CN112924523A - Mass spectrum detection system and method with rapid extraction function for detecting pesticide residues - Google Patents

Mass spectrum detection system and method with rapid extraction function for detecting pesticide residues Download PDF

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Publication number
CN112924523A
CN112924523A CN202110119789.2A CN202110119789A CN112924523A CN 112924523 A CN112924523 A CN 112924523A CN 202110119789 A CN202110119789 A CN 202110119789A CN 112924523 A CN112924523 A CN 112924523A
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China
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module
sample
map
mass
pesticide
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Inventor
李建勋
李熠
邓凯琳
范春林
陈辉
张�荣
高敏
刘淑艳
单吉浩
张紫鹃
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Institute of Food Science and Technology of CAAS
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Institute of Food Science and Technology of CAAS
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/62Investigating 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
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/34Purifying; Cleaning
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40Concentrating samples

Abstract

The invention belongs to the technical field of pesticide detection, and discloses a mass spectrum detection system and a mass spectrum detection method for detecting pesticide residues with a rapid extraction function, wherein the mass spectrum detection system for detecting the pesticide residues with the rapid extraction function comprises the following components: the device comprises a sample extraction module, a solid phase extraction module, a sample ionization module, a map acquisition module, a display module, a central processing module, a communication module, a cloud service module, a mass spectrometry module, a map processing module, a map storage module and a pesticide residue evaluation module. According to the invention, a sample is treated through a solid phase extraction module, a target compound and impurities are reserved through solid phase extraction, and whether the components of the sample contain pesticide residues or not is comprehensively detected; corresponding map information can be accurately acquired through the map acquisition module and the map processing module, and corresponding map data are provided for judging whether pesticide is remained on the product; the cloud server is used for processing data by utilizing a big data processing technology, so that the speed and the precision of data judgment are improved.

Description

Mass spectrum detection system and method with rapid extraction function for detecting pesticide residues
Technical Field
The invention belongs to the technical field of pesticide detection, and particularly relates to a mass spectrum detection system and method with a rapid extraction function for detecting pesticide residues.
Background
At present, the detection technology of the pesticide residue which is relatively popular in China needs to be realized by means of instruments such as a liquid chromatograph or a gas chromatograph, wherein a sample which needs to be detected needs to be subjected to complex pretreatment, and the treatment steps comprise: firstly, an agricultural product sample is crushed, a certain solvent is added for extraction, an extracting solution is injected into an activated solid phase extraction column to remove impurities, then a specific eluent is used for eluting pesticide residues, the eluent enters a liquid chromatograph or a gas chromatograph through a filtering device and then enters a mass spectrometer for detection, so that the detection sensitivity and the result accuracy are ensured. The detection mode has the defects and problems that the pretreatment and analysis processes of a detected sample need several hours, the procedure is complex, the process is complicated, the time is long, the efficiency is low, and the working intensity of an operator is high.
Through the above analysis, the problems and defects of the prior art are as follows: in the prior art, the pretreatment and analysis processes of a detected sample need several hours, the procedure is complex, the process is complicated, the time is long, the efficiency is low, and the working intensity of an operator is high.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a mass spectrum detection system and a mass spectrum detection method for detecting pesticide residues with a rapid extraction function.
The invention is realized in such a way that a mass spectrometric detection method for detecting pesticide residues with a rapid extraction function comprises the following steps:
the method comprises the following steps that firstly, a sample extraction module carries out quantitative extraction on a sample to be detected to obtain a corresponding detection sample; the solid phase extraction module is used for treating a sample, and a target compound and impurities are reserved by solid phase extraction;
step two, the central processing module is respectively connected with the sample extraction module, the solid phase extraction module, the sample ionization module, the map acquisition module, the display module, the communication module, the mass spectrometry module, the map processing module, the map storage module and the pesticide residue evaluation module, and coordinates normal operation of the modules;
step three, the sample ionization module ionizes the sample under the high vacuum condition through an ion source; the ionized molecules are further broken into a plurality of fragment ions with smaller mass and neutral particles due to receiving excessive energy; acquiring average kinetic energy with the same energy under the action of an accelerating electric field and enabling the average kinetic energy to enter a mass analyzer, wherein the mass analyzer separates ions with different masses entering the mass analyzer at the same time according to the mass-to-charge ratio;
step four, the spectrum acquisition module respectively leads in the separated ions through an ion detector, acquires amplified ion signals and draws the amplified ion signals into a mass spectrum; the spectrum processing module processes the acquired mass spectrum through an image processing program;
step five, the mass spectrometry module carries out comparative analysis through a prestored map and a detected map to judge whether pesticide residues are contained; meanwhile, the pesticide residue evaluation module compares the pesticide residue content with the standard according to the acquired map, and evaluates the grade of the pesticide residue content to determine whether the pesticide residue can be eaten or not; the map storage module is used for storing maps through a storage;
step six, the communication module realizes information interaction between the central processing module and the cloud service module through signal transmission equipment; the cloud service module processes data by using a big data processing technology through a cloud server; the display module is used for displaying data in the whole system through a display screen;
in the first step, the solid phase extraction module processes the sample, and the specific process of solid phase extraction and target compound retention is as follows:
removing impurities in the small column and creating a certain solvent environment in the process of extracting a sample to be detected by an extractor;
dissolving the sample with a solvent, transferring into a column and retaining the components on the column;
removing the interferents to the maximum extent by a leaching mode;
eluting the measured substance with small volume of solvent and collecting;
in the fifth step, the mass spectrometry module performs comparative analysis through the prestored map and the detected map, and the specific process of judging whether pesticide residues are contained is as follows:
extracting corresponding features from a pre-stored map and a detected map, and generating a feature descriptor for the extracted features;
determining the similarity between the feature descriptors in the two maps, comparing the similarity with a certain threshold value, and judging whether the two maps are similar;
when the two maps are similar, judging whether the sample contains pesticide residues or not according to the description of the characteristics in the prestored maps;
in the fifth step, the specific process of the pesticide residue evaluation module is as follows:
detecting the content of the residual pesticide, comparing the content with the standard content, and if the content exceeds the standard content, the pesticide cannot be eaten; if the pesticide remains within the standard range, the product can be eaten.
Further, in the first step, the sample is extracted by using a disposable syringe, and the quantitative extraction can be measured by using a measuring cup.
Further, in the first step, the solid phase extraction module processes the sample, and the specific process of solid phase extraction and impurity retention is as follows:
in the process of extracting a sample to be detected through an extractor, removing impurities in the column and creating a certain solvent environment;
transferring the sample into a column, wherein most of the target compound flows out along with the base solution of the sample, impurities are retained on the column, and the impurities are continuously collected;
the fractions were rinsed off with a small volume of solvent and collected, and the pools were combined.
Further, in the fourth step, the processing process of the acquired mass spectrogram by the spectrogram processing module is as follows:
establishing an image processing set for the acquired mass spectrogram, and carrying out gray processing;
after the gray level processing of the image is finished, geometric transformation is carried out;
and enhancing the image through an image filtering algorithm.
Further, the geometric transformation comprises: mass spectrogram translation, mass spectrogram transposition, mass spectrogram mirror image, mass spectrogram rotation and mass spectrogram scaling.
Further, the specific process of enhancing the mass spectrogram is as follows:
determining a certain circular neighborhood in the image after the geometric change is finished;
determining the pixel value of the image in the circular neighborhood, and calculating the average value of the pixels in the circular neighborhood;
and taking the average value of the pixels as the pixel value in the circular neighborhood, and continuously moving the circular neighborhood to correct the pixels of the image.
Another object of the present invention is to provide a mass spectrometric detection system for detecting pesticide residue with a rapid extraction function, which implements the mass spectrometric detection method for detecting pesticide residue with a rapid extraction function, the mass spectrometric detection system for detecting pesticide residue with a rapid extraction function comprising:
the sample extraction module is connected with the central processing module and is used for quantitatively extracting the sample to be detected to obtain a corresponding detection sample;
the solid phase extraction module is connected with the central processing module and is used for processing the sample, and the target compound and impurities are reserved by solid phase extraction; the solid phase extraction module processes a sample, and the specific process of retaining a target compound by solid phase extraction comprises the following steps: removing impurities in the small column and creating a certain solvent environment in the process of extracting a sample to be detected by an extractor; dissolving the sample with a solvent, transferring into a column and retaining the components on the column; removing the interferents to the maximum extent by a leaching mode; eluting the measured substance with small volume of solvent and collecting; the solid phase extraction module processes a sample, and the specific process of solid phase extraction and impurity retention is as follows: in the process of extracting a sample to be detected through an extractor, removing impurities in the column and creating a certain solvent environment; transferring the sample into a column, wherein most of the target compound flows out along with the base solution of the sample, impurities are retained on the column, and the impurities are continuously collected; eluting the components with a small volume of solvent and collecting, and combining the collected solutions;
the sample ionization module is connected with the central processing module and ionizes the sample under the high vacuum condition through an ion source; the ionized molecules are further broken into a plurality of fragment ions with smaller mass and neutral particles due to receiving excessive energy; acquiring average kinetic energy with the same energy under the action of an accelerating electric field and enabling the average kinetic energy to enter a mass analyzer, wherein the mass analyzer separates ions with different masses entering the mass analyzer at the same time according to the mass-to-charge ratio;
the spectrum acquisition module is connected with the central processing module, and is used for respectively introducing the separated ions through the ion detector, acquiring amplified ion signals and drawing a mass spectrum;
the display module is connected with the central processing module and is used for displaying the data in the whole system through a display screen;
and the central processing module is respectively connected with the sample extraction module, the solid-phase extraction module, the sample ionization module, the map acquisition module, the display module, the communication module, the mass spectrometry module, the map processing module, the map storage module and the pesticide residue evaluation module, and coordinates normal operation of the modules.
Further, the mass spectrometric detection system for pesticide residue detection with a rapid extraction function further comprises:
the communication module is connected with the central processing module and realizes information interaction between the central processing module and the cloud service module through the signal transmission equipment;
the cloud service module is connected with the communication module and is used for processing data by utilizing a big data processing technology through a cloud server;
the mass spectrum analysis module is connected with the central processing module, and is used for comparing and analyzing a prestored map and a detected map to judge whether pesticide residues are contained; the mass spectrometry module carries out comparison analysis through a prestored map and a detected map, and the specific process of judging whether pesticide residues are contained is as follows: extracting corresponding features from a pre-stored map and a detected map, and generating a feature descriptor for the extracted features; determining the similarity between the feature descriptors in the two maps, comparing the similarity with a certain threshold value, and judging whether the two maps are similar; when the two maps are similar, judging whether the sample contains pesticide residues or not according to the description of the characteristics in the prestored maps;
the spectrum processing module is connected with the central processing module and is used for processing the acquired mass spectrum through an image processing program; the processing process of the acquired mass spectrogram by the spectrogram processing module comprises the following steps: establishing an image processing set for the acquired mass spectrogram, and carrying out gray processing; after the gray level processing of the image is finished, geometric transformation is carried out; enhancing the image through an image filtering algorithm;
and the map storage module is connected with the central processing module and used for storing the map through the storage.
The pesticide residue evaluation module is connected with the central processing module, compares the pesticide residue content with the standard according to the acquired map, and evaluates the grade of the pesticide residue content to determine whether the pesticide residue can be eaten or not; the specific process of the pesticide residue evaluation module comprises the following steps: detecting the content of the residual pesticide, comparing the content with the standard content, and if the content exceeds the standard content, the pesticide cannot be eaten; if the pesticide remains within the standard range, the product can be eaten;
another object of the present invention is to provide a computer program product stored on a computer readable medium, which includes a computer readable program for providing a user input interface to implement the method for mass spectrometry for pesticide residue detection with fast extraction function when the computer program product is executed on an electronic device.
Another object of the present invention is to provide a computer-readable storage medium storing instructions which, when executed on a computer, cause the computer to execute the mass spectrometry for pesticide residue detection with rapid extraction function.
By combining all the technical schemes, the invention has the advantages and positive effects that: according to the invention, a sample is treated through a solid phase extraction module, a target compound and impurities are reserved through solid phase extraction, and whether the components of the sample contain pesticide residues or not is comprehensively detected; according to the invention, through the map acquisition module and the map processing module, corresponding map information can be accurately acquired, and corresponding map data is provided for judging whether pesticide is remained on the product; according to the invention, the cloud server is used for processing the data by utilizing a big data processing technology, so that the speed and the precision of data judgment are improved. Meanwhile, the precision of the judgment result can be improved by arranging the mass spectrometry module and the pesticide residue evaluation module.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings needed to be used in the embodiments of the present application will be briefly described below, and it is obvious that the drawings described below are only some embodiments of the present application, and it is obvious for those skilled in the art that other drawings can be obtained from the drawings without creative efforts.
Fig. 1 is a schematic structural diagram of a mass spectrometry detection system with a rapid extraction function for detecting pesticide residues provided by an embodiment of the present invention.
Fig. 2 is a flow chart of a mass spectrometry detection method for detecting pesticide residues with a rapid extraction function according to an embodiment of the present invention.
FIG. 3 is a flow chart of a method for processing a sample by a solid phase extraction module and retaining a target compound by solid phase extraction according to an embodiment of the present invention.
FIG. 4 is a flow chart of a method for processing a sample and retaining impurities by solid phase extraction using the solid phase extraction module according to the embodiment of the present invention.
Fig. 5 is a flowchart of a method for determining whether pesticide residue is contained by comparing and analyzing a pre-stored spectrum and a detected spectrum by a mass spectrometry module according to an embodiment of the present invention.
In the figure: 1. a sample extraction module; 2. a solid phase extraction module; 3. a sample ionization module; 4. the map acquisition module; 5. a display module; 6. a central processing module; 7. a communication module; 8. a cloud service module; 9. a mass spectrometry module; 10. a map processing module; 11. the map storage module; 12. and a pesticide residue evaluation module.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Aiming at the problems in the prior art, the invention provides a mass spectrometry detection system and a mass spectrometry detection method for pesticide residue detection with a rapid extraction function, and the technical scheme of the invention is described in detail below by combining with the accompanying drawings.
As shown in fig. 1, the mass spectrometry detection system for detecting pesticide residue with a rapid extraction function provided in the embodiment of the present invention includes:
the sample extraction module 1 is connected with the central processing module 6 and is used for quantitatively extracting a sample to be detected to obtain a corresponding detection sample;
and the solid phase extraction module 2 is connected with the central processing module 6 and is used for processing the sample, and the target compound and impurities are reserved by solid phase extraction.
The sample ionization module 3 is connected with the central processing module 6 and ionizes the sample under the high vacuum condition through an ion source; the ionized molecules are further fragmented into a plurality of fragment ions and neutral particles of smaller mass due to the excessive energy received. The ions with different masses entering the mass analyzer at the same time are separated according to the mass-to-charge ratio.
And the spectrum acquisition module 4 is connected with the central processing module 6, and is used for introducing the separated ions through the ion detector, acquiring amplified ion signals and drawing a mass spectrum.
And the display module 5 is connected with the central processing module 6 and is used for displaying the data in the whole system through a display screen.
The central processing module 6 is respectively connected with the sample extraction module 1, the solid phase extraction module 2, the sample ionization module 3, the spectrum acquisition module 4, the display module 5, the communication module 7, the mass spectrometry module 9, the spectrum processing module 10, the spectrum storage module 11 and the pesticide residue evaluation module 12, and coordinates normal operation of each module.
And the communication module 7 is connected with the central processing module 6, and realizes information interaction between the central processing module and the cloud service module through signal transmission equipment.
And the cloud service module 8 is connected with the communication module 7 and processes data by utilizing a big data processing technology through a cloud server.
And the mass spectrum analysis module 9 is connected with the central processing module 6, and judges whether pesticide residues are contained or not by comparing and analyzing a prestored map and a detected map.
And the spectrum processing module 10 is connected with the central processing module 6 and is used for processing the acquired mass spectrum through an image processing program.
And the map storage module 11 is connected with the central processing module 6 and used for storing maps through the storage.
And the pesticide residue evaluation module 12 is connected with the central processing module 6, compares the pesticide residue content with the standard according to the acquired map, and evaluates the grade of the pesticide residue content to determine whether the pesticide residue can be eaten.
As shown in fig. 2, the mass spectrometry detection method for detecting pesticide residue with a rapid extraction function provided in the embodiment of the present invention includes:
s101: the sample extraction module quantitatively extracts a sample to be detected to obtain a corresponding detection sample; and the solid phase extraction module is used for treating the sample, and the target compound and impurities are reserved by solid phase extraction.
S102: the central processing module is respectively connected with the sample extraction module, the solid phase extraction module, the sample ionization module, the map acquisition module, the display module, the communication module, the mass spectrometry module, the map processing module, the map storage module and the pesticide residue evaluation module, and coordinates normal operation of the modules.
S103: the sample ionization module ionizes a sample under a high vacuum condition through an ion source; the ionized molecules are further broken into a plurality of fragment ions with smaller mass and neutral particles due to receiving excessive energy; the ions with different masses entering the mass analyzer at the same time are separated according to the mass-to-charge ratio.
S104: the spectrum acquisition module is respectively introduced with the separated ions through an ion detector, acquires amplified ion signals and draws the amplified ion signals into a mass spectrum; and the spectrum processing module processes the acquired mass spectrum through an image processing program.
S105: the mass spectrometry module compares and analyzes a prestored map and a detected map to judge whether pesticide residues are contained; meanwhile, the pesticide residue evaluation module compares the pesticide residue content with the standard according to the acquired map, and evaluates the grade of the pesticide residue content to determine whether the pesticide residue can be eaten or not; the map storage module is used for storing the map through the storage.
S106: the communication module realizes information interaction between the central processing module and the cloud service module through the signal transmission equipment; the cloud service module processes data by using a big data processing technology through a cloud server; the display module is used for displaying the data in the whole system through the display screen.
In S101 provided by the embodiment of the present invention, a disposable syringe is used for sample extraction, and a measuring cup can be used for quantitative extraction.
In S101 provided by the embodiment of the present invention, a solid phase extraction module processes a sample, and a specific process for retaining a target compound by solid phase extraction includes:
s201: in the process of extracting a sample to be detected through the extractor, impurities in the small column are removed and a certain solvent environment is created.
S202: the sample is dissolved with a solvent, transferred to the column and the components are retained on the column.
S203: the interfering substances are removed to the maximum extent by means of rinsing.
S204: the test substance is eluted with a small volume of solvent and collected.
In S101 provided by the embodiment of the present invention, a solid phase extraction module processes a sample, and a specific process of solid phase extraction to retain impurities includes:
s301: in the process of extracting a sample to be detected through the extractor, impurities in the column are removed and a certain solvent environment is created.
S302: and transferring the sample into the column, wherein most of the target compound flows out along with the sample base solution, and impurities are retained on the column and are continuously collected.
S303: the fractions were rinsed off with a small volume of solvent and collected, and the pools were combined.
In S104 provided by the embodiment of the present invention, the processing process of the acquired mass spectrogram by the spectrogram processing module is as follows:
establishing an image processing set for the acquired mass spectrogram, and carrying out gray processing;
after the gray level processing of the image is finished, geometric transformation is carried out;
and enhancing the image through an image filtering algorithm.
The geometric transformation includes: mass spectrogram translation, mass spectrogram transposition, mass spectrogram mirror image, mass spectrogram rotation and mass spectrogram scaling.
The specific process for enhancing the mass spectrogram comprises the following steps:
determining a certain circular neighborhood in the image after the geometric change is finished;
determining the pixel value of the image in the circular neighborhood, and calculating the average value of the pixels in the circular neighborhood;
and taking the average value of the pixels as the pixel value in the circular neighborhood, and continuously moving the circular neighborhood to correct the pixels of the image.
In S105 provided by the embodiment of the present invention, the mass spectrometry module performs comparative analysis on the pre-stored spectrum and the detected spectrum, and the specific process of determining whether pesticide residues are contained is as follows:
s401: extracting corresponding features from a pre-stored map and a detected map, and generating a feature descriptor for the extracted features;
s402: determining the similarity between the feature descriptors in the two maps, comparing the similarity with a certain threshold value, and judging whether the two maps are similar;
s403: and when the two maps are similar, judging whether the sample contains pesticide residues or not according to the description of the characteristics in the pre-stored maps.
In S105 provided by the embodiment of the present invention, the specific process of the pesticide residue evaluation module evaluation is as follows:
detecting the content of the residual pesticide, comparing the content with the standard content, and if the content exceeds the standard content, the pesticide cannot be eaten; if the pesticide remains within the standard range, the product can be eaten.
In the description of the present invention, "a plurality" means two or more unless otherwise specified; the terms "upper", "lower", "left", "right", "inner", "outer", "front", "rear", "head", "tail", and the like, indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, are only for convenience in describing and simplifying the description, and do not indicate or imply that the device or element referred to must have a particular orientation, be constructed in a particular orientation, and be operated, and thus, should not be construed as limiting the invention. Furthermore, the terms "first," "second," "third," and the like are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention, and the scope of the present invention is not limited thereto, and any modification, equivalent replacement, and improvement made by those skilled in the art within the technical scope of the present invention disclosed herein, which is within the spirit and principle of the present invention, should be covered by the present invention.

Claims (10)

1. A mass spectrometric detection method for pesticide residue detection with a rapid extraction function is characterized in that the mass spectrometric detection method for pesticide residue detection with a rapid extraction function comprises the following steps:
the method comprises the following steps that firstly, a sample extraction module carries out quantitative extraction on a sample to be detected to obtain a corresponding detection sample; the solid phase extraction module is used for treating a sample, and a target compound and impurities are reserved by solid phase extraction;
step two, the central processing module is respectively connected with the sample extraction module, the solid phase extraction module, the sample ionization module, the map acquisition module, the display module, the communication module, the mass spectrometry module, the map processing module, the map storage module and the pesticide residue evaluation module, and coordinates normal operation of the modules;
step three, the sample ionization module ionizes the sample under the high vacuum condition through an ion source; the ionized molecules are further broken into a plurality of fragment ions with smaller mass and neutral particles due to receiving excessive energy; acquiring average kinetic energy with the same energy under the action of an accelerating electric field and enabling the average kinetic energy to enter a mass analyzer, wherein the mass analyzer separates ions with different masses entering the mass analyzer at the same time according to the mass-to-charge ratio;
step four, the spectrum acquisition module respectively leads in the separated ions through an ion detector, acquires amplified ion signals and draws the amplified ion signals into a mass spectrum; the spectrum processing module processes the acquired mass spectrum through an image processing program;
step five, the mass spectrometry module carries out comparative analysis through a prestored map and a detected map to judge whether pesticide residues are contained; meanwhile, the pesticide residue evaluation module compares the pesticide residue content with the standard according to the acquired map, and evaluates the grade of the pesticide residue content to determine whether the pesticide residue can be eaten or not; the map storage module is used for storing maps through a storage;
step six, the communication module realizes information interaction between the central processing module and the cloud service module through signal transmission equipment; the cloud service module processes data by using a big data processing technology through a cloud server; the display module is used for displaying data in the whole system through a display screen;
in the first step, the solid phase extraction module processes the sample, and the specific process of solid phase extraction and target compound retention is as follows:
removing impurities in the small column and creating a certain solvent environment in the process of extracting a sample to be detected by an extractor;
dissolving the sample with a solvent, transferring into a column and retaining the components on the column;
removing the interferents to the maximum extent by a leaching mode;
eluting the measured substance with small volume of solvent and collecting;
in the fifth step, the mass spectrometry module performs comparative analysis through the prestored map and the detected map, and the specific process of judging whether pesticide residues are contained is as follows:
extracting corresponding features from a pre-stored map and a detected map, and generating a feature descriptor for the extracted features;
determining the similarity between the feature descriptors in the two maps, comparing the similarity with a certain threshold value, and judging whether the two maps are similar;
when the two maps are similar, judging whether the sample contains pesticide residues or not according to the description of the characteristics in the prestored maps;
in the fifth step, the specific process of the pesticide residue evaluation module is as follows:
detecting the content of the residual pesticide, comparing the content with the standard content, and if the content exceeds the standard content, the pesticide cannot be eaten; if the pesticide remains within the standard range, the product can be eaten.
2. The method for mass spectrometry detection of pesticide residue with rapid extraction function as claimed in claim 1, wherein in the first step, the sample is extracted by using a disposable syringe, and the quantitative extraction is measured by using a measuring cup.
3. The mass spectrometry detection method for pesticide residue detection with the rapid extraction function according to claim 1, wherein in the step one, the solid phase extraction module processes the sample, and the specific process of solid phase extraction and impurity retention is as follows:
in the process of extracting a sample to be detected through an extractor, removing impurities in the column and creating a certain solvent environment;
transferring the sample into a column, wherein most of the target compound flows out along with the base solution of the sample, impurities are retained on the column, and the impurities are continuously collected;
the fractions were rinsed off with a small volume of solvent and collected, and the pools were combined.
4. The mass spectrometry detection method for pesticide residue detection with a rapid extraction function according to claim 1, wherein in the fourth step, the processing process of the acquired mass spectrogram by the spectrogram processing module comprises:
establishing an image processing set for the acquired mass spectrogram, and carrying out gray processing;
after the gray level processing of the image is finished, geometric transformation is carried out;
and enhancing the image through an image filtering algorithm.
5. The mass spectrometry detection method for pesticide residue detection with rapid extraction function according to claim 4, wherein the geometric transformation comprises: mass spectrogram translation, mass spectrogram transposition, mass spectrogram mirror image, mass spectrogram rotation and mass spectrogram scaling.
6. The method for mass spectrometry detection of pesticide residue with rapid extraction function of claim 4, wherein the specific process for enhancing the mass spectrogram is as follows:
determining a certain circular neighborhood in the image after the geometric change is finished;
determining the pixel value of the image in the circular neighborhood, and calculating the average value of the pixels in the circular neighborhood;
and taking the average value of the pixels as the pixel value in the circular neighborhood, and continuously moving the circular neighborhood to correct the pixels of the image.
7. A mass spectrometric detection system for detecting a pesticide residue with a rapid extraction function, which is used for implementing the mass spectrometric detection method for detecting a pesticide residue with a rapid extraction function according to any one of claims 1 to 6, comprising:
the sample extraction module is connected with the central processing module and is used for quantitatively extracting the sample to be detected to obtain a corresponding detection sample;
the solid phase extraction module is connected with the central processing module and is used for processing the sample, and the target compound and impurities are reserved by solid phase extraction; the solid phase extraction module processes a sample, and the specific process of retaining a target compound by solid phase extraction comprises the following steps: removing impurities in the small column and creating a certain solvent environment in the process of extracting a sample to be detected by an extractor; dissolving the sample with a solvent, transferring into a column and retaining the components on the column; removing the interferents to the maximum extent by a leaching mode; eluting the measured substance with small volume of solvent and collecting; the solid phase extraction module processes a sample, and the specific process of solid phase extraction and impurity retention is as follows: in the process of extracting a sample to be detected through an extractor, removing impurities in the column and creating a certain solvent environment; transferring the sample into a column, wherein most of the target compound flows out along with the base solution of the sample, impurities are retained on the column, and the impurities are continuously collected; eluting the components with a small volume of solvent and collecting, and combining the collected solutions;
the sample ionization module is connected with the central processing module and ionizes the sample under the high vacuum condition through an ion source; the ionized molecules are further broken into a plurality of fragment ions with smaller mass and neutral particles due to receiving excessive energy; acquiring average kinetic energy with the same energy under the action of an accelerating electric field and enabling the average kinetic energy to enter a mass analyzer, wherein the mass analyzer separates ions with different masses entering the mass analyzer at the same time according to the mass-to-charge ratio;
the spectrum acquisition module is connected with the central processing module, and is used for respectively introducing the separated ions through the ion detector, acquiring amplified ion signals and drawing a mass spectrum;
the display module is connected with the central processing module and is used for displaying the data in the whole system through a display screen;
and the central processing module is respectively connected with the sample extraction module, the solid-phase extraction module, the sample ionization module, the map acquisition module, the display module, the communication module, the mass spectrometry module, the map processing module, the map storage module and the pesticide residue evaluation module, and coordinates normal operation of the modules.
8. The mass spectrometry detection system for detecting pesticide residue with rapid extraction function according to claim 7, further comprising:
the communication module is connected with the central processing module and realizes information interaction between the central processing module and the cloud service module through the signal transmission equipment;
the cloud service module is connected with the communication module and is used for processing data by utilizing a big data processing technology through a cloud server;
the mass spectrum analysis module is connected with the central processing module, and is used for comparing and analyzing a prestored map and a detected map to judge whether pesticide residues are contained; the mass spectrometry module carries out comparison analysis through a prestored map and a detected map, and the specific process of judging whether pesticide residues are contained is as follows: extracting corresponding features from a pre-stored map and a detected map, and generating a feature descriptor for the extracted features; determining the similarity between the feature descriptors in the two maps, comparing the similarity with a certain threshold value, and judging whether the two maps are similar; when the two maps are similar, judging whether the sample contains pesticide residues or not according to the description of the characteristics in the prestored maps;
the spectrum processing module is connected with the central processing module and is used for processing the acquired mass spectrum through an image processing program; the processing process of the acquired mass spectrogram by the spectrogram processing module comprises the following steps: establishing an image processing set for the acquired mass spectrogram, and carrying out gray processing; after the gray level processing of the image is finished, geometric transformation is carried out; enhancing the image through an image filtering algorithm;
the map storage module is connected with the central processing module and used for storing the map through the storage;
the pesticide residue evaluation module is connected with the central processing module, compares the pesticide residue content with the standard according to the acquired map, and evaluates the grade of the pesticide residue content to determine whether the pesticide residue can be eaten or not; the specific process of the pesticide residue evaluation module comprises the following steps: detecting the content of the residual pesticide, comparing the content with the standard content, and if the content exceeds the standard content, the pesticide cannot be eaten; if the pesticide remains within the standard range, the product can be eaten.
9. A computer program product stored on a computer readable medium, comprising a computer readable program for providing a user input interface to implement the method for mass spectrometric detection of pesticide residue with rapid extraction function of any one of claims 1 to 6 when executed on an electronic device.
10. A computer-readable storage medium storing instructions which, when executed on a computer, cause the computer to execute the mass spectrometric detection method for pesticide residue detection with rapid extraction function according to any one of claims 1 to 6.
CN202110119789.2A 2021-01-28 2021-01-28 Mass spectrum detection system and method with rapid extraction function for detecting pesticide residues Pending CN112924523A (en)

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