CN116930305B - Method and system for detecting pesticide residues in honeysuckle formula particles - Google Patents
Method and system for detecting pesticide residues in honeysuckle formula particles Download PDFInfo
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- 241000205585 Aquilegia canadensis Species 0.000 title claims abstract description 68
- 239000002245 particle Substances 0.000 title claims abstract description 62
- 239000000447 pesticide residue Substances 0.000 title claims abstract description 56
- 238000000034 method Methods 0.000 title claims abstract description 43
- 238000000605 extraction Methods 0.000 claims abstract description 134
- 239000007788 liquid Substances 0.000 claims abstract description 97
- 238000001514 detection method Methods 0.000 claims abstract description 64
- 238000005070 sampling Methods 0.000 claims abstract description 51
- 238000001819 mass spectrum Methods 0.000 claims abstract description 14
- 238000006073 displacement reaction Methods 0.000 claims abstract description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 27
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 238000009472 formulation Methods 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims 1
- 239000000575 pesticide Substances 0.000 abstract description 25
- 238000004458 analytical method Methods 0.000 abstract description 6
- 230000008569 process Effects 0.000 abstract description 4
- 230000000694 effects Effects 0.000 description 13
- 239000000284 extract Substances 0.000 description 11
- 239000011159 matrix material Substances 0.000 description 11
- 239000012535 impurity Substances 0.000 description 9
- 239000008187 granular material Substances 0.000 description 7
- TWFZGCMQGLPBSX-UHFFFAOYSA-N Carbendazim Natural products C1=CC=C2NC(NC(=O)OC)=NC2=C1 TWFZGCMQGLPBSX-UHFFFAOYSA-N 0.000 description 5
- 239000006013 carbendazim Substances 0.000 description 5
- JNPZQRQPIHJYNM-UHFFFAOYSA-N carbendazim Chemical compound C1=C[CH]C2=NC(NC(=O)OC)=NC2=C1 JNPZQRQPIHJYNM-UHFFFAOYSA-N 0.000 description 5
- 238000011084 recovery Methods 0.000 description 5
- 238000000926 separation method Methods 0.000 description 5
- 230000005684 electric field Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 230000000903 blocking effect Effects 0.000 description 2
- 230000003750 conditioning effect Effects 0.000 description 2
- 230000026058 directional locomotion Effects 0.000 description 2
- 238000010494 dissociation reaction Methods 0.000 description 2
- 230000005593 dissociations Effects 0.000 description 2
- 238000005363 electrowinning Methods 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 230000037427 ion transport Effects 0.000 description 2
- 230000005012 migration Effects 0.000 description 2
- 238000013508 migration Methods 0.000 description 2
- 238000004445 quantitative analysis Methods 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 241000238631 Hexapoda Species 0.000 description 1
- 241000607479 Yersinia pestis Species 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000005685 electric field effect Effects 0.000 description 1
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 238000000589 high-performance liquid chromatography-mass spectrometry Methods 0.000 description 1
- 238000000703 high-speed centrifugation Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000017260 vegetative to reproductive phase transition of meristem Effects 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
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Abstract
The invention provides a method and a system for detecting pesticide residues in honeysuckle formula particles, and relates to the technical field of pesticide detection, wherein the method comprises the following steps: extracting the honeysuckle formula particles with preset quality through a sampling module to obtain a detection sample; placing the detection sample in an electric extraction module, and introducing extraction liquid with preset flow to perform electric extraction at preset extraction voltage to obtain liquid to be detected; introducing the liquid to be tested into an ionization module, and introducing the liquid to be tested into an electrospray needle for ionization through an ion source with preset ionization voltage to obtain electrospray; the invention can solve the technical problems of complex analysis and detection procedures, complicated process, long time consumption, complex operation and low efficiency of pesticides in the prior art by adjusting the displacement of the electrospray needle through the adjusting module and aiming the electrospray needle at a mass spectrum sample inlet so that the electrospray enters a mass spectrometer to measure pesticide residues.
Description
Technical Field
The invention relates to the technical field of pesticide detection, in particular to a method and a system for detecting pesticide residues in honeysuckle formula particles.
Background
The honeysuckle formula granule is prepared by adding honeysuckle medicinal materials, and carrying out standard extraction, concentration, drying and granulation, has the effects of clearing heat, detoxicating and dispelling wind and heat, does not need decoction, is convenient to store and is easy to prepare. The honeysuckle flower as a raw material has longer flowering phase and multiple diseases and insect pests in the planting process, and the adsorption capacity of the flower crops on pesticides is strong, so that the problem of pesticide residues on the honeysuckle flower is outstanding.
The pesticides are usually analyzed and detected by pretreatment such as sample crushing, dissolving, high-speed centrifugation, column separation and the like, and then are analyzed by GC-MS or HPLC-MS, so that the process is complex, the time is long, the operation is complex and the efficiency is low.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a method and a system for detecting pesticide residues in honeysuckle formula particles, and aims to solve the technical problems of complex analysis and detection procedures, complex process, long time consumption, complex operation and low efficiency of pesticides in the prior art.
An aspect of the present invention is to provide a method for detecting pesticide residues in honeysuckle flower formulation particles, the method comprising:
extracting the honeysuckle formula particles with preset quality through a sampling module to obtain a detection sample;
placing the detection sample in an electric extraction module, and introducing extraction liquid with preset flow rate to perform electric extraction at preset extraction voltage to obtain liquid to be detected, wherein the preset flow rate is 2-10 mu L/min, and the preset extraction voltage is 1-3 kV;
introducing the liquid to be tested into an ionization module, and introducing the liquid to be tested into an electrospray needle for ionization through an ion source with preset ionization voltage to obtain electrospray;
and the electrospray needle is subjected to displacement adjustment through the adjusting module, and the electrospray needle is aligned to the mass spectrum sample inlet, so that the electrospray enters the mass spectrometer to measure pesticide residues.
Compared with the prior art, the invention has the beneficial effects that: the method for detecting the pesticide residue in the honeysuckle formula particles can be used for carrying out rapid mass spectrum detection, is simple and rapid to operate, reduces pretreatment time, shortens analysis time and is high in efficiency, and specifically, the honeysuckle formula particles are extracted by a sampling module to obtain detection samples; placing the detection sample in an electric extraction module, and introducing extraction liquid with preset flow to perform electric extraction at preset extraction voltage to obtain liquid to be detected; through the direct current electric field generated by preset extraction voltage, charged particles of each molecule in the detection sample generate directional motion in the extraction liquid, and then through selection and proportioning of the extraction liquid, the selectivity is improved, so that the dissociation degree of the molecules in the detection sample is different, and the migration speed of each molecule in the detection sample is different, so that the separation of a matrix and a pesticide is realized, the enrichment effect of the pesticide is achieved, on one hand, the enrichment effect of the pesticide can be effectively improved, and the accuracy and the efficiency of quantitative analysis of a mass spectrometer are improved; on the other hand, the enrichment effect of the pesticide can reduce the contents of the matrix and the impurities, so that the interference of the matrix and the impurities in the detection of a mass spectrometer is reduced, the efficiency and the accuracy of pesticide residues are improved, and the impurity peaks caused by the matrix and the impurities are avoided, so that the detection of the mass spectrometer is influenced; the method comprises the steps of introducing liquid to be detected into an ionization module, introducing the liquid to be detected into an electrospray needle for ionization through an ion source with preset ionization voltage, obtaining electrospray, ionizing the pesticide, further improving analysis accuracy of a mass spectrometer, carrying out displacement adjustment on the electrospray needle through an adjustment module, aiming at a mass spectrum sample inlet, enabling the electrospray to enter the mass spectrometer for measuring pesticide residues, directly connecting an electric extraction module and the ionization module, enabling a detection sample to be electrically extracted to obtain the liquid to be detected, introducing the liquid to be detected into the electrospray needle for ionization, forming electrospray, and then introducing the electrospray into the mass spectrometer for detection, so that direct and rapid detection and analysis of the pesticide residues in honeysuckle formula particles are achieved.
According to an aspect of the above technical solution, the extract comprises methanol, water and acetic acid.
According to one aspect of the above technical solution, in the extract, the volume ratio of methanol, water and acetic acid is (48-50): (49-51): 1.
according to an aspect of the above technical scheme, the preset mass is 5mg-100mg.
According to an aspect of the above technical solution, the preset ionization voltage is 5kV-7kV.
Another aspect of the present invention is to provide a system for detecting pesticide residues in honeysuckle formulation particles, for implementing the method for detecting pesticide residues in honeysuckle formulation particles as described above, the system comprising:
the device comprises a sampling module, an electric extraction module, an ionization module, an adjustment module and a mass spectrometer;
the sampling module is sequentially connected with the electric extraction module, the ionization module and the mass spectrometer, and the other end of the ionization module is connected with the adjusting module;
the sampling module is used for extracting the obtained honeysuckle formula particles with preset quality so as to obtain a detection sample, and comprises a gas-liquid sleeve and a sampling metering tube connected with the gas-liquid sleeve, and the honeysuckle formula particles are extracted to the sampling metering tube through the gas-liquid sleeve;
the electric extraction module is used for carrying out electric extraction on the detection sample to obtain liquid to be detected, and comprises an extraction cavity connected with the sampling quantitative tube and a discharge assembly arranged on the side wall of the extraction cavity, the detection sample is placed in the extraction cavity, and under the preset extraction voltage provided by the discharge assembly, the extraction liquid is introduced into the extraction cavity, and the detection sample is subjected to electric extraction to obtain the liquid to be detected;
the ionization module is used for ionizing the liquid to be tested into an electrospray needle through an ion source with preset ionization voltage to obtain electrospray, and comprises a filter assembly connected with the extraction cavity, the electrospray needle connected with the filter assembly and an external high-voltage assembly connected with the electrospray needle, wherein the liquid to be tested is filtered through the filter assembly, the ion source with preset ionization voltage is introduced into the electrospray needle through the external high-voltage assembly, and the liquid to be tested is introduced into the electrospray needle to be ionized to obtain electrospray;
the adjusting module is used for adjusting the displacement of the electrospray needle, aiming the electrospray at the mass spectrum sample inlet, so that the electrospray enters the mass spectrometer to measure pesticide residues.
According to an aspect of the above solution, the system further comprises an extraction introduction module for delivering an extraction liquid into the extraction chamber.
According to one aspect of the above technical solution, the gas-liquid sleeve is connected with a vacuum adjusting device, and the honeysuckle formula particles are extracted into the sampling metering tube by suction of the vacuum adjusting device.
According to an aspect of the above-described aspect, the mass spectrometer is set to a positive ion detection mode.
Drawings
The foregoing and/or additional aspects and advantages of the invention will become apparent and may be better understood from the following description of embodiments taken in conjunction with the accompanying drawings in which:
FIG. 1 is a flow chart of a method for detecting pesticide residues in honeysuckle flower formula particles in the invention;
FIG. 2 is a schematic diagram of a system for detecting pesticide residues in honeysuckle flower formula particles;
description of the drawings element symbols:
sampling module 10, extraction introduction module 20, electroextraction module 30, ionization module 40, conditioning module 50, mass spectrometer 60.
Detailed Description
In order to make the objects, features and advantages of the present invention more comprehensible, embodiments accompanied with figures are described in detail below. Several embodiments of the invention are presented in the figures. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
It will be understood that when an element is referred to as being "mounted" on another element, it can be directly on the other element or intervening elements may also be present. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present. The terms "vertical," "horizontal," "left," "right," "upper," "lower," and the like are used herein for descriptive purposes only and not to indicate or imply that the apparatus or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore should not be construed as limiting the invention.
In the present invention, unless explicitly stated and limited otherwise, the terms "mounted," "connected," "secured," and the like are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium, and can be communication between two elements. The specific meaning of the above terms in the present invention can be understood by those of ordinary skill in the art according to the specific circumstances. The term "and/or" as used herein includes any and all combinations of one or more of the associated listed items.
Referring to fig. 1, the method for detecting pesticide residues in honeysuckle formula particles provided by the invention comprises the following steps of:
step S10, extracting the honeysuckle formula particles with preset quality through a sampling module to obtain a detection sample;
wherein the preset mass is 5mg-100mg.
Step S11, placing the detection sample in an electric extraction module, and introducing extraction liquid with preset flow rate to perform electric extraction at preset extraction voltage to obtain liquid to be detected, wherein the preset flow rate is 2 mu L/min-10 mu L/min, and the preset extraction voltage is 1kV-3kV;
the method comprises the steps of electrically extracting pesticide residues in a detection sample through a similar compatibility principle of an extraction liquid and an electric field effect of a preset extraction voltage, so as to obtain a liquid to be detected containing pesticide and a small amount of matrixes.
Preferably, the extract comprises methanol, water and acetic acid, and the volume ratio of methanol, water and acetic acid in the extract is (48-50): (49-51): 1, the preset extraction voltage is 1kV-3kV, and according to the field intensity effect and the similar compatibility principle, different preset extraction voltages and the volume ratio of the extraction liquid influence the electric extraction effect and the extraction and separation of pesticides. It should be noted that, through the direct current electric field generated by the preset extraction voltage, the charged particles of each molecule in the detection sample generate directional motion in the extraction liquid, and then through the selection and the proportioning of the extraction liquid, the selectivity is improved, so that the dissociation degree of the molecules in the detection sample is different, and the migration speed of each molecule in the detection sample is different, thereby realizing the separation of the matrix and the pesticide, achieving the enrichment effect of the pesticide, on one hand, the enrichment effect of the pesticide can effectively improve the electric extraction effect of the pesticide, and the accuracy and the efficiency of the quantitative analysis of the mass spectrometer are improved; on the other hand, the enrichment effect of the pesticide can reduce the contents of the matrix and the impurities, so that the interference of the matrix and the impurities in the detection of the mass spectrometer is reduced, the efficiency and the accuracy of pesticide residues are improved, and the impurity peaks caused by the matrix and the impurities are avoided, so that the detection of the mass spectrometer is influenced.
Further, the preset flow is 2-10 mu L/min, and the setting of the preset flow can influence the separation effect of the matrix and the pesticide, so that the electric extraction effect and the electric extraction rate of the pesticide are influenced.
Step S12, introducing the liquid to be tested into an ionization module, and introducing the liquid to be tested into an electrospray needle for ionization by an ion source with preset ionization voltage to obtain electrospray;
the method comprises the steps of carrying out ionization on liquid to be detected in an electrospray needle, generating electrospray by pesticide in the liquid to be detected under the action of a strong electric field with preset ionization voltage, enabling the ionized liquid to be detected to enter a mass spectrometer for detection, and effectively improving the accuracy and efficiency of the mass spectrometer for detection.
Preferably, the preset ionization voltage is 5kV-7kV.
And S13, carrying out displacement adjustment on the electrospray needle through an adjusting module, and aiming the electrospray needle at a mass spectrum sample inlet so that the electrospray enters a mass spectrometer to measure pesticide residues.
The method comprises the steps of adopting an extraction liquid with preset flow and preset extraction voltage to electrically extract a liquid to be detected, then entering an electrospray needle to obtain electrospray, separating pesticide from a matrix in the liquid to be detected, achieving the enrichment effect and ionization of the pesticide, reducing the interference of the matrix and impurities, enabling the ionized liquid to be detected to enter a mass spectrometer, and realizing rapid and accurate mass spectrum detection.
In addition, referring to fig. 2, a system for detecting pesticide residues in honeysuckle flower formula particles is provided, the system comprises:
sampling module 10, electroextraction module 30, ionization module 40, conditioning module 50, mass spectrometer 60;
the sampling module 10 is sequentially connected with the electric extraction module 30, the ionization module 40 and the mass spectrometer 60, and the other end of the ionization module 40 is connected with the adjusting module 50.
The sampling module 10 is used for extracting the obtained honeysuckle formula particles with preset quality so as to obtain a detection sample;
the sampling module 10 includes a gas-liquid sleeve and a sampling metering tube connected with the gas-liquid sleeve, and extracts the honeysuckle prescription granule to the sampling metering tube through the gas-liquid sleeve, so that different sampling metering tubes can be replaced according to the preset quality of the required honeysuckle prescription granule.
Further, the sampling quantitative tube is connected with a vacuum adjusting device, and honeysuckle formula particles are extracted into the sampling quantitative tube through a gas-liquid sleeve by sucking the vacuum adjusting device. Specifically, a diaphragm is arranged in the sampling quantitative tube and is connected with a vacuum adjusting device, and the diaphragm is vacuumized and sucked through the vacuum adjusting device, so that honeysuckle formula particles are extracted into the sampling quantitative tube.
The electric extraction module 30 is used for carrying out electric extraction on the detection sample to obtain a liquid to be detected;
the sampling module 10 is connected to the electric extraction module 30 to electrically extract the detection sample, so as to obtain a liquid to be detected from which pesticides are electrically extracted.
The electric extraction module 30 comprises an extraction cavity connected with the sampling quantitative tube and a discharge assembly arranged on the side wall of the extraction cavity, a detection sample is placed in the extraction cavity, extraction liquid is introduced into the extraction cavity under the preset extraction voltage provided by the discharge assembly, and the detection sample is subjected to electric extraction, so that a liquid to be detected is obtained.
The system further comprises an extraction introduction module 20, the extraction introduction module 20 being adapted to deliver an extraction liquid into the extraction chamber, the extraction introduction module 20 comprising an extraction conduit through which the extraction liquid is pushed into the extraction chamber for electrically extracting the test sample.
The ionization module 40 is configured to ionize the solution to be tested by introducing the solution to be tested into an electrospray needle through an ion source with a preset ionization voltage, so as to obtain electrospray;
the ionization module 40 includes a filter assembly connected with the extraction cavity, an electrospray needle connected with the filter assembly, and an external high-voltage assembly connected with the electrospray needle, and filters the liquid to be tested through the filter assembly to block the larger detection sample of particles from entering the electrospray needle, thereby causing a blocking problem, and the ion source with preset ionization voltage is introduced into the electrospray needle through the external high-voltage assembly, so that the liquid to be tested is introduced into the electrospray needle for ionization, and electrospray is obtained.
The adjustment module 50 is configured to adjust the displacement of the electrospray needle, and direct the electrospray needle toward a mass spectrum sample inlet, so that the electrospray enters the mass spectrometer 60 to determine pesticide residues.
Wherein the adjustment module 50 adjusts the electrospray target mass spectrum sample inlet such that the adjustment module 50 is coupled with the mass spectrometer 60, and the electrospray needle generates electrospray into the mass spectrometer 60 to determine pesticide residues.
Wherein the mass spectrometer 60 is set to a positive ion detection mode, ion source voltage: 6 kV; ion transport tube temperature: 300 ℃; capillary voltage: 10 V, V; lens voltage: 40 V, V; mass scan range: m/z 50-2000; flow Rate: 5. mu L/min.
It should be noted that, the electric extraction module 30 and the ionization module 40 are directly connected, so that the detection sample is electrically extracted to obtain the liquid to be detected, and the liquid to be detected enters the electric spray needle to form electric spray, so that the liquid enters the mass spectrometer 60 for detection, and the direct and rapid detection and analysis of pesticide residues in the honeysuckle formula particles are realized.
The invention is further illustrated by the following examples:
example 1
Referring to fig. 1, a method for detecting pesticide residues in honeysuckle flower granules according to a first embodiment of the present invention is shown, and the method includes steps S10-S13:
step S10, extracting the honeysuckle formula particles with preset quality through a sampling module to obtain a detection sample;
wherein the preset mass is 10mg.
Step S11, placing the detection sample in an electric extraction module, and introducing extraction liquid with preset flow rate to perform electric extraction at preset extraction voltage to obtain liquid to be detected, wherein the preset flow rate is 2 mu L/min-10 mu L/min, and the preset extraction voltage is 1kV-3kV;
wherein the extracting solution comprises methanol, water and acetic acid, and the volume ratio of the methanol to the water to the acetic acid in the extracting solution is 49:50:1.
further, the preset flow rate was 5. Mu.L/min, and the preset extraction voltage was 2kV.
Step S12, introducing the liquid to be tested into an ionization module, and introducing the liquid to be tested into an electrospray needle for ionization by an ion source with preset ionization voltage to obtain electrospray;
wherein, preset ionization voltage is 6kV.
And S13, carrying out displacement adjustment on the electrospray needle through an adjusting module, and aiming the electrospray needle at a mass spectrum sample inlet so that the electrospray enters a mass spectrometer to measure pesticide residues.
Accordingly, the system for detecting pesticide residues in honeysuckle flower formula particles is used for realizing the method, and comprises the following steps:
the device comprises a sampling module, an electric extraction module, an ionization module, an adjustment module and a mass spectrometer;
the sampling module is sequentially connected with the electric extraction module, the ionization module and the mass spectrometer, and the other end of the ionization module is connected with the adjusting module.
The sampling module is used for extracting the obtained honeysuckle formula particles with preset quality so as to obtain a detection sample;
the sampling module comprises a gas-liquid sleeve and a sampling quantitative pipe connected with the gas-liquid sleeve, honeysuckle formula particles are extracted to the sampling quantitative pipe through the gas-liquid sleeve, and different sampling quantitative pipes can be replaced according to the preset quality of the required honeysuckle formula particles.
Further, the sampling quantitative tube is connected with a vacuum adjusting device, and honeysuckle formula particles are extracted into the sampling quantitative tube through a gas-liquid sleeve by sucking the vacuum adjusting device. Specifically, a diaphragm is arranged in the sampling quantitative tube and is connected with a vacuum adjusting device, and the diaphragm is vacuumized and sucked through the vacuum adjusting device, so that honeysuckle formula particles are extracted into the sampling quantitative tube.
The electric extraction module is used for carrying out electric extraction on the detection sample so as to obtain a liquid to be detected;
the sampling module is connected with the electric extraction module so as to electrically extract the detection sample to obtain the liquid to be detected of the pesticide.
The electric extraction module comprises an extraction cavity connected with the sampling quantitative tube and a discharge assembly arranged on the side wall of the extraction cavity, a detection sample is placed in the extraction cavity, extraction liquid is introduced into the extraction cavity under the preset extraction voltage provided by the discharge assembly, and the detection sample is subjected to electric extraction, so that a liquid to be detected is obtained.
The system also includes an extraction introduction module for delivering an extraction fluid into the extraction chamber, the extraction introduction module including an extraction conduit through which the extraction fluid is pushed into the extraction chamber for electrically extracting the test sample.
The ionization module is used for introducing the liquid to be tested into an electrospray needle for ionization through an ion source with preset ionization voltage to obtain electrospray;
the ionization module comprises a filter assembly connected with the extraction cavity, an electrospray needle connected with the filter assembly and an external high-voltage assembly connected with the electrospray needle, wherein the liquid to be detected is filtered through the filter assembly so as to prevent a detection sample with larger particles from entering the electrospray needle and causing a blocking problem, an ion source with preset ionization voltage is introduced into the electrospray needle through the external high-voltage assembly, and the liquid to be detected is introduced into the electrospray needle for ionization, so that electrospray is obtained.
The adjusting module is used for adjusting the displacement of the electrospray needle, aiming the electrospray needle at the mass spectrum sample inlet, so that the electrospray enters the mass spectrometer to measure pesticide residues.
The adjusting module adjusts the electrospray target mass spectrum sample inlet, so that the adjusting module is coupled with the mass spectrometer, and the electrospray needle generates electrospray to enter the mass spectrometer for measuring pesticide residues.
Wherein the mass spectrometer is set to a positive ion detection mode, ion source voltage: 6 kV; ion transport tube temperature: 300 ℃; capillary voltage: 10 V, V; lens voltage: 40 V, V; mass scan range: m/z 50-2000; flow Rate: 5. mu L/min.
Example two
The method for detecting pesticide residue in honeysuckle flower formula particles provided by the second embodiment of the invention is different from the method for detecting pesticide residue in honeysuckle flower formula particles in the first embodiment in that:
the preset flow rate was 10. Mu.L/min.
Example III
The method for detecting pesticide residue in honeysuckle flower formula particles provided by the third embodiment of the invention is different from the method for detecting pesticide residue in honeysuckle flower formula particles in the first embodiment in that:
the preset flow rate was 2. Mu.L/min.
Example IV
The method for detecting pesticide residue in honeysuckle flower formula particles provided by the fourth embodiment of the invention is different from the method for detecting pesticide residue in honeysuckle flower formula particles in the first embodiment in that:
the preset ionization voltage is 5kV.
Example five
The method for detecting pesticide residue in honeysuckle flower formula particles provided by the fifth embodiment of the invention is different from the method for detecting pesticide residue in honeysuckle flower formula particles in the first embodiment in that:
the preset ionization voltage is 7kV.
Example six
The method for detecting pesticide residue in honeysuckle flower formula particles provided by the sixth embodiment of the invention is different from the method for detecting pesticide residue in honeysuckle flower formula particles in the first embodiment in that:
in the extract, the volume ratio of methanol, water and acetic acid is 48:51:1.
example seven
The method for detecting pesticide residue in honeysuckle flower formula particles provided by the seventh embodiment of the invention is different from the method for detecting pesticide residue in honeysuckle flower formula particles in the first embodiment in that:
in the extract, the volume ratio of methanol to water to acetic acid is 50:49:1.
referring to table 1 below, parameters corresponding to the above embodiments of the present invention are shown.
TABLE 1
The honeysuckle flower formulation granule samples used in the above examples one to seven were labeled simulation samples of 20 ug/L.
By combining the data of the first to seventh embodiments, the method for detecting the pesticide residue in the honeysuckle prescription granule can be used for rapidly and effectively detecting the pesticide residue in the honeysuckle prescription granule.
As can be seen from the data of the first to third embodiments, the predetermined flow rate of the extraction liquid will affect the recovery rate of carbendazim, and when the predetermined flow rate is too high or too low relative to the predetermined flow rate of the first embodiment, the recovery rate of carbendazim will be relatively reduced.
As can be seen from the data of the first, fourth and fifth embodiments, the predetermined ionization voltage affects the recovery rate of carbendazim, and when the predetermined ionization voltage is too high or too low relative to the predetermined ionization voltage of the first embodiment, the recovery rate of carbendazim is relatively reduced.
The data of the first, sixth and seventh embodiments show that the ratio of the extract will affect the recovery rate of carbendazim.
In conclusion, by adopting the method for detecting the pesticide residue in the honeysuckle formula particles, the pesticide residue in the honeysuckle formula particles can be rapidly and effectively detected.
In the description of the present specification, a description referring to terms "one embodiment," "some embodiments," "examples," "specific examples," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing examples illustrate only a few embodiments of the invention, and are described in detail, but are not to be construed as limiting the scope of the invention. It should be noted that it is possible for those skilled in the art to make several variations and modifications without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.
Claims (6)
1. A method for detecting pesticide residues in honeysuckle flower formula particles, which is characterized by comprising the following steps:
extracting the honeysuckle formula particles with preset quality through a sampling module to obtain a detection sample, wherein the detection sample comprises the following components:
the sampling module comprises a gas-liquid sleeve and a sampling quantitative pipe connected with the gas-liquid sleeve, and honeysuckle formula particles are extracted to the sampling quantitative pipe through the gas-liquid sleeve;
placing the detection sample in an electric extraction module, and introducing an extraction liquid with preset flow rate to perform electric extraction at preset extraction voltage to obtain a liquid to be detected, wherein the preset flow rate is 5 mu L/min, the preset extraction voltage is 1kV-3kV, and the volume ratio of methanol, water and acetic acid in the extraction liquid is 49:50:1, comprising:
the electric extraction module comprises an extraction cavity connected with the sampling quantitative pipe and a discharge assembly arranged on the side wall of the extraction cavity, the detection sample is placed in the extraction cavity, and under the preset extraction voltage provided by the discharge assembly, an extraction liquid is introduced into the extraction cavity, and the detection sample is subjected to electric extraction to obtain a liquid to be detected;
introducing the liquid to be tested into an ionization module, and introducing the liquid to be tested into an electrospray needle for ionization through an ion source with preset ionization voltage to obtain electrospray, wherein the method comprises the following steps of:
the ionization module comprises a filter assembly connected with the extraction cavity, an electrospray needle connected with the filter assembly and an external high-voltage assembly connected with the electrospray needle, wherein the filter assembly is used for filtering the liquid to be tested, an ion source with preset ionization voltage is introduced into the electrospray needle through the external high-voltage assembly, and the liquid to be tested is introduced into the electrospray needle for ionization, so that electrospray is obtained;
and the electrospray needle is subjected to displacement adjustment through the adjusting module, and the electrospray needle is aligned to the mass spectrum sample inlet, so that the electrospray enters the mass spectrometer to measure pesticide residues.
2. The method for detecting pesticide residues in honeysuckle flower formulated particles according to claim 1, wherein the preset mass is 5mg-100mg.
3. A system for detecting pesticide residues in honeysuckle flower formula particles, for implementing the method for detecting pesticide residues in honeysuckle flower formula particles as claimed in any one of claims 1 to 2, characterized in that the system comprises:
the device comprises a sampling module, an electric extraction module, an ionization module, an adjustment module and a mass spectrometer;
the sampling module is sequentially connected with the electric extraction module, the ionization module and the mass spectrometer, and the other end of the ionization module is connected with the adjusting module;
the sampling module is used for extracting the obtained honeysuckle formula particles with preset quality so as to obtain a detection sample, and comprises a gas-liquid sleeve and a sampling metering tube connected with the gas-liquid sleeve, and the honeysuckle formula particles are extracted to the sampling metering tube through the gas-liquid sleeve;
the electric extraction module is used for carrying out electric extraction on the detection sample to obtain liquid to be detected, and comprises an extraction cavity connected with the sampling quantitative tube and a discharge assembly arranged on the side wall of the extraction cavity, the detection sample is placed in the extraction cavity, and under the preset extraction voltage provided by the discharge assembly, the extraction liquid is introduced into the extraction cavity, and the detection sample is subjected to electric extraction to obtain the liquid to be detected;
the ionization module is used for ionizing the liquid to be tested into an electrospray needle through an ion source with preset ionization voltage to obtain electrospray, and comprises a filter assembly connected with the extraction cavity, the electrospray needle connected with the filter assembly and an external high-voltage assembly connected with the electrospray needle, wherein the liquid to be tested is filtered through the filter assembly, the ion source with preset ionization voltage is introduced into the electrospray needle through the external high-voltage assembly, and the liquid to be tested is introduced into the electrospray needle to be ionized to obtain electrospray;
the adjusting module is used for adjusting the displacement of the electrospray needle, aiming the electrospray at the mass spectrum sample inlet, so that the electrospray enters the mass spectrometer to measure pesticide residues.
4. A system for detecting pesticide residues in honeysuckle flower formulation particles as claimed in claim 3, wherein the system further comprises an extraction introduction module for delivering an extraction liquid into the extraction chamber.
5. The system for detecting pesticide residues in honeysuckle flower formulation particles according to claim 3, wherein the gas-liquid sleeve is connected with a vacuum adjusting device, and the honeysuckle flower formulation particles are extracted into the sampling metering tube by sucking the vacuum adjusting device.
6. A system for detecting pesticide residues in honeysuckle flower formulation particles as claimed in claim 3, wherein the mass spectrometer is set to a positive ion detection mode.
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