card acquires and converts the electric signals output by the detector;
the control panel controls the mass spectrum system to work and is connected with the external control software processor, and the power supply supplies power to the mass spectrum system.
In some embodiments of the invention, the ion optics comprise a laser system, a target electrode to which the sample target can be attached, a pulse electrode and a grounded accelerating electrode, the laser head of the laser system facing the sample target, the pulse electrode and the grounded accelerating electrode being provided with channels for ions to pass through, the channels facing the electric field-free flight tube.
In other embodiments of the present invention, the laser system includes a pulsed laser generator, a laser energy conditioner, a laser focusing lens, and a laser spot conditioning device.
In other embodiments of the present invention, an ion lens is disposed in the flight tube, and focuses and flies the ions flying in the aircraft.
In other embodiments of the present invention, the data acquisition card employs a high performance cumulative data acquisition card, with 8-bit resolution, and a sampling rate up to 1GS/s per channel.
In other embodiments of the present invention, the detector generates electrons on the microchannel plate after receiving the impact of the high-speed kinetic energy of the sample ions, the electrons are accelerated and then impact the walls of the microchannel, thereby generating more secondary electrons, and the electron flow from the microchannel is amplified by the preamplifier.
In other embodiments of the present invention, the vacuum degree in the vacuum region of the sample target can reach 3 × 10-4Pa or less.
In other embodiments of the present invention, the voltage of the target electrode is 20 KV.
In the invention, the vacuum system can make the pressure in the vacuum area reach 3 multiplied by 10-4Pa below, under the irradiation of high pulse laser emitted by the sample and the matrix, the sample and the matrix are effectively ionized, the ion flight time can be accurately measured, the detection limit reaches 1fmol/ul, and the quality accuracy is as follows: the precision of the internal standard method is 150ppm, and the precision of the external standard method is 200 ppm.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:
fig. 1 is a schematic diagram of the internal structure of a mass spectrometry system according to the present invention.
FIG. 2 is a schematic diagram of a mass spectrometry system according to the present invention.
Fig. 3 is a schematic view of an ion source according to the present invention.
In the figure, 1, a sample injection cavity; 2. an ion source; 3. a flight tube; 4. a power source; 5. a high voltage pulse generator; 6. a laser; 7. a control panel; 8. a mechanical pump; 9. a molecular pump.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
The invention provides a biochemical micromolecule flight time mass spectrum system, which comprises a sample introduction module, a vacuum module, an ion source 2, a flight time mass analyzer, a detector, a data acquisition card, a control panel 7 and a power supply 4, wherein the sample introduction module is connected with the vacuum module;
the sample introduction module comprises a sample target and a sample introduction cavity, the sample target is arranged at the position of the sample introduction cavity, and a target cabin door is arranged on the sample introduction cavity;
the vacuum module comprises three electromagnetic valves, a molecular pump 9 and a backing pump, a backing valve is arranged between the backing pump and the molecular pump 9, a deflation valve is arranged on the sample injection cavity, and a pre-pumping valve is arranged in a main cavity where the ion source 2 is positioned;
the ion source 2 comprises an XY platform, a vacuum lock and an ion optical part, wherein the XY platform is used for moving a sample target to a corresponding position, the vacuum lock is used for isolating the atmosphere from a sample target vacuum region, the ion optical part comprises a laser system, a target electrode, a pulse electrode and a grounded accelerating electrode, and the sample target is placed on the target electrode;
the flight time mass analyzer is a non-electric field flight tube 3 and is arranged between the ion source 2 and the detector, and a same vacuum cavity is arranged between the flight time mass analyzer and the main cavity;
the detector is a microchannel plate detector and consists of two microchannel plates;
the data acquisition card adopts a high-performance accumulation data acquisition card, and the data acquisition card acquires and converts the electric signals output by the detector;
the control panel 7 controls the mass spectrum system to work and is connected with an external control software processor, and the power supply 4 supplies power to the mass spectrum system.
Coating the mixed point of the sample and the matrix on the target point of the sample target, closing the target cabin door, closing the front valve and the air release valve, opening the pre-pumping valve, and pumping the vacuum formed by the sample target and the cavity to be below 200Pa so as to enable the target to enter. At the moment, the pre-stage valve is opened, the pre-pumping valve is closed, the final vacuum pumping is carried out, the instrument returns to the vacuum state in normal work, and the vacuum in the cavity can be pumped to be below 3 multiplied by 10 < -4 > Pa under the normal condition.
The matrix on the sample target and the sample are converted into ions from molecules under the irradiation of high-frequency pulsed laser, so that ionization is realized. Meanwhile, a high voltage of 20kV (target electrode) is added on the sample target, a high-voltage electric field is formed in the ion source 2, sample ions accelerate flight under the action of an extraction electrode (pulse electrode), when the ions fly out of the ion source 2, the ions enter a field-free flight tube 3 (flight time mass analyzer) and finally reach a detector, the ions with different mass-to-charge ratios reach the detector at different times, the ions with small mass-to-charge ratios first reach the detector, the ions finally generate electric signals on the detector, and the mass spectrogram of the sample can be obtained on a computer after the ions are processed by a digital converter and the like.
The ion optical part comprises a laser system, a target electrode, a pulse electrode and a grounded accelerating electrode, the sample target can be attached to the target electrode, a laser head of the laser system faces the sample target, channels for ions to pass through are arranged on the pulse electrode and the grounded accelerating electrode, and the channels face the electric-field-free flight tube 3.
The high-speed kinetic energy of ions is utilized to impact on the microchannel plate to generate electrons, the electrons impact on the wall of the microchannel again after being accelerated, so that more secondary electrons are generated, the electron flow coming out of the microchannel passes through a preamplifier and is collected by a high-speed data acquisition card, and finally, the ion intensity is converted into digital voltage signals at different moments.
The voltage applied to the microchannel plate (MCP) detector provides an equipotential electric field, which provides kinetic energy by accelerating the impinging electrons a second time. Within a certain range, the higher the voltage value of the MCP, the stronger the signal strength, but too high a voltage may also compromise the lifetime of the MCP.
The laser system comprises a pulse laser generator, a laser energy regulator, a laser focusing lens and a laser spot regulating device. The laser emission frequency can reach 60HZ at most, and the laser is arranged in a laser panel of the software main interface.
Note that: the instrument contains a 3-stage class B laser 6 capable of emitting ultraviolet laser light at a wavelength of 337 nm. The instrument housing may protect a user from indirect radiation damage from invisible light. Opening the instrument housing panel during instrument operation exposes the operator to laser radiation, which can have serious consequences such as operator blindness. It is noted that the eye may not be directly opposite the laser. Before opening the side panel of the instrument, the goggles are worn each time and the other people are not exposed to the laser radiation. A reflective surface with a smooth surface (e.g., screwdriver, watch, ring, etc.) is not placed in the laser beam because the reflected visible or invisible light may be incident on the eye, causing unrecoverable damage.
And an ion lens is arranged in the flight tube 3 to focus and fly ions flying in the aircraft.
The data acquisition card adopts a high-performance accumulation data acquisition card, 8-bit resolution and sampling rate can reach 1GS/s per channel. The acquisition card acquires and converts the electric signals output by the MCP and transmits the electric signals to the computer to form digital signals, and the digital signals are used for subsequent calculation and analysis.
The vacuum degree of the sample target in the vacuum area can reach 3 multiplied by 10-4Pa or less.
Before using the instrument, the following guidelines were read in detail and followed:
1) before using the instrument, please read all the contents of this manual in detail;
2) when preparing samples and solutions, protective clothing, masks, gloves and the like are worn in order to minimize biological and chemical hazards;
3) the casing of the instrument can be wiped by dipping neutral detergent and aqueous solution with soft cloth, so that strong acid, strong alkali and other unsuitable solutions are not required to be used for cleaning;
4) because the instrument has larger mass and the performance parameters of the instrument can be influenced by the oscillation, a user is not advised to carry the instrument privately so as to avoid damaging the instrument;
5) a high-voltage (20KV) and ultraviolet pulse laser device (120 muJ, 337nm) are arranged in the instrument, so that a user cannot disassemble an instrument shell privately;
6) the instrument normally works in a high vacuum state, the instrument is kept stable in operation, and the environmental temperature and the environment temperature are moderate to meet the relevant requirements of the manual;
7) the air outlet at the back of the instrument is not blocked, so that the air vent is ensured to be smooth;
8) before the instrument is carried, please take out the sample target, otherwise the instrument may be damaged;
9) in the sampling and sampling process, the cabin door can automatically move, and the target plate is placed or taken out after the cabin door stops moving so as to avoid clamping fingers;
10) after the instrument is installed, debugged and operated without errors, the user is advised not to turn off the main power supply 4 of the instrument in normal use. After the instrument is used each time, the instrument naturally enters a standby state so as to be convenient for the next use. After the instrument is turned off, please wait for a period of time before turning off the power switch 4 because it has a high voltage. Similarly, when restarting the instrument, it takes a while before the instrument can be operated normally, and the user is asked to wait for the instrument. If the instrument is not idle for a long time, the main power supply 4 of the instrument is not required to be turned off, and only the high-voltage power supply 4 of the software is required to be turned off so as to be convenient to use.
Safety of electricity consumption of instrument
1) And (3) conventional safety: before installing the instrument, a user needs to confirm the safety of laboratory power supply setting and whether the voltage meets the instrument use specification, the user needs to know relevant laboratory safety management regulations and the safety management regulations of the instrument, and before installing and using the instrument, the user needs to listen to the suggestions and guidance of engineers in time.
2) The room in which the instrument is placed needs to be kept clean and dustless, and the instrument should avoid direct sunlight, vibration, corrosive gas, smoke, dust particles and the like as much as possible. The periphery of the instrument needs to be kept ventilated and dry, the instrument needs to be provided with a qualified protective grounding wire, the protective grounding wire must be connected to the real ground, and anyone cannot personally cut off the protective grounding wire.
3) The user should ensure that the power supply 4 line in the laboratory conforms to the relevant national safety standard and that the power resources can supply the instrument and the system with stable operation, and should configure the backup power supply 4 if necessary to prevent the instrument from being unnecessarily damaged by unexpected power failure.
4) The inside of the instrument has high voltage (20kV at most), and a user does not need to open the outer shell of the instrument by private, disassemble the instrument by private and try to maintain the instrument, otherwise, unnecessary personal injury can be caused. If the instrument fails, please contact the technical support of the company in time.
5) The connection of the instrument to the external circuit does not involve a) the accessible components of the external circuit becoming dangerously charged under normal conditions and single-fault conditions, or b) the accessible components of the device becoming dangerously charged under normal conditions and single-fault conditions.
6) The pollution grade of the product is 2 grades, and the overvoltage category is I.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (8)
1. A biochemical small molecule time-of-flight mass spectrometry system is characterized in that: the device comprises a sample introduction module, a vacuum module, an ion source, a time-of-flight mass analyzer, a detector, a data acquisition card, a control panel and a power supply;
the sample introduction module comprises a sample target and a sample introduction cavity, the sample target is arranged at the position of the sample introduction cavity, and a target cabin door is arranged on the sample introduction cavity;
the vacuum module comprises three electromagnetic valves, a molecular pump and a backing pump, wherein a backing valve is arranged between the backing pump and the molecular pump, a deflation valve is arranged on the sample injection cavity, and a pre-pumping valve is arranged in a main cavity body where the ion source is positioned;
the ion source comprises an XY platform, a vacuum lock and an ion optical part, wherein the XY platform is used for moving a sample target to a corresponding position, the vacuum lock is used for isolating the atmosphere from a sample target vacuum region, the ion optical part comprises a laser system, a target electrode, a pulse electrode and a grounded accelerating electrode, and the sample target is placed on the target electrode;
the flight time mass analyzer is a non-electric field flight tube and is arranged between the ion source and the detector, and a same vacuum cavity is arranged between the flight time mass analyzer and the main cavity;
the detector is a microchannel plate detector and consists of two microchannel plates;
the data acquisition card adopts a high-performance accumulation data acquisition card, and the data acquisition card acquires and converts the electric signals output by the detector;
the control panel controls the mass spectrum system to work and is connected with the external control software processor, and the power supply supplies power to the mass spectrum system.
2. The biochemical small molecule time-of-flight mass spectrometry system of claim 1, wherein: the ion optical part comprises a laser system, a target electrode, a pulse electrode and a grounded accelerating electrode, the sample target can be attached to the target electrode, a laser head of the laser system faces the sample target, channels for ions to pass through are arranged on the pulse electrode and the grounded accelerating electrode, and the channels face the electric field-free flight tube.
3. The biochemical small-molecule time-of-flight mass spectrometry system of claim 2, wherein: the laser system comprises a pulse laser generator, a laser energy regulator, a laser focusing lens and a laser spot regulating device.
4. The biochemical small molecule time-of-flight mass spectrometry system of claim 1, wherein: and an ion lens is arranged in the flight tube, and is used for focusing and flying ions flying in the aircraft.
5. The biochemical small molecule time-of-flight mass spectrometry system of claim 1, wherein: the data acquisition card adopts a high-performance accumulation data acquisition card, 8-bit resolution and sampling rate can reach 1GS/s per channel.
6. The biochemical small molecule time-of-flight mass spectrometry system of claim 1, wherein: the detector receives the impact of the high-speed kinetic energy of the sample ions, electrons are generated on the microchannel plate, the electrons are accelerated and then impact the wall of the microchannel, so that more secondary electrons are generated, and the electron flow from the microchannel is amplified by the preamplifier.
7. The biochemical small molecule time-of-flight mass spectrometry system of claim 1, wherein: the vacuum degree of the sample target in the vacuum area can reach 3 multiplied by 10-4Pa or less.
8. The biochemical small molecule time-of-flight mass spectrometry system of claim 1, wherein: the voltage of the target electrode is 20 KV.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202111080513.4A CN113725065A (en) | 2021-09-15 | 2021-09-15 | Biochemical small molecule flight time mass spectrum system |
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| CN202111080513.4A CN113725065A (en) | 2021-09-15 | 2021-09-15 | Biochemical small molecule flight time mass spectrum system |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116153761A (en) * | 2023-04-21 | 2023-05-23 | 浙江迪谱诊断技术有限公司 | Time-of-flight mass spectrometer |
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| CN104237175A (en) * | 2014-08-28 | 2014-12-24 | 中国科学院近代物理研究所 | Analyzer for synchronously measuring in-situ laser mass spectrum and light spectrum |
| CN204086141U (en) * | 2014-08-28 | 2015-01-07 | 中国科学院近代物理研究所 | Local laser mass spectrum spectroscopic simultaneous analyzer |
| CN109545647A (en) * | 2018-11-23 | 2019-03-29 | 暨南大学 | Mass spectrograph and mass spectrometric analysis method with mass spectrum sample rapid draing function |
| CN211238162U (en) * | 2020-03-12 | 2020-08-11 | 厦门汉可真空仪器有限公司 | Small-sized matrix-assisted laser analysis linear time-of-flight mass spectrometer |
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2021
- 2021-09-15 CN CN202111080513.4A patent/CN113725065A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104237175A (en) * | 2014-08-28 | 2014-12-24 | 中国科学院近代物理研究所 | Analyzer for synchronously measuring in-situ laser mass spectrum and light spectrum |
| CN204086141U (en) * | 2014-08-28 | 2015-01-07 | 中国科学院近代物理研究所 | Local laser mass spectrum spectroscopic simultaneous analyzer |
| CN109545647A (en) * | 2018-11-23 | 2019-03-29 | 暨南大学 | Mass spectrograph and mass spectrometric analysis method with mass spectrum sample rapid draing function |
| CN211238162U (en) * | 2020-03-12 | 2020-08-11 | 厦门汉可真空仪器有限公司 | Small-sized matrix-assisted laser analysis linear time-of-flight mass spectrometer |
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| CN116153761A (en) * | 2023-04-21 | 2023-05-23 | 浙江迪谱诊断技术有限公司 | Time-of-flight mass spectrometer |
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