CN112362718A - Method and device for widening mass spectrometer detection quality range - Google Patents
Method and device for widening mass spectrometer detection quality range Download PDFInfo
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- 238000001514 detection method Methods 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 30
- 230000003247 decreasing effect Effects 0.000 claims description 3
- 238000004458 analytical method Methods 0.000 abstract description 17
- 230000003321 amplification Effects 0.000 abstract description 3
- 238000003199 nucleic acid amplification method Methods 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 150000002500 ions Chemical class 0.000 description 15
- 238000000105 evaporative light scattering detection Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 238000004949 mass spectrometry Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000005040 ion trap Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920001184 polypeptide Polymers 0.000 description 1
- 102000004196 processed proteins & peptides Human genes 0.000 description 1
- 108090000765 processed proteins & peptides Proteins 0.000 description 1
- 238000004451 qualitative analysis Methods 0.000 description 1
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- 239000012855 volatile organic compound Substances 0.000 description 1
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- H01J49/26—Mass spectrometers or separator tubes
Abstract
The application relates to a method and a device for widening mass spectrometer detection mass range, which comprises the following steps: s1, adjusting the frequency and amplitude of the radio frequency signal to preset values; s2, keeping the frequency of the radio frequency signal unchanged, and adjusting the amplitude of the radio frequency signal to enable the amplitude of the radio frequency signal to scan along a specific direction; s3, when the amplitude of the radio frequency signal is adjusted to the limit value, keeping the amplitude of the radio frequency signal unchanged, and adjusting the frequency of the radio frequency signal so as to enable the frequency of the radio frequency signal to scan along a specific direction; and S4, stopping scanning when the frequency of the radio frequency signal is adjusted to the limit value, and outputting the detection result of the quality range. The invention has the beneficial effects that: the radio frequency amplitude scanning and the radio frequency scanning are performed in a segmented mode in one period, and the quality analysis range can be amplified to a certain degree under the same radio frequency amplification system.
Description
Technical Field
The application belongs to the technical field of mass spectrometry, and particularly relates to a method for widening a mass spectrometer detection mass range.
Background
The mass spectrometry technology can analyze the mass-to-charge ratio information of a substance to be detected, has high specificity and extremely fast analysis speed compared with other analysis means, and can finish qualitative and quantitative analysis of the substance in extreme time, thereby becoming an important analysis means in the fields of chemistry, biology, clinical medicine and the like. The need for high precision, high accuracy analysis in some fields has also driven the miniaturization of mass spectrometers, and researchers have developed numerous miniaturized mass spectrometers that employ different mass analyzers.
However, the miniaturization of the mass spectrometer also sacrifices certain instrument performance, and the requirement of being able to cope with variable environments also limits the power consumption of the miniaturized mass spectrometer, further limiting the amplitude and frequency range of the high voltage on the mass analyzer. The currently developed miniaturized mass spectrometer, especially a miniaturized mass spectrometer using an ion trap as a mass analyzer, focuses on the analysis and detection of a substance with a small mass-to-charge ratio range, for example, is suitable for the analysis of volatile organic compounds in the range of 0-300 Da, or suitable for the analysis of small molecular substances such as chemical substances or biological polypeptides in the range of 300-700 Da.
To widen the application range of the miniaturized mass spectrometer and improve the application universality, the mass analysis range of the mass analyzer needs to be widened within the power consumption and volume range required by portability.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: in order to widen the mass analysis range of a miniaturized mass spectrometer, the invention provides a method and a device for widening the mass detection range of a mass spectrometer.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a method of broadening the detection mass range of a mass spectrometer comprising the steps of:
s1, adjusting the frequency and amplitude of the radio frequency signal to preset values;
s2, keeping the frequency of the radio frequency signal unchanged, and adjusting the amplitude of the radio frequency signal to enable the amplitude of the radio frequency signal to scan along a specific direction;
s3, when the amplitude of the radio frequency signal is adjusted to the limit value, keeping the amplitude of the radio frequency signal unchanged, and adjusting the frequency of the radio frequency signal so as to enable the frequency of the radio frequency signal to scan along a specific direction;
and S4, stopping scanning when the frequency of the radio frequency signal is adjusted to the limit value, and outputting the detection result of the quality range.
Preferably, in the method for widening the mass spectrometer detection mass range, the preset value of the radio frequency signal frequency is the maximum value.
Preferably, in the method for widening the mass spectrometer detection mass range, the preset value of the radio frequency signal amplitude is the minimum value.
Preferably, in step S2, the amplitude of the rf signal is increased from the minimum value to the maximum value in a linear manner.
Preferably, in step S3, the frequency of the rf signal is gradually decreased from the maximum value to the minimum value in a linear change manner.
Preferably, the limit value of the method for widening the mass spectrometer detection mass range is the maximum value or the minimum value of the frequency or the amplitude of the radio frequency signal which can be output by the mass spectrometer.
An apparatus for broadening the detection mass range of a mass spectrometer, comprising:
the numerical value setting module is used for adjusting the frequency and the amplitude of the radio frequency signal to preset values;
the radio frequency signal adjusting module is used for keeping the frequency of the radio frequency signal unchanged and adjusting the amplitude of the radio frequency signal so as to enable the amplitude of the radio frequency signal to scan along a specific direction; or after the amplitude of the radio frequency signal is adjusted to the limit value, keeping the amplitude of the radio frequency signal unchanged, and adjusting the frequency of the radio frequency signal so as to enable the frequency of the radio frequency signal to scan along a specific direction;
and the result output module is used for stopping scanning and outputting the quality range detection result when the frequency of the radio frequency signal is adjusted to the limit value.
The invention has the beneficial effects that: the radio frequency amplitude scanning and the radio frequency scanning are performed in a segmented mode in one period, and the analysis range can be amplified to a certain extent under the same radio frequency amplification system.
Drawings
The technical solution of the present application is further explained below with reference to the drawings and the embodiments.
FIG. 1 is a flow chart of the method steps for broadening the mass spectrometer detection mass range of example 1 of the present application;
FIG. 2 is a graph showing the relationship between the amplitude and frequency of the RF signal in the mass spectrometer of example 1 of the present application;
FIG. 3 is a graph showing the relationship between the amplitude and frequency of the RF signal in the mass spectrometer of example 2 of the present application;
fig. 4 is a graph of the correspondence between the amplitude and the frequency of the rf signal when the mass spectrometer of example 3 of the present application detects a mass range.
Detailed Description
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict.
In the description of the present application, it is to be understood that the terms "center," "longitudinal," "lateral," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," and the like are used in the orientation or positional relationship indicated in the drawings for convenience in describing the present application and for simplicity in description, and are not intended to indicate or imply that the referenced devices or elements must have a particular orientation, be constructed in a particular orientation, and be operated in a particular manner, and are not to be considered limiting of the scope of the present application. Furthermore, the terms "first", "second", etc. are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first," "second," etc. may explicitly or implicitly include one or more of that feature. In the description of the invention, the meaning of "a plurality" is two or more unless otherwise specified.
In the description of the present application, it is to be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meaning of the above terms in the present application can be understood by those of ordinary skill in the art through specific situations.
The technical solutions of the present application will be described in detail below with reference to the accompanying drawings in conjunction with embodiments.
Example 1
In order to widen the mass analysis range of a miniaturized mass spectrometer, the invention provides a dual-mode combined radio frequency scanning method, which can widen the mass analysis range of a corresponding mass analyzer and improve the application universality of the corresponding miniaturized mass spectrometer under the condition of not changing the power consumption of the instrument, so that the detection of analytes in a wide mass range can be simultaneously met.
Taking a quadrupole mass analyzer as an example, two groups of electrodes of a quadrupole are respectively applied with a direct current voltage U with equal value and opposite polarity and a radio frequency signal amplitude V, the frequency of the radio frequency signal is omega, and a hyperbolic electric field is generated in a space surrounded by the radio frequency signal amplitude V. The motion trail of the ions in the quadrupole rod satisfies the Marseh equation
The parameter of DC intensity can be represented by a, and the intensity of RF AC parameter can be represented by q, wherein
r0As an electrode meterAnd (3) solving the Marseh equation according to the distance between the surface and the center of the quadrupole rod to obtain a stability diagram (a, q) of the ion motion in the quadrupole rod. The first stable region is selected to carry out ion operation, the peak of the stable region is taken as an operation point, the quadrupole mass filtering function is realized by changing the parameters of radio frequency voltage under the condition of fixed direct current voltage, ions meeting the conditions enter a detector through a quadrupole rod, and non-target ions are annihilated in the quadrupole rod.
The embodiment provides a method for widening the mass detection range of a mass spectrometer, which comprises the following steps:
s1, adjusting the frequency and amplitude of the radio frequency signal to preset values;
s2, keeping the frequency of the rf signal unchanged, and adjusting the amplitude of the rf signal so that the amplitude of the rf signal scans along a specific direction (i.e. the amplitude of the rf signal changes from large to small or from small to large);
s3, when the rf signal amplitude is adjusted to the limit value, keeping the rf signal amplitude unchanged, and adjusting the rf signal frequency to scan the rf signal frequency along a specific direction (i.e. the change of the rf signal frequency is from large to small or from small to small);
and S4, stopping scanning when the frequency of the radio frequency signal is adjusted to the limit value, and outputting the detection result of the quality range.
Preferably, in the method for widening the mass spectrometer detection mass range of the embodiment, the preset value of the radio frequency signal frequency is a maximum value.
Preferably, in the method for widening the mass spectrometer detection mass range, the preset value of the radio frequency signal amplitude is the minimum value.
Preferably, in the method for widening the mass spectrometer detection mass range of the present embodiment, in step S2, the amplitude of the radio frequency signal is increased from the minimum value to the maximum value in a linear change manner.
Preferably, in the method for widening the mass spectrometer detection mass range of the present embodiment, in step S3, the frequency of the radio frequency signal is gradually decreased from the maximum value to the minimum value in a linear change manner.
Preferably, in the method for widening the mass spectrometer detection mass range, the limit value is the maximum value or the minimum value of the frequency of the radio frequency signal or the amplitude of the radio frequency signal which can be output by the mass spectrometer.
The embodiment provides an apparatus for widening mass spectrometer detection quality range, which comprises:
the numerical value setting module is used for adjusting the frequency and the amplitude of the radio frequency signal to preset values;
the radio frequency signal adjusting module is used for keeping the frequency of the radio frequency signal unchanged and adjusting the amplitude of the radio frequency signal so as to enable the amplitude of the radio frequency signal to scan along a specific direction; or after the amplitude of the radio frequency signal is adjusted to the limit value, keeping the amplitude of the radio frequency signal unchanged, and adjusting the frequency of the radio frequency signal so as to enable the frequency of the radio frequency signal to scan along a specific direction;
and the result output module is used for stopping scanning and outputting the quality range detection result when the frequency of the radio frequency signal is adjusted to the limit value.
Specifically, in this example, a quadrupole mass analyzer is taken as an example, the quadrupole length L is set, and the distance between the electrode surface and the center of the quadrupole is r0As shown in FIG. 2, the RF circuit can be boosted to 100-500V, frequency varied to 200-1000 kHz, and total time of single scan is t2. One scanning period is divided into two stages, 0-t1In the time period, the frequency of the radio frequency signal is kept unchanged at 1000kHz, the amplitude of the radio frequency signal is linearly scanned from 100V to 500V, and the voltage is t1The moment reaches 500V, t1～t2The amplitude of the radio frequency signal is kept 500V in the time period, and the frequency of the radio frequency signal is swept and reduced from 1000kHz to 200 kHz. And the ions in the whole scanning period sequentially pass through the quadrupole rods according to the sequence of the mass-to-charge ratio from small to large to reach the detector, so that the analysis process is completed. In principle, the DC signal U applied to the quadrupole rod electrode is kept the same in the operation process, and the ions are selected under the same q point condition. In a scanning period, firstly fixing the same frequency omega of the radio frequency signal, scanning the amplitude V of the radio frequency signal from low to high, and because the q point is operated and the frequency of the radio frequency signal is fixed, ions in the quadrupole can be in accordance with the mass-to-charge ratioThe four-pole rods are sequentially passed through from low to high and are captured by a detector. When the radio frequency voltage is scanned to the highest value V output by the radio frequency circuitmaxThe operation mode is changed to ensure that the voltage of the radio frequency signal keeps the maximum value VmaxGradually changing the frequency omega of the radio frequency signal to make the frequency of the radio frequency signal scan from high to low, at the moment, due to the q point and the radio frequency voltage VmaxAnd fixing, wherein ions meeting the conditions in the quadrupole rod sequentially pass through the quadrupole rod from low to high according to the mass-to-charge ratio along with the continuous reduction of the frequency omega of the radio frequency signal and are captured by a detector. Compared with radio frequency amplitude scanning or radio frequency scanning, the scanning mode increases the coverage range of the ion mass-to-charge ratio under the same radio frequency condition.
Example 2
The embodiment provides a method for widening the mass detection range of a mass spectrometer, which comprises the following steps:
s1, adjusting the frequency and the amplitude of the radio frequency signal to a first preset value;
s2, keeping the frequency of the radio frequency signal unchanged, and adjusting the amplitude of the radio frequency signal to enable the amplitude of the radio frequency signal to scan along a specific direction;
s3, when the amplitude of the radio frequency signal is adjusted to a second preset value, keeping the amplitude of the radio frequency signal unchanged, and adjusting the frequency of the radio frequency signal so as to enable the frequency of the radio frequency signal to scan along a specific direction;
s4, readjusting the frequency of the radio frequency signal to a first preset value, and adjusting the amplitude of the radio frequency signal to a limit value from a second preset value; and stopping scanning and outputting the detection result of the quality range.
Taking a quadrupole mass analyzer as an example, the quadrupole length L is set, and the distance between the electrode surface and the center of the quadrupole is r0As shown in FIG. 3, the RF circuit can boost the RF signal to 100-500V, but the second preset value of the RF signal amplitude is an intermediate value in the boost range, such as 300V, the frequency variation range is 200-1000 kHz, and the total time of a single scan is t3. In this case, the scanning period can be divided into three stages, 0 to t1In the time period, the frequency of the radio frequency signal is kept unchanged at 1000kHz, and the amplitude of the radio frequency signal is kept unchangedLinear sweep from 100V to 300V, with RF signal amplitude (voltage) at t1The moment reaches 300V, t1～t2The amplitude of the radio frequency signal is kept at 300V in a time period, and the frequency of the radio frequency signal is swept from 1000kHz to 200kHz, t2～t3The frequency of the radio frequency signal is kept unchanged at 1000kHz in the time period, and the amplitude of the radio frequency signal is linearly scanned from 300V to 500V. And the ions in the whole scanning period sequentially pass through the quadrupole rods according to the sequence of the mass-to-charge ratio from small to large to reach the detector, so that the analysis process is completed. Compared with radio frequency amplitude scanning or radio frequency scanning, the scanning mode increases the coverage range of the ion mass-to-charge ratio under the same radio frequency condition. .
Example 3
The embodiment provides a method for widening the mass detection range of a mass spectrometer, which comprises the following steps:
s1, adjusting the frequency and the amplitude of the radio frequency signal to a first preset value;
s2, keeping the frequency of the radio frequency signal unchanged, and adjusting the amplitude of the radio frequency signal to enable the amplitude of the radio frequency signal to scan along a specific direction;
s3, when the amplitude of the rf signal is adjusted to a second preset value, keeping the amplitude of the rf signal unchanged, and adjusting the frequency of the rf signal to a second preset value (the second preset value is different from the second preset value of the amplitude of the rf signal), so that the frequency of the rf signal scans along a specific direction;
and S4, stopping scanning when the frequency of the radio frequency signal is adjusted to the limit value, and outputting the detection result of the quality range.
In this embodiment, the first preset values of the frequency and the amplitude of the rf signal are not at the adjusted end points.
The present embodiment provides a method for widening the mass detection range of a mass spectrometer, and specifically, in this embodiment, taking a quadrupole mass analyzer as an example, a quadrupole length L is set, and a distance between the electrode surface and the center of the quadrupole is r0As shown in FIG. 4, the RF circuit can be boosted to 100-500V, frequency varied to 200-1000 kHz, and total time of single scan is t2. One scanning period is divided into two stages, 0-t1In the time period, the frequency of the radio frequency signal is kept unchanged at 800kHz, the amplitude of the radio frequency signal is linearly scanned from 100V to 500V, and the voltage is t1The moment reaches 500V, t1～t2The amplitude of the radio frequency signal is kept at 300V in the time period, and the frequency of the radio frequency signal is swept and reduced from 1000kHz to 200 kHz. And the ions in the whole scanning period sequentially pass through the quadrupole rods according to the sequence of the mass-to-charge ratio from small to large to reach the detector, so that the analysis process is completed. Compared with radio frequency amplitude scanning or radio frequency scanning, the scanning mode increases the coverage range of the ion mass-to-charge ratio under the same radio frequency condition.
It can be seen that the mass spectrometer mass range detection method in embodiments 1, 2, and 3 is different from the conventional single rf frequency scanning or rf amplitude scanning, combines two rf scanning modes, and performs rf amplitude scanning and rf frequency scanning in a period in segments by using the relationship between the rf signal amplitude and frequency and the ion mass-to-charge ratio, and can expand the analysis range to a certain extent under the same rf amplification system.
In light of the foregoing description of the preferred embodiments according to the present application, it is to be understood that various changes and modifications may be made without departing from the spirit and scope of the invention. The technical scope of the present application is not limited to the contents of the specification, and must be determined according to the scope of the claims.
Claims (7)
1. A method of broadening the detection mass range of a mass spectrometer comprising the steps of:
s1, adjusting the frequency and amplitude of the radio frequency signal to preset values;
s2, keeping the frequency of the radio frequency signal unchanged, and adjusting the amplitude of the radio frequency signal to enable the amplitude of the radio frequency signal to scan along a specific direction;
s3, when the amplitude of the radio frequency signal is adjusted to the limit value, keeping the amplitude of the radio frequency signal unchanged, and adjusting the frequency of the radio frequency signal so as to enable the frequency of the radio frequency signal to scan along a specific direction;
and S4, stopping scanning when the frequency of the radio frequency signal is adjusted to the limit value, and outputting the detection result of the quality range.
2. The method for broadening the detection mass range of a mass spectrometer as defined in claim 1 wherein said predetermined value of the rf signal frequency is a maximum value.
3. The method for broadening the detection mass range of a mass spectrometer as claimed in claim 2, wherein said predetermined value of the rf signal amplitude is a minimum value.
4. The method for broadening detection mass range of mass spectrometer as claimed in claim 3, wherein said RF signal amplitude is increased in a linear variation from a minimum value to a maximum value in step S2.
5. The method for broadening the detection mass range of a mass spectrometer as claimed in claim 4, wherein said RF signal frequency is decreased in a linear variation from a maximum value to a minimum value in step S3.
6. The method for broadening the detection mass range of a mass spectrometer as claimed in claim 1 wherein said limit is the maximum or minimum of the rf signal frequency or rf signal amplitude that the mass spectrometer is capable of outputting.
7. An apparatus for broadening a detection mass range of a mass spectrometer, comprising:
the numerical value setting module is used for adjusting the frequency and the amplitude of the radio frequency signal to preset values;
the radio frequency signal adjusting module is used for keeping the frequency of the radio frequency signal unchanged and adjusting the amplitude of the radio frequency signal so as to enable the amplitude of the radio frequency signal to scan along a specific direction; or after the amplitude of the radio frequency signal is adjusted to the limit value, keeping the amplitude of the radio frequency signal unchanged, and adjusting the frequency of the radio frequency signal so as to enable the frequency of the radio frequency signal to scan along a specific direction;
and the result output module is used for stopping scanning and outputting the quality range detection result when the frequency of the radio frequency signal is adjusted to the limit value.
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