CN112668839A - Method and device for evaluating performance of ionization device - Google Patents

Method and device for evaluating performance of ionization device Download PDF

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CN112668839A
CN112668839A CN202011455850.2A CN202011455850A CN112668839A CN 112668839 A CN112668839 A CN 112668839A CN 202011455850 A CN202011455850 A CN 202011455850A CN 112668839 A CN112668839 A CN 112668839A
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ionization device
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闻路红
余晓梅
胡舜迪
陈安琪
刘云
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China Innovation Instrument Co ltd
Ningbo University
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Ningbo University
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Abstract

The invention provides an evaluation method and an evaluation device for the performance of an ionization device, wherein the evaluation method for the performance of the ionization device comprises the following steps: (A1) the collecting unit is arranged between an ion outlet of the ionization device and a mass spectrum sample inlet and is used for collecting information of ion current emitted from the ion outlet; (A2) detecting the collecting unit, and obtaining the electrical parameter A of the collecting unit for multiple timesiN is an integer, i is 1,2,3 · N; (A3) according to the electrical parameter AiObtaining an evaluation parameter C;
Figure DDA0002828821540000011
(A4) obtaining an evaluation result of the ionization device according to the evaluation parameter C: if the evaluation parameter C > C0Threshold value C0∈[0.05,0.15]The ionization device is unqualified; if the evaluation parameter C is less than or equal to C0And the ionization device is qualified. Hair brushThe method has the advantages of scientific and accurate evaluation and the like.

Description

Method and device for evaluating performance of ionization device
Technical Field
The present invention relates to a mass spectrometer ionization device, and more particularly, to a method and apparatus for evaluating the performance of an ionization device.
Background
The mass spectrometry has the characteristics of high sensitivity, good specificity and the like, and has the function of being difficult to replace in trace analysis. The direct mass spectrum ionization device is used as a key part of a mass spectrum instrument, and the engineering and industrialization development of the direct mass spectrum ionization device has great promotion effect on the development of the mass spectrum instrument industry in China.
In recent years, the direct mass spectrometry ionization technology is a new revolution in the analysis field, has the advantages of less sample consumption, high analysis speed, real-time in-situ detection support, low detection cost and the like, realizes the application of the mass spectrometry technology in on-site high-throughput analysis, and is a powerful detection weapon in the fields of public safety, food safety, drug analysis, life science and the like.
Modern direct mass spectrometry ionization technology takes ESI as a starting end, DESI, DART and the like are developed successively, and domestic scholars also develop EESI, DBDI, DAPCI, AFAI and other direct ionization technologies, wherein more than 10 types of commercial products are mature and formed. However, the following common problems exist:
1. different direct mass spectrometry ionization devices have different principles, and different performance characteristics and application emphasis points are different. However, due to lack of uniform standards and specifications, the direct mass spectrometry ionization device has many problems of non-uniform performance indexes, inspection methods and the like in the processes of research and development, manufacture, inspection, acceptance and the like, and is easy to cause disputes.
2. The lack of uniform acceptance standards and specifications leads to disorder competition in the direct mass spectrometry ionization device industry to a great extent, and is not beneficial to the promotion of core technology, independent part innovation capability and industrial development in the mass spectrometry field in China.
The existing research is mainly focused on an ion detection end in a mass spectrometer, performance detection analysis is not carried out on the effect of an open type ion source technology, influence factor analysis of a sample detection result in an open type environment is greatly increased, and therefore a device and a method for evaluating the performance of an ionization device are lacked.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides the method for evaluating the performance of the ionization device, which is scientific in evaluation and good in evaluation effect.
The purpose of the invention is realized by the following technical scheme:
a method of evaluating performance of an ionization apparatus, the method comprising:
(A1) the collecting unit is arranged between an ion outlet of the ionization device and a mass spectrum sample inlet and is used for collecting information of ion current emitted from the ion outlet;
(A2) detecting the collecting unit, and obtaining the electrical parameter A of the collecting unit for multiple timesiN is an integer, i is 1,2,3 · N;
(A3) according to the electrical parameter AiObtaining an evaluation parameter C;
Figure RE-GDA0002962643050000021
(A4) obtaining an evaluation result of the ionization device according to the evaluation parameter C:
if the evaluation parameter C > C0Threshold value C0∈[0.05,0.15]The ionization device is unqualified;
if the evaluation parameter C is less than or equal to C0And the ionization device is qualified.
Another object of the present invention is to provide an apparatus for evaluating performance of an ionization apparatus, which is achieved by the following means:
an apparatus for evaluating performance of an ionization apparatus, comprising:
a collecting unit adapted to be disposed between an ion outlet of the ionization device and a mass spectrometry sample inlet for collecting information of an ion stream exiting the ion outlet;
a detection unit detecting an electrical parameter of the collection unitNumber AiN, N is an integer and is transmitted to the calculation unit;
a calculation unit based on the electrical parameter AiCalculating to obtain evaluation parameters
Figure RE-GDA0002962643050000022
Compared with the prior art, the invention has the beneficial effects that:
1. the evaluation is scientific;
a scientific evaluation method is constructed, the ion current emitted by the ionization device is detected, the obtained electrical parameters are converted into evaluation parameters, the evaluation parameters are used for evaluating the working performance of the ionization device, such as the working stability of the emitted ion current, qualified evaluation is given when the performance requirements are met, and the whole evaluation process is scientific and rigorous;
the accuracy of evaluation is improved by scientifically setting the threshold value;
the evaluation method meets the requirements of national standards, and is scientific and reasonable;
2. the evaluation effect is good;
the operating stability (stability of the output ion current) of the ionization device is scientifically evaluated according to the evaluation parameters, and the operating performance of the ionization device is accurately reflected.
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The disclosure of the present invention will become more readily understood with reference to the accompanying drawings. As is readily understood by those skilled in the art: these drawings are only for illustrating the technical solutions of the present invention and are not intended to limit the scope of the present invention. In the figure:
FIG. 1 is a flow chart of a method of evaluating ionization apparatus performance according to an embodiment of the present invention;
fig. 2 is a schematic view of a current detection result according to verification example 1;
FIG. 3 is a secondary mass spectrum of the ice toxin according to verification example 1;
fig. 4 is a schematic view of a current detection result according to verification example 2;
FIG. 5 is a secondary mass spectrum of the ice toxin according to validation example 2;
fig. 6 is a schematic view of a current detection result according to verification example 3;
FIG. 7 is a secondary mass spectrum of glacial toxin according to validation example 3;
fig. 8 is a diagram showing a current detection result according to verification example 4;
FIG. 9 is a secondary mass spectrum of the ice toxin according to verification example 4.
Detailed Description
Fig. 1-9 and the following description depict alternative embodiments of the invention to teach those skilled in the art how to make and use the invention. Some conventional aspects have been simplified or omitted for the purpose of teaching the present invention. Those skilled in the art will appreciate that variations or substitutions from these embodiments will be within the scope of the invention. Those skilled in the art will appreciate that the features described below can be combined in various ways to form multiple variations of the invention. Thus, the present invention is not limited to the following alternative embodiments, but is only limited by the claims and their equivalents.
Example 1:
fig. 1 is a flowchart showing an evaluation method of performance of an ionization apparatus according to an embodiment of the present invention, which includes the steps of, as shown in fig. 1:
(A1) the collecting unit is arranged between an ion outlet of the ionization device and a mass spectrum sample inlet and is used for collecting information of ion current emitted from the ion outlet;
(A2) detecting the collecting unit, and obtaining the electrical parameter A of the collecting unit for multiple timesiSuch as voltage, current and the like, i is 1,2, 3. cndot. N, and N is an integer;
(A3) according to the electrical parameter AiObtaining an evaluation parameter C;
Figure RE-GDA0002962643050000041
(A4) obtaining an evaluation result of the ionization device according to the evaluation parameter C:
if the evaluation parameter C > C0Threshold value C0∈[0.05,0.15]The ionization device is unqualified;
if the evaluation parameter C is less than or equal to C0And the ionization device is qualified.
In order to accurately reflect the working performance of the ionization device, the distance L between the collection unit and the mass spectrum sample inlet is further provided1∈(0，2]mm, distance L between the collecting unit and the ion outlet2∈[5，20]mm。
In order to accurately reflect the working performance of the ionization device, the collecting unit is further annular, and the center of the collecting unit is collinear with the central axis of the mass spectrum sample inlet.
An apparatus for evaluating performance of an ionization apparatus according to an embodiment of the present invention includes:
a collecting unit adapted to be disposed between an ion outlet of the ionization device and a mass spectrometry sample inlet for collecting information of an ion stream exiting the ion outlet;
a detection unit for detecting the electrical parameter A of the collection unitiN, N is an integer and is transmitted to the calculation unit;
a calculation unit based on the electrical parameter AiCalculating to obtain evaluation parameters
Figure RE-GDA0002962643050000051
In order to automatically evaluate the performance of the ionization device, further, the apparatus for evaluating the performance of the ionization device further comprises:
a comparison unit for comparing the evaluation parameter C with a threshold evaluation parameter C0Threshold value C0∈[0.05,0.15]And the comparison result is sent to an evaluation unit.
In order to automatically evaluate the performance of the ionization device, further, the apparatus for evaluating the performance of the ionization device further comprises:
an evaluation unit that outputs an evaluation result according to the comparison result; if the evaluation parameter C > C0The evaluation result is unqualified, if the evaluation parameter C is less than or equal to C0The evaluation result is qualified;
an output unit for outputting the evaluation result.
In order to accurately detect the ion current, further, the collecting unit is ring-shaped, and the electrical parameter is current or voltage.
In order to adapt to mass spectrum injection ports with different heights, further, the device for evaluating the performance of the ionization device further comprises:
the collecting unit is arranged on the bearing unit, and the distance between the collecting unit and the bearing unit is adjustable.
Example 2:
the method for evaluating the performance of the ionization device comprises the following steps of:
(A1) the annular collecting unit is arranged between an ion outlet of the ionization device and a mass spectrum sample inlet and is used for collecting information of ion current emitted from the ion outlet; the central axis of the annular collection unit (of the enclosed region) is collinear with the central axis of the mass spectrum sample inlet;
the distance L between the collection unit and the mass spectrum sample inlet1∈(0，2]mm, e.g. 1mm, 1.4mm, 2mm, etc., the distance L between the collecting unit and the ion outlet2∈[5，20]mm, such as 5mm, 8mm, 12mm, 16mm, 20mm, and the like;
(A2) detecting the collecting unit, and obtaining the electrical parameter A of the collecting unit for multiple timesiIn this embodiment, the electrical parameter is current, i ═ 1,2,3 · · N, N is an integer, for example, 3, 5, 7, 10, 13, 17, 20;
(A3) according to the electrical parameter AiObtaining an evaluation parameter C;
Figure RE-GDA0002962643050000061
(A4) obtaining an evaluation result of the ionization device according to the evaluation parameter C:
if the evaluation parameter C > C0Threshold value C0∈[0.05,0.15]E.g., 0.05, 0.08, 0.1, 0.15, the ionization apparatus failed;
if the evaluation parameter C is less than or equal to C0And the ionization device is qualified.
An apparatus for evaluating performance of an ionization apparatus according to an embodiment of the present invention includes:
the collection unit is supported by an annular conductor and is suitable for being arranged between an ion outlet and a mass spectrum sample inlet of the ionization device and used for collecting information of an ion flow emitted from the ion outlet; the central axis of the annular collection unit (of the enclosed region) is collinear with the central axis of the mass spectrum sample inlet; the distance L between the collection unit and the mass spectrum sample inlet1∈(0，2]mm, e.g. 1mm, 1.4mm, 2mm, etc., the distance L between the collecting unit and the ion outlet2∈[5，20]mm, such as 5mm, 8mm, 12mm, 16mm, 20mm, and the like;
the collection unit is arranged on the bearing unit, and the distance between the collection unit and the bearing unit is adjustable, so that the collection unit is suitable for mass spectrum sample inlets with different heights;
a detection unit for detecting the electrical parameter A of the collection unitiN, N is an integer and is transmitted to the calculation unit; in this embodiment, N is 20, the electrical parameter is current, and the current detection is the prior art in the field;
a calculation unit based on the electrical parameter AiCalculating to obtain evaluation parameters
Figure RE-GDA0002962643050000071
A comparison unit for comparing the evaluation parameter C with a threshold evaluation parameter C0Threshold value C0∈[0.05,0.15]E.g. 0.05, 0.08, 0.1, 0.15, the comparison result is sent to an evaluation unit;
an evaluation unit that outputs an evaluation result according to the comparison result; if the evaluation parameter C > C0The evaluation result is unqualified, if the evaluation parameter C is less than or equal to C0The evaluation result is qualified;
an output unit for outputting the evaluation result.
Verification example 1:
a DBDI ionization apparatus plasma beam stability experiment was performed according to the evaluation method and apparatus in example 2.
Annular collection unit from ion exit of ion source: 15mm, and the distance between the annular collection unit and the mass spectrum sample inlet is 2 mm;
a current detector: a current detection sensor (HET50mab15U 10);
sample preparation: methamphetamine (methamphetamine), 100 ppb.
The annular collection unit is placed between the ion source and the mass spectrum through the bearing unit, an ion outlet of the ion source, the annular collection unit and a mass spectrum sample inlet are coaxial, and a sample introduction experiment is carried out through a capillary tube.
The experimental results are as follows:
FIG. 2 is a diagram of the current detection result of the DBDI ion source, which is used for measuring the ion current value for 7 times continuously, carrying out high resolution and sectional adoption, and capturing the waveform to carry out data processing in a performance evaluation system. Taking specific frequency 3200 as a period, obtaining a maximum value at each period point by adopting a peak searching algorithm, carrying out sliding average at 1700-1950 points to obtain a corresponding numerical value, obtaining 7 groups of data by maximum current 8.980mA, wherein C is 0.051, and a threshold value C is0When the DBDI ionization device is an atmospheric pressure ionization device, the threshold thereof is set to 10% because the DBDI ionization device is completely placed under atmospheric pressure and is greatly affected by the environment, it is found that the DBDI ionization device performance is judged to be acceptable.
FIG. 3 shows a secondary mass spectrum of the DBDI ionization device for detecting the ice toxicity, wherein m/z of a parent ion is 118.92, the signal intensity is 8.14E3, the detection result is well matched with the ion current detection result, and the effectiveness of the evaluation method and the device for detecting and measuring the ionization device by utilizing the ion current is fully verified.
Verification example 2:
a second DBDI ionization apparatus plasma beam stability experiment was conducted according to the evaluation method and apparatus of example 2.
Annular collection unit from ion exit of ion source: 15mm, and the distance between the annular collection unit and the mass spectrum sample inlet is 2 mm;
a current detector: a current detection sensor (HET50mab15U 10);
sample preparation: methamphetamine (methamphetamine), 100 ppb.
The annular collection unit is placed between the ion source and the mass spectrum through the bearing unit, an ion outlet of the ion source, the annular collection unit and a mass spectrum sample inlet are coaxial, and a sample introduction experiment is carried out through a capillary tube.
The experimental results are as follows:
fig. 4 is a diagram of a DBDI ion source current detection result, which is used for measuring an ion current value for 7 times continuously, performing high resolution and sectional adoption, and capturing a waveform to perform data processing in a performance evaluation system. Taking a specific frequency 3200 as a period, obtaining a maximum value at each period point by adopting a peak searching algorithm, carrying out sliding average at 1700-1950 points to obtain a corresponding numerical value, obtaining 7 groups of data by a maximum current 6.943mA, wherein C is 0.231, and a threshold value C0When the DBDI ionization device performance is determined to be not good, the DBDI ionization device performance is determined to be not good (the threshold value is set to 10% because the DBDI ionization device is greatly affected by the environment).
FIG. 5 shows the second DBDI ionization device detecting the secondary mass spectrum of the ice toxicity, no mass spectrum signal is detected, and rework is required. The detection result is well matched with the ion current detection result, and the effectiveness of the evaluation method and the device for detecting and measuring the ionization device by using the ion current is fully verified.
Verification example 3:
a Nano ESI ionization apparatus plasma beam reproducibility experiment was performed according to the evaluation method and apparatus in example 2
Annular collection unit from ion exit of ion source: 5mm, and the distance between the annular collection unit and the mass spectrum sample inlet is 2 mm;
a current detector: a skin safety watch;
sample preparation: methamphetamine (methamphetamine), 100 ppb.
The Nano ESI source is excited by direct current high voltage (3KV), the current is very small (dozens of nA level), the current value cannot be detected through a current loop, and therefore the scheme is changed into a scheme of passing through a metal plate (the area is 3 x 5 cm)2) The ion beam current was absorbed and then the current on the metal plate was converted to a voltage value by a picoammeter, the sample flow rate was 5 uL/min.
The experimental results are as follows:
the high voltage of Nano ESI adopts direct current high voltage, and the Nano ESI adopts acquisition card continuously to continuously sample data.
Fig. 6 is a graph showing the detection result of Nano ESI source current, in which 7 sets of data (hereinafter, data 1 second and 6 points) were obtained with an average current of 17nA, C being 0.018, and a threshold value C0When the Nano ESI ionization apparatus performance was judged to be acceptable, the Nano ESI ionization apparatus performance was judged to be 0.05 (the threshold was set to 5% since the Nano ESI ionization apparatus is less affected by the environment).
FIG. 7 shows a secondary mass spectrum of the Nano ESI ionization device for detecting the acidosis, wherein m/z of a parent ion is 119.03, signal intensity is 9.47E3, and a detection result is well matched with an ion flow detection result, so that the effectiveness of the method and the device for evaluating the ionization device by using ion current detection is fully verified.
Verification example 4:
a plasma beam repeatability test using the PDESI ionizer was conducted in accordance with the evaluation method and apparatus described in example 2.
Annular collection unit from ion exit of ion source: 15mm, and the distance between the annular collection unit and the mass spectrum sample inlet is 5 mm;
a current detector: a skin safety watch;
sample preparation: methamphetamine (methamphetamine), 100 ppb.
Because the PDESI ionization device adopts direct current high voltage (3KV) excitation, the PDESI ionization device passes through a metal plate (the area is 3 x 5 cm)2) And absorbing the current of the ion beam, and converting the current on the metal plate into a voltage value through a self-made current detection tool. The sample is dipped through a capillary glass tube, and the distance between the dipped solution and the tip of the tube is about 5 mm.
The experimental results are as follows:
the PDESI high pressure adopts direct current high pressure, and because the liquid volume of the capillary tube is limited, the caffeine touch injection is completed within 1-2 s of one-time sample injection, so that multiple sample injection is needed to obtain experimental data.
Fig. 8 is a graph showing the current detection results of the PDESI ionizer, where the maximum current 280nA is calculated by taking the maximum value because the number of sampling points is small, and the performance evaluation system is obtained by obtaining 7 sets of data (hereinafter, data is set at 6 points for 1 second), where C is 0.032, and the threshold C is set to 0.0320When the PDESI ionization apparatus performance is determined to be acceptable, the PDESI ionization apparatus performance is determined to be 0.05 (the threshold value is set to 5% since the PDESI ionization apparatus is less affected by the environment).
Fig. 9 shows a secondary mass spectrum of the PDESI ionization device for detecting the ice toxicity, wherein m/z of the parent ion is 119.05, the signal intensity is 6.15E3, the detection result is well matched with the detection result of the ion current, and the effectiveness of the method and the device for evaluating the ionization device by using the ion current detection is fully verified.
Through the above three sets of experiments, the experimental data are shown in the following table, and can be obtained: although the three ionization devices used in the experiment have different principles and cannot be compared with the ionization devices of the same type, evaluation parameters below a threshold value can obtain good mass spectrum signals, and the effectiveness of the evaluation method and the evaluation device for measuring the ionization devices by using ion current detection is further proved.
Test result table for three ionization devices
Serial number Ionization device Test sample Detecting the concentration of a sample Evaluation parameter C Second order mass spectrum signal intensity
1 DBDI-1 Ice toxin 100ppb 0.052 8.14E3
2 DBDI-2 Ice toxin 100ppb 0.231 0
3 Nano ESI Ice toxin 100ppb 0.018 9.47E3
4 PDESI Ice toxin 100ppb 0.032 6.15E3

Claims (10)

1. A method of evaluating performance of an ionization apparatus, the method comprising:
(A1) the collecting unit is arranged between an ion outlet of the ionization device and a mass spectrum sample inlet and is used for collecting information of ion current emitted from the ion outlet;
(A2) detecting the collecting unit, and obtaining the electrical parameter A of the collecting unit for multiple timesiI is 1,2,3 … N, N is an integer;
(A3) according to the electrical parameter AiObtaining an evaluation parameter C;
Figure FDA0002828821510000011
(A4) obtaining an evaluation result of the ionization device according to the evaluation parameter C:
if the evaluation parameter C > C0Threshold value C0∈[0.05,0.15]The ionization device is unqualified;
if the evaluation parameter C is less than or equal to C0And the ionization device is qualified.
2. The method of claim 1, wherein the distance L between the collection unit and the mass spectrometer sample inlet is less than the mass spectrometer sample inlet1∈(0，2]mm, distance L between the collecting unit and the ion outlet2∈[5，20]mm。
3. The method of claim 1, wherein the collection unit is in a ring shape or a plate shape, and a center of the collection unit and a central axis of the mass spectrometer inlet are collinear.
4. The method of claim 1, wherein the electrical parameter is voltage or current.
5. The method of claim 1, wherein the ionization device is a direct mass spectrometry ion source.
6. An apparatus for evaluating performance of an ionization apparatus, comprising:
a collecting unit adapted to be disposed between an ion outlet of the ionization device and a mass spectrometry sample inlet for collecting information of an ion stream exiting the ion outlet;
a detection unit for detecting the electrical parameter A of the collection unitiI is 1,2,3 … N, N is an integer and is transmitted to the calculation unit;
a calculation unit based on the electrical parameter AiCalculating to obtain evaluation parameters
Figure FDA0002828821510000021
7. The apparatus according to claim 6, wherein the apparatus further comprises:
a comparison unit for comparing the evaluation parameter C with a threshold evaluation parameter C0Threshold value C0∈[0.05,0.15]And the comparison result is sent to an evaluation unit.
8. The apparatus according to claim 7, wherein the apparatus further comprises:
an evaluation unit that outputs an evaluation result according to the comparison result; if the evaluation parameter C > C0The evaluation result is unqualified, if the evaluation parameter C is less than or equal to C0The evaluation result is qualified;
an output unit for outputting the evaluation result.
9. The apparatus of claim 6, wherein the collection unit is ring-shaped, and the electrical parameter is current or voltage.
10. The apparatus according to claim 6, wherein the apparatus further comprises:
the collecting unit is arranged on the bearing unit, and the distance between the collecting unit and the bearing unit is adjustable.
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Application publication date: 20210416