Mass spectrometry systems and methods

Abstract

The present invention provides a mass spectrometry system and method, comprising an ion source and a vacuum device, wherein the ion source includes electrodes, and the vacuum device includes an injection port, a multi-stage vacuum chamber connected in series, and a pump; the vacuum device also includes a sealing cover having a movable member and an opening for allowing a pipe of the ion source to pass through, the movable member being used to close and open the opening, and the sealing cover being used to surround the injection port; a carrying device having a guide rail that allows the ion source to move; the ion source also includes a cavity and a cover, the cover having a pipe, the interior of the pipe communicating with the interior of the cavity, and the electrodes being disposed within the pipe; and the distance between the central axis of the pipe and the central axis of the injection port is less than R3+R2, where R3 is the inner diameter of the pipe. The present invention has the advantages of low energy consumption and low cost.

Description

Technical Field

[0001] The present invention relates to mass spectrometry analysis, and in particular to a mass spectrometry analysis system and method. Background Art

[0002] In the field of analytical instruments, mass spectrometers represent the pinnacle of sensitivity and selectivity. They not only have extremely low detection limits, but also have an excellent ability to distinguish molecules based on molecular weight and fragmentation patterns. They are the only mainstream analytical technology that can perform both qualitative and quantitative analysis and the only method that can determine molecular weight.

[0003] In complex analytical environments, especially those requiring rapid on-site screening, the mobility of portable field mass spectrometers makes them irreplaceable for real-time, in-situ rapid analysis and detection. Compared to mature large-scale laboratory mass spectrometers, field mass spectrometers have a much more complex development path. While miniaturized mass spectrometers of various types are readily available in laboratories, developing mass spectrometers suitable for complex field environments is extremely challenging.

[0004] There are two major difficulties in the research of mass spectrometers: the problem of maintaining the vacuum system and the problem of rapid on-site sampling.

[0005] Regarding the problem of maintaining the vacuum system, high vacuum can provide sufficient mean free path, collision-free ion orbits, reduce ion-molecule reactions, reduce background interference, extend filament life, eliminate discharges, and increase sensitivity. High vacuum is achieved through a two-stage vacuum pump. First, pre-vacuum is obtained by the front vacuum pump (usually a mechanical pump), and then continuous pumping by the high vacuum pump (diffusion pump or molecular turbo pump) is completed. There are currently two methods. One is continuous pumping at a high pumping speed. This method consumes a lot of energy, and the pump is very large, which is not suitable for on-site detection. The other is an adjustable speed vacuum pump, which reduces the speed when there is no sample and increases the speed when the sample is injected. Although this method reduces energy consumption to a certain extent and better maintains vacuum, it is not the best choice. It is not combined with the specific detection end to achieve the best, and there is no feedback, which also results in a huge waste of energy.

[0006] Regarding the problem of rapid on-site sampling, when testing samples on-site, both pre-treatment and sampling are very inconvenient, and the simpler the better. Currently, pre-treatment is usually completed before entering the ion source for ionization, which is a relatively cumbersome step.

[0007] Therefore, there is a lack of an on-site mass spectrometer and a working method thereof that can quickly inject samples and improve the vacuum degree. Summary of the Invention

[0008] In order to solve the deficiencies in the above-mentioned prior art solutions, the present invention provides a mass spectrometry analysis system.

[0009] The purpose of the present invention is achieved through the following technical solutions:

[0010] A mass spectrometry system, comprising an ion source and a vacuum device, wherein the ion source comprises an electrode, and the vacuum device comprises an inlet, a multi-stage vacuum chamber connected in series, and a pump; the vacuum device further comprises:

[0011] A sealing cover having a movable member and an opening for allowing the passage of the ion source pipe, the movable member being used to close and open the opening, and the sealing cover being used to surround the injection port; the distance between the central axis of the opening and the central axis of the injection port being less than R1+R2, where R1 is the radius of the opening and R2 is the radius of the injection port;

[0012] A carrying device, wherein the carrying device has a guide rail allowing the ion source to move;

[0013] The ion source also includes a cavity and a cover, the cover has a pipe, the interior of the pipe is connected to the interior of the cavity, and the electrode is arranged in the pipe; the distance between the central axis of the pipe and the central axis of the injection port is less than R3+R2, where R3 is the inner diameter of the pipe.

[0014] Another object of the present invention is to provide a mass spectrometry method according to the above mass spectrometry system, which is achieved by the following technical solutions:

[0015] A mass spectrometry analysis method, comprising the following steps:

[0016] (A1) The liquid to be tested is placed in the cavity of the ion source, and the cavity is sealed with a cover;

[0017] (A2) The ion source described in the above-mentioned embodiment moves on the carrier device and gradually approaches the sealing cover of the vacuum device, and the opening of the sealing cover is closed by the moving member;

[0018] (A3) the moving member opens the opening and, at the same time, increases the pumping speed of the vacuum device;

[0019] (A4) The ion source continues to move, and the ion source pipe passes through the opening and enters the sealed cover; the pipe is connected to the interior of the cavity, and the electrode is arranged in the pipe;

[0020] (A5) The ion source is moved to a determined position, the electrodes are discharged, the liquid to be tested is ionized, and the ions pass through the inlet of the vacuum device and enter the vacuum chamber;

[0021] The distance between the central axis of the pipeline and the central axis of the injection port is less than R3+R2, where R3 is the inner diameter of the pipeline.

[0022] Compared with the prior art, the present invention has the following beneficial effects:

[0023] 1. Low energy consumption;

[0024] A sealing cover is set at the injection port, which opens when injection is required and closes when injection is completed. The vacuum system is controlled according to the test results to achieve maximum vacuum maintenance and reduce energy consumption.

[0025] The trigger device is used to accurately trigger the pump's speed-increasing operation, further reducing energy consumption;

[0026] 2. Low cost;

[0027] The ion source has the function of liquid storage and processing. Pre-processing is performed using the ion source. For example, the cavity is set as a hollow cone, and the ionization device and the sample processing device are integrated into one design. This simplifies the pre-processing steps and saves time, avoids the common cross-contamination problem of ionization devices, saves disposable detection consumables, and reduces costs.

[0028] 3. Good working performance;

[0029] A sealing cover is set at the sample inlet, and the ionization and sample processing are integrated into one design, which is convenient for on-site operation and prevents interference from environmental factors such as wind and sand during on-site operation, thereby improving the detection signal-to-noise ratio and reliability. BRIEF DESCRIPTION OF THE DRAWINGS

[0030] The disclosure of the present invention will become more easily understood with reference to the accompanying drawings. Those skilled in the art will readily appreciate that these drawings are merely used to illustrate the technical solutions of the present invention and are not intended to limit the scope of protection of the present invention.

[0031] Figure 1 1 is a flow chart of the mass spectrometry analysis method according to Example 1 of the present invention. DETAILED DESCRIPTION

[0032] Figure 1 The following description describes alternative embodiments of the present invention to teach those skilled in the art how to implement and reproduce the present invention. In order to explain the technical solution of the present invention, some conventional aspects have been simplified or omitted. Those skilled in the art will understand that variations or substitutions derived from these embodiments will be within the scope of the present invention. Those skilled in the art will understand that the following features can be combined in various ways to form multiple variations of the present invention. Thus, the present invention is not limited to the following alternative embodiments, but is limited only by the claims and their equivalents.

[0033] Example 1:

[0034] The mass spectrometry analysis system of embodiment 1 of the present invention comprises:

[0035] A vacuum device, comprising a sample inlet, a multi-stage vacuum chamber connected in series, and a pump, wherein the operating speed of the pump is adjustable to achieve different pumping speeds;

[0036] A sealing cover having a movable member and an opening for allowing the passage of the ion source pipe, the movable member being used to close and open the opening, and the sealing cover being used to surround the injection port; the distance between the central axis of the opening and the central axis of the injection port being less than R1+R2, where R1 is the radius of the opening and R2 is the radius of the injection port;

[0037] A carrying device, wherein the carrying device has a guide rail allowing the ion source to move;

[0038] An ion source includes an electrode, a cavity and a cover, the cover having a pipe, the interior of the pipe being connected to the interior of the cavity, and the electrode being arranged in the pipe; the distance between the central axis of the pipe and the central axis of the injection port is less than R3+R2, where R3 is the inner diameter of the pipe.

[0039] In order to improve the efficiency of ions entering the vacuum device, further, the cavity is in the form of a hollow cone, and the central axis of the pipe is collinear with the central axis of the cavity.

[0040] In order to automatically open the opening and increase the pumping speed of the pump, the mass spectrometry analysis system further includes:

[0041] A trigger device, the trigger device is used to generate a trigger signal and transmit it to the control device; the trigger device includes a position sensor, and the position sensor is arranged on the carrier;

[0042] The control device is used to drive the moving part and increase the pumping speed of the pump, thereby improving the vacuum degree in the vacuum chamber.

[0043] In order to automatically achieve electrical connection, the carrying device further includes:

[0044] A limiting member, the limiting member is used to limit the movement of the ion source;

[0045] The conductor is used to contact the electrode when the ion source is blocked by the limiting member.

[0046] In order to accurately reflect the vacuum degree in the vacuum chamber in real time, the vacuum device further includes:

[0047] A plurality of sensors are arranged at corners of the vacuum chamber to obtain the vacuum degree of the vacuum chamber.

[0048] In order to prevent external interference with the liquid to be measured in the cavity, the ion source further includes:

[0049] The closure is used to close the opening of the pipeline.

[0050] Figure 1 A flow chart of a mass spectrometry analysis method according to an embodiment of the present invention is schematically provided. As shown in the figure, the mass spectrometry analysis method comprises the following steps:

[0051] (A1) The liquid to be tested is placed in the cavity of the ion source, and the cavity is sealed with a cover;

[0052] (A2) The ion source described in the above-mentioned embodiment moves on the carrier device and gradually approaches the sealing cover of the vacuum device, and the opening of the sealing cover is closed by the moving member;

[0053] (A3) the moving member opens the opening and, at the same time, increases the pumping speed of the vacuum device;

[0054] (A4) The ion source continues to move, and the ion source pipe passes through the opening and enters the sealed cover; the pipe is connected to the interior of the cavity, and the electrode is arranged in the pipe;

[0055] (A5) The ion source is moved to a determined position, the electrodes are discharged, the liquid to be tested is ionized, and the ions pass through the inlet of the vacuum device and enter the vacuum chamber;

[0056] The distance between the central axis of the pipeline and the central axis of the injection port is less than R3+R2, where R3 is the inner diameter of the pipeline.

[0057] In order to reduce the energy consumption of the pump, the mass spectrometry analysis method further includes the following steps:

[0058] (A6) After the mass spectrometry detection is completed, the pipeline of the ion source exits the sealing cover; at the same time, the moving part closes the opening and reduces the pumping speed of the pump.

[0059] In order to automatically open the opening and improve the vacuum degree in the vacuum chamber, further, in step (A3), when the position sensor detects the ion source, a trigger signal is issued;

[0060] The control device drives the moving part to open the opening according to the trigger signal.

[0061] In order to automatically achieve electrical connection, further, in step (A5), the ion source is blocked by a limiting member, and at the same time, the conductor is in contact with the electrode, and the conductor is connected to a power source.

[0062] Example 2:

[0063] An example of application of the mass spectrometry analysis system and method according to Example 1 of the present invention in hair detection.

[0064] In this application example, within the ion source, the cavity is a hollow cone, the cover is a disc, a pipe is arranged at the center of the cover and communicates with the interior of the cavity; an electrode is arranged in the pipe and passes through the interior of the cover; a sealing cover is fixed to the cover by a hinge, and a flexible sealing member is arranged on one side of the sealing cover. When the sealing cover rotates in the forward direction, the sealing member surrounds the open end of the pipe, and when the sealing cover rotates in the reverse direction, the sealing member opens the open end of the pipe; the ion source is arranged on a linear guide rail of a carrying device;

[0065] The vacuum device includes an injection port and multiple vacuum chambers connected in series. Sensors are installed at the four corners of each vacuum chamber to detect the vacuum degree of the vacuum chamber. A sealing cover surrounds the injection port, and a moving part is used to close and open the opening. The central axis of the injection port, the central axis of the opening, and the central axis of the pipeline are collinear.

[0066] The position sensor of the trigger device is used to detect whether the ion source on the guide rail has reached a certain position, and sends a trigger signal after reaching the certain position. The control device drives the moving part and increases the pumping speed of the pump according to the trigger signal;

[0067] The conductor is connected to a power source and fixed on the carrying device; the sealing cover is used as a limiter, and its side portion blocks further movement of the ion source.

[0068] The mass spectrometry analysis method of the embodiment of the present invention, that is, the working method of the mass spectrometry analysis system of this embodiment, comprises the following steps:

[0069] (A1) Hair processing: The hair sample is washed for the first time with a deionized water solution containing a surfactant, wherein the volume percentage of the surfactant is 0.5-5%, and the surfactant contains at least sodium dodecyl sulfate or sodium dodecylbenzene sulfonate. The hair sample that has been washed for the first time is washed for the second time with an organic solvent, wherein the organic solvent is one or more of the following organic reagents: acetone, methanol, ethanol, dichloromethane, acetonitrile or ethyl acetate. Furthermore, the cleaned hair sample is cut into small segments of 0.1-3 cm using clean scissors and placed in a grinding tube containing 1-10 grinding beads. The amount of hair used is 15-35 mg, the grinding beads used can be made of zirconium oxide or stainless steel, and the grinding tube used can be made of stainless steel or a polymer material of a certain strength. Furthermore, 0.1-1 mL of grinding liquid is added, and the sample is placed in a grinder and ground at a frequency of 20-100 Hz for 1-30 minutes; the grinding liquid is a mixture of one or more of the following solutions: water, methanol, ethanol, acetonitrile, acetone, propanol;

[0070] After centrifugation at a speed of 5000-15000 rpm for 1-10 minutes, the supernatant is aspirated into the cavity of the ion source, the cavity is sealed with a cover, the open end of the pipe is sealed with a sealing cover, and the sample is centrifuged again before being placed in a linear guide rail.

[0071] (A2) The ion source described in the above-mentioned embodiment moves on the carrier device and gradually approaches the sealing cover of the vacuum device, and the opening of the sealing cover is closed by the moving member;

[0072] (A3) when the position sensor detects the ion source, a trigger signal is issued;

[0073] The control device drives the moving member to open the opening and increase the pumping speed of the pump according to the trigger signal, thereby further increasing the vacuum degree in the vacuum chamber;

[0074] (A4) The ion source continues to move, and the ion source pipe passes through the opening and enters the sealed cover; the pipe is connected to the interior of the cavity, and the electrode is arranged in the pipe;

[0075] (A5) The ion source continues to move. When it is blocked by the sealing cover, it indicates that the ion source has moved to a certain position. At this time, the electrode contacts the conductor to achieve electrical connection; the distance between the open end of the pipe and the injection port is 1-5 mm;

[0076] The electrodes discharge, the liquid to be tested is ionized, and the ions pass through the inlet of the vacuum device and enter the vacuum chamber;

[0077] (A6) After the mass spectrometry is completed, the ion source retreats, and the conductor and the electrode separate;

[0078] When the signal of the position sensor changes suddenly, that is, the pipeline exits the sealing cover, the position sensor sends a trigger signal, and the control device controls the moving part to close the opening and, at the same time, reduces the pumping speed of the pump.

Claims

1. A mass spectrometry system, comprising an ion source and a vacuum device, wherein the ion source comprises an electrode, and the vacuum device comprises an inlet, a multi-stage vacuum chamber connected in series, and a pump; characterized in that: The vacuum device further comprises: A sealing cover having a movable member and an opening for allowing the passage of the ion source pipe, the movable member being used to close and open the opening, and the sealing cover being used to surround the injection port; the distance between the central axis of the opening and the central axis of the injection port being less than R1+R2, where R1 is the radius of the opening and R2 is the radius of the injection port; A carrying device, wherein the carrying device has a guide rail allowing the ion source to move; The ion source also includes a cavity and a cover, the cover has a pipe, the interior of the pipe is connected to the interior of the cavity, and the electrode is arranged in the pipe; the distance between the central axis of the pipe and the central axis of the injection port is less than R3+R2, where R3 is the inner diameter of the pipe.

2. The mass spectrometry system according to claim 1, wherein The cavity is in the shape of a hollow cone, and the central axis of the pipe is collinear with the central axis of the cavity.

3. The mass spectrometry system according to claim 1, wherein The mass spectrometry analysis system further comprises: A trigger device, the trigger device is used to generate a trigger signal and transmit it to the control device; the trigger device includes a position sensor, and the position sensor is arranged on the carrier; A control device is used to drive the moving part and increase the pumping speed of the pump.

4. The mass spectrometry system according to claim 1, wherein The carrying device further includes: A limiting member, the limiting member is used to limit the movement of the ion source; The conductor is used to contact the electrode when the ion source is blocked by the limiting member.

5. The mass spectrometry system according to claim 1, wherein The vacuum device further comprises: A plurality of sensors are arranged at corners of the vacuum chamber to obtain the vacuum degree of the vacuum chamber.

6. The mass spectrometry system according to claim 1, wherein: The ion source further comprises: The closure is used to close the opening of the pipeline.

7. A mass spectrometry analysis method based on the mass spectrometry analysis system according to any one of claims 1 to 6, the mass spectrometry analysis method comprising the following steps: (A1) The liquid to be tested is placed in the cavity of the ion source, and the cavity is sealed with a cover; The ion source (A2) moves on the carrier device and gradually approaches the sealing cover of the vacuum device, and the opening of the sealing cover is closed by the moving member; (A3) the moving member opens the opening and, at the same time, increases the pumping speed of the vacuum device; (A4) The ion source continues to move, and the ion source pipe passes through the opening and enters the sealing cover; the pipe is connected to the interior of the cavity, and the electrode is arranged in the pipe; (A5) The ion source is moved to a determined position, the electrodes are discharged, the liquid to be tested is ionized, and the ions pass through the inlet of the vacuum device and enter the vacuum chamber; The distance between the central axis of the pipeline and the central axis of the injection port is less than R3+R2, where R3 is the inner diameter of the pipeline.

8. The mass spectrometry analysis method according to claim 7, characterized in that The mass spectrometry analysis method further comprises the following steps: (A6) After the mass spectrometry detection is completed, the pipeline of the ion source exits the sealing cover; at the same time, the moving part closes the opening and reduces the pumping speed of the pump.

9. The mass spectrometry analysis method according to claim 7, characterized in that In step (A3), when the position sensor detects the ion source, a trigger signal is issued; The control device drives the moving part to open the opening according to the trigger signal.

10. The mass spectrometry analysis method according to claim 8, characterized in that In step (A5), the ion source is blocked by a limiting member, and at the same time, the conductor contacts the electrode, and the conductor is connected to a power source.

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