CN110618189A - Analysis method for rapidly detecting dithiocarbamate pesticide residues by adopting ion mobility spectrometry - Google Patents
Analysis method for rapidly detecting dithiocarbamate pesticide residues by adopting ion mobility spectrometry Download PDFInfo
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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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
- G01N1/38—Diluting, dispersing or mixing samples
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- G—PHYSICS
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- 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
- G01N27/622—Ion mobility spectrometry
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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
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2866—Grinding or homogeneising
Abstract
The invention discloses an analysis method for rapidly detecting dithiocarbamate pesticide residues by adopting ion mobility spectrometry, which comprises five analysis objects of thiram, metiram, zineb, mancozeb and a metabolite Ethylene Thiourea (ETU) thereof, and can perform independent qualitative and quantitative analysis on each analysis object for the first time. The method comprises the steps of preparing a standard solution in the first step, developing IMS instrument conditions in the second step, performing field tests in the third step, pretreating a sample in the fourth step, and detecting IMS in the fifth step. The invention has the beneficial effects that: the method adopts pyridine for dissolution for the first time, combines Ion Mobility Spectrometry (IMS) to realize rapid detection after cotton swabs are wiped, directly detects the target without deriving carbon disulfide by an analytical method, has simple and rapid operation, easy mastering and low cost, is suitable for rapid detection of pesticide residues in fruits and vegetables, can accurately distinguish the types of each pesticide, can perform independent qualitative and quantitative analysis on each pesticide, and can be applied to daily monitoring, market detection and the like of the pesticide residues in vegetable bases.
Description
Technical Field
The invention belongs to the field of food safety detection, and particularly relates to an analysis method for rapidly detecting dithiocarbamate pesticide residues by adopting an ion mobility spectrometry.
Background
Ion mobility spectrometry, IMS for short, is a detection technique that has emerged in the end of the 60 s of the 20 th century. The ion mobility spectrometer works under atmospheric environment air pressure without vacuum equipment; the detection range covers the detection fields of gas chromatography and liquid chromatography, high-sensitivity signal response is generated on characteristic spectrums of various organic molecules, and good separation and detection are realized on various molecules which are difficult to degrade in an HPLC (high performance liquid chromatography) in polarity, non-polarity, isomeride, a chromatographic column and the like by using an IMS (ion mobility spectrometry) technology; the substance information contained in the response spectrogram of the organic mixture is rich and complete; the analysis sensitivity to specific target substances can reach pg magnitude; the IMS is simple to operate, and samples can be directly subjected to sample injection detection without pretreatment or only by simple pretreatment; the time of IMS detection and analysis is in the order of minutes, the required sample size is very small, and the consumable materials required by detection and analysis are simple; therefore, the ion mobility spectrometer has the advantages of simple equipment, small volume, light weight, low power consumption, short analysis time, low detection cost and the like, and is multi-component, on-line, accurate and quick analysis equipment.
Dithiocarbamate (DTCs) compounds are useful as enzyme inhibitors because of their strong metal chelating bond, often in the form of heavy metal salts. The bactericidal composition is used as an extremely important bactericide in agricultural production, has the characteristics of high efficiency, low toxicity, safety to people, livestock and plants, broad spectrum prevention and control of plant diseases and the like, and can prevent and control various fungal plant diseases such as epidemic diseases, leaf spot diseases, downy mildew, anthracnose and the like. The medicaments are not easy to induce pathogen resistance and have wide application, and can be divided into dimethyl dithiocarbamate (DMDs for short), ethylene dithiocarbamate (EBDs for short) and propylene dithiocarbamate (PBDs for short) 3 according to the chemical structures. The commonly used DTCs bactericide mainly comprises thiram, ziram, manbam, mancozeb, zineb, propineb and the like. With the widespread use of DTCs, the safety of DTCs is being evaluated. Researches show that the medicaments move fast in soil and easily enter underground water; its metabolites in plants, soil and animals, Ethylene Thiourea (ETU) and Propylene Thiourea (PTU), are also carcinogenic, mutagenic and teratogenic. At present, great attention is paid to the safety of DTCs bactericides at home and abroad, the medicines are particularly reviewed for many times, the use of the medicines is limited, and suggestions and measures for strengthening management are provided. Therefore, it is important to enhance the detection of the residue of DTCs and their metabolites in crops and food. Residue detection has been a challenging issue due to the specific chemical structure of DTCs-based biocides.
The existing analysis methods for dithiocarbamates mainly comprise spectrophotometry, gas chromatography, liquid chromatography-mass spectrometry, capillary electrophoresis and the like. Wherein the acid is hydrolyzed to CS2The method adopts spectrophotometry, gas chromatography-mass spectrometry or flow injection spectrophotometry, or adopts derivatization mode, high performance liquid chromatography-mass spectrometry and other modes for analysis. However, the traditional detection methods have the problems of complex pretreatment, high toxicity, time and labor consumption, insufficient professional personnel, high detection cost and the like, and the detection methods can only carry out large-scale detection to obtain the total, can not determine which pesticide is, can not carry out independent qualitative and quantitative analysis on a single pesticide, can not carry out independent risk assessment on the pesticide, and can not meet the requirements of rapid detection and batch sample detection.
Disclosure of Invention
The invention aims to establish an analysis method for rapidly detecting dithiocarbamate pesticide residues by adopting an ion mobility spectrometry, aims to simply and rapidly detect the dithiocarbamate pesticide residues, can accurately distinguish each pesticide residue and the amount of each pesticide residue, and can be used for daily production basis monitoring, market detection, agricultural product safety supervision and the like.
The technical scheme for solving the technical problems is as follows:
1. an analytical method for rapidly detecting dithiocarbamate pesticide residues by adopting pyridine dissolution and cotton swab wiping combined with Ion Mobility Spectrometry (IMS), which comprises the following steps:
1) respectively preparing standard mother liquor of zineb, metiram, mancozeb, thiram and Ethylene Thiourea (ETU), and diluting the standard mother liquor into standard working solution with different concentrations step by step. The thiocarbamate is a metal complex, and a common solvent for experiments cannot be well dissolved.
2) The standard working solution is detected by IMS-KS-100 type ion mobility spectrometry provided by Wuhan silicon-sensitive technology.
3) And (4) field test. Aiming at the registration information of different medicines on tomatoes and grapes, a test cell is designed according to the pesticide residue test criterion requirement, and the area of the cell is 50m2The cells are randomly arranged, and guard bands are arranged among the cells. And a control cell is arranged.
4) And (4) pretreating a sample. And (3) extracting pesticide residues on the surface of the substrate in a mode of wiping the surface of the substrate with a cotton swab. After soaking the swab stick with acetonitrile, the surface of the substrate was wiped for 1 minute, and the swab was immersed in 2ml of acetonitrile and vortexed for 5 minutes to elute the pesticide.
5) The treated field samples were tested using IMS-KS-100 type ion mobility spectrometry as provided by Wuhan silicon technology.
The invention has the advantages that: the traditional detection method has complex pretreatment, needs to derive target pesticides into carbon disulfide by adopting gas phase and mass spectrum detection, is time-consuming and labor-consuming, has high requirements on professionals, has high detection cost, cannot perform qualitative and quantitative analysis on single pesticides, can only obtain the total residual quantity of large-class dithiocarbamates pesticides, and the like, cannot meet the requirements of rapid detection and batch sample detection, and cannot perform independent risk assessment on single pesticides with different toxicological meanings. The invention adopts pyridine for dissolution for the first time, and combines ion mobility spectrometry to realize rapid detection after cotton swab wiping, and the analytical method has simple operation, rapidness, easy mastering and low cost, is suitable for rapid detection of pesticide residues in fruits and vegetables, can accurately distinguish the types of each pesticide, and can be applied to daily pesticide residue monitoring, market detection and the like in vegetable bases.
Drawings
FIG. 1 is a representative ion mobility spectrometry spectrum of the present invention.
In the figure, the detection targets from left to right are metiram, mancozeb, zineb, thiram and ethylene thiourea.
FIG. 2 is a graph of recovery for the process of the present invention.
In the figure, the recovery rates of the three pesticide addition concentrations of 0.1, 0.5 and 5mg/kg are respectively provided.
Detailed Description
The present invention will be described in further detail with reference to examples. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not limiting.
According to the invention, through indoor tests and field tests, an analysis method for rapidly detecting dithiocarbamate pesticide residues by adopting an Ion Mobility Spectrometry (IMS) is established, compared with the traditional detection method, the analysis method has the advantages of complex pretreatment, high toxicity, time and labor consumption, professional staff deficiency, high detection cost and incapability of meeting the requirements of rapid detection and batch sample detection, the IMS analysis method is simple, rapid and easy to master, is more suitable for rapidly detecting pesticide residues in fruits and vegetables, can accurately distinguish the types of each pesticide, and is applied to market detection and the like.
Example 1
An analytical method for rapidly detecting dithiocarbamate pesticide residues by adopting pyridine dissolution and cotton swab wiping combined with Ion Mobility Spectrometry (IMS), which comprises the following steps:
1. respectively preparing standard mother liquor of zineb, metiram, mancozeb, thiram and Ethylene Thiourea (ETU), and diluting the standard mother liquor into standard working solution with different concentrations step by step.
2. The standard working solution is detected by IMS-KS-100 type ion mobility spectrometry provided by Wuhan silicon-sensitive technology. The apparatus conditions are shown in Table 1, and the reduced ion mobility of each agent is shown in Table 2.
3. And (4) field test. For different drugsRegistering information on tomato and grape, designing test cell with area of 50m according to pesticide residue test criterion2The cells are randomly arranged, and guard bands are arranged among the cells. And a control cell is arranged.
4. And (4) pretreating a sample. And (3) extracting pesticide residues on the surface of the substrate in a mode of wiping the surface of the substrate with a cotton swab. After soaking the swab stick with acetonitrile, the surface of the substrate was wiped for 1 minute, and the swab was immersed in 2ml of acetonitrile and vortexed for 5 minutes to elute the pesticide.
5. The treated field samples were tested using IMS-KS-100 type ion mobility spectrometry provided by Wuhan silicon technology. The sensitivity and substrate recovery of the detection method for dithiocarbamate pesticides and metabolites are shown in Table 3.
Example 2
An analysis method for rapidly detecting 2 dithiocarbamate pesticides and metabolite residues in tomatoes by adopting an Ion Mobility Spectrometry (IMS).
The method takes tomatoes as representatives of vegetables for patent verification, and comprises the following steps:
1. 0.0641g and 0.0650g of zineb and mancozeb standard substances are respectively weighed, pyridine with the volume of 0.2ml is added for dissolution, the solution is placed in a 50ml brown volumetric flask, water is added for constant volume to prepare a standard solution with the volume of 1000mg/kg, and the standard solution with the volume of 0.1, 0.2, 0.5, 1 and 5mg/kg is respectively diluted by ultrapure water. Metabolite ethylenethiourea standard solution: 0.0507g of ETU is weighed, dissolved by methanol, placed in a 50ml brown volumetric flask, and diluted to 1000mg/kg standard solution by water, and then diluted to 0.1, 0.2, 0.5, 1 and 2mg/kg standard solution respectively.
2. The standard working solution is detected by IMS-KS-100 type ion mobility spectrometry provided by Wuhan silicon-sensitive technology. The apparatus conditions are shown in Table 1, and the reduced ion mobility of each agent is shown in Table 2.
3. And step three, performing field test. Aiming at the registration information of dithiocarbamate pesticides on tomato crops, 80% mancozeb wettable powder and 80% mancozeb wettable powder registered on tomatoes are adopted for tests. Designing a test cell according to the pesticide residue test criterion, wherein the area of the cell is 50m2The cells are randomly arranged, and guard bands are arranged among the cells. And a control cell is arranged. The fruits were harvested at 2h, 1d, 3d, 5d, 7d, 10d, 14d, respectively, according to time.
4. And step four, pretreating the sample. The method comprises the steps of extracting pesticide residues on the surface of a substrate in a surface wiping substrate mode, soaking a cotton swab rod with acetonitrile, wiping the surface of the substrate for 1 minute, immersing the cotton swab in 2ml of acetonitrile, and carrying out vortex for 5 minutes to elute the pesticide.
5. And step five, detecting the treated field sample by adopting an IMS-KS-100 type ion mobility spectrometry provided by Wuhan silicon-sensing technology. The sensitivity and substrate recovery of the detection method for dithiocarbamate pesticides and metabolites are shown in Table 3.
By the scheme provided by the invention, the analysis method for rapidly detecting dithiocarbamate pesticide residues by using the IMS is simple to operate, is rapid and easy to master, and is suitable for field detection of pesticide residues.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Example 3
An analysis method for rapidly detecting 4 dithiocarbamate pesticides and metabolite residues in grapes by adopting an Ion Mobility Spectrometry (IMS). The method comprises the following steps:
1. respectively weighing 0.0641g, 0.0606g and 0.0650g of zineb, metiram and mancozeb standard substances, adding 0.2ml of pyridine for dissolving, placing in a 50ml brown volumetric flask, diluting with water to a constant volume to prepare a 1000mg/kg standard solution, and respectively diluting with ultrapure water to obtain 0.1, 0.2, 0.5, 1 and 5mg/kg standard solutions. 0.0502g of thiram standard substance is weighed, diluted by 5ml of acetone and placed in a 50ml brown volumetric flask, the volume is determined by water to prepare 1000mg/kg standard solution, and the standard solution is respectively diluted by water to be 0.1, 0.2, 0.5, 1 and 2mg/kg standard solution. Ethylene thiourea standard solution: 0.0507g of ETU is weighed, dissolved by methanol, placed in a 50ml brown volumetric flask, and diluted to 1000mg/kg standard solution by water, and then diluted to 0.1, 0.2, 0.5, 1 and 2mg/kg standard solution respectively.
2. Step two, the IMS-KS-100 type ion mobility spectrometry provided by Wuhan silicon-sensing technology is adopted to detect the standard working solution. The apparatus conditions are shown in Table 1, and the reduced ion mobility of each agent is shown in Table 2.
3. And (4) field test. Aiming at the registration information of dithiocarbamate pesticides on grape crops, 80 percent of mancozeb wettable powder, 60 percent of metiram water dispersible granules and 50 percent of thiram wettable powder. Designing a test cell according to the pesticide residue test criterion, wherein the area of the cell is 50m2The cells are randomly arranged, and guard bands are arranged among the cells. And a control cell is arranged. The fruits were harvested at 2h, 1d, 3d, 5d, 7d, 10d, 14d, respectively, according to time.
4. And (4) pretreating a sample. The method comprises the steps of extracting pesticide residues on the surface of a substrate in a surface wiping substrate mode, soaking a cotton swab rod with acetonitrile, wiping the surface of the substrate for 1 minute, immersing the cotton swab in 2ml of acetonitrile, and carrying out vortex for 5 minutes to elute the pesticide.
5. The treated field samples were tested using IMS-KS-100 type ion mobility spectrometry provided by Wuhan silicon technology. The sensitivity and substrate recovery of the detection method for dithiocarbamate pesticides and metabolites are shown in Table 3.
By the scheme provided by the invention, the analysis method for rapidly detecting dithiocarbamate pesticide residues by using the IMS is simple to operate, is rapid and easy to master, and is suitable for field detection of pesticide residues.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Table 1 IMS instrument conditions
TABLE 2 reduced ion mobility of dithiocarbamate pesticides and metabolites
TABLE 3 Process sensitivity and substrate recovery for dithiocarbamate pesticides and metabolites
Claims (3)
1. An analytical method for rapidly detecting dithiocarbamate pesticide residues by adopting ion mobility spectrometry comprises the following steps:
1) respectively preparing standard mother liquor of zineb, metiram, mancozeb, thiram and Ethylene Thiourea (ETU), and diluting the standard mother liquor into standard working solutions with different concentrations step by step; the thiocarbamate is a metal complex, and a common solvent for experiments cannot be well dissolved;
2) detecting the standard working solution by IMS-KS-100 type ion mobility spectrometry provided by Wuhan silicon-sensitive technology to obtain qualitative and quantitative information of each pesticide;
3) and (3) field test: aiming at the registration information of different medicines on tomatoes and grapes, a test cell is designed according to the pesticide residue test criterion requirement for field pesticide application and sampling, a cell sample is obtained for method development and confirmation, and the area of the cell is 50m2Setting a guard band between cells and setting a contrast cell;
4) sample pretreatment: extracting pesticide residues on the surface of the substrate in a mode of wiping the surface of the substrate with a cotton swab; soaking a cotton swab rod with acetonitrile, wiping the surface of the substrate for 1 minute, immersing the cotton swab into 2ml of acetonitrile, and carrying out vortex for 5 minutes to elute the pesticide;
5) the treated field samples were tested using IMS-KS-100 type ion mobility spectrometry provided by Wuhan silicon technology.
2. An analysis method for rapidly detecting 2 dithiocarbamate pesticides and metabolite residues in tomatoes by adopting ion mobility spectrometry is disclosed, and the method carries out patent implementation verification by taking tomatoes as representatives of vegetables, and comprises the following steps:
1) weighing 0.0641g and 0.0650g of zineb and mancozeb standard substances respectively, adding pyridine with the volume of 0.2ml for dissolution, placing the solution in a 50ml brown volumetric flask, adding water to a constant volume to prepare a standard solution of 1000mg/kg, and diluting the solution with ultrapure water into standard solutions of 0.1, 0.2, 0.5, 1 and 5mg/kg and a metabolite ethylene thiourea standard solution respectively: weighing 0.0507g ETU, dissolving with methanol, placing in a 50ml brown volumetric flask, diluting with water to constant volume to prepare 1000mg/kg standard solution, and diluting with water to obtain 0.1, 0.2, 0.5, 1, 2mg/kg standard solution respectively;
2) detecting the standard working solution by IMS-KS-100 type ion mobility spectrometry provided by Wuhan silicon-sensitive technology;
3) and (3) field test: aiming at the registration information of dithiocarbamate pesticides on tomato crops, 80 percent mancozeb wettable powder and 80 percent mancozeb wettable powder registered on tomatoes are adopted for tests, test cells are designed according to the requirements of pesticide residue test criteria, and the area of each cell is 50m2Randomly arranging, arranging a protective band among cells, arranging a contrast cell, and collecting fruits at 2h, 1d, 3d, 5d, 7d, 10d and 14d according to time;
4) sample pretreatment: extracting pesticide residues on the surface of the substrate by wiping the substrate on the surface, soaking a cotton swab rod with acetonitrile, wiping the surface of the substrate for 1 minute, immersing the cotton swab rod in 2ml of acetonitrile, and carrying out vortex elution for 5 minutes to elute the pesticide;
5) the treated field samples were tested using IMS-KS-100 type ion mobility spectrometry provided by Wuhan silicon technology.
3. An analytical method for rapidly detecting residues of 4 dithiocarbamate pesticides and metabolites thereof in grapes by adopting ion mobility spectrometry comprises the following steps:
1) weighing 0.0641g, 0.0606g and 0.0650g of zineb, metiram and mancozeb standard substances respectively, adding pyridine with the volume of 0.2ml for dissolving, placing in a 50ml brown volumetric flask, using water to fix the volume to prepare a 1000mg/kg standard solution, then using ultrapure water to respectively dilute the solution into 0.1, 0.2, 0.5, 1 and 5mg/kg standard solution, weighing 0.0502g of thiram standard substance, using 5ml of acetone for diluting, placing in a 50ml brown volumetric flask, using water to fix the volume to prepare a 1000mg/kg standard solution, using water to respectively dilute the solution into 0.1, 0.2, 0.5, 1 and 2mg/kg standard solution and ethylene thiourea standard solution: weighing 0.0507g ETU, dissolving with methanol, placing in a 50ml brown volumetric flask, diluting with water to constant volume to prepare 1000mg/kg standard solution, and diluting with water to obtain 0.1, 0.2, 0.5, 1, 2mg/kg standard solution respectively;
2) detecting the standard working solution by IMS-KS-100 type ion mobility spectrometry provided by Wuhan silicon-sensitive technology;
3) and (3) field test: aiming at the registration information of dithiocarbamate pesticides on grape crops, 80 percent mancozeb wettable powder, 60 percent metiram water dispersible granule and 50 percent thiram wettable powder, a test cell is designed according to the requirements of pesticide residue test criteria, and the area of the cell is 50m2Randomly arranging, arranging a protective band among cells, arranging a contrast cell, and collecting fruits at 2h, 1d, 3d, 5d, 7d, 10d and 14d according to time;
4) sample pretreatment: extracting pesticide residues on the surface of the substrate by wiping the substrate on the surface, soaking a cotton swab rod with acetonitrile, wiping the surface of the substrate for 1 minute, immersing the cotton swab rod in 2ml of acetonitrile, and carrying out vortex elution for 5 minutes to elute the pesticide;
5) the treated field samples were tested using IMS-KS-100 type ion mobility spectrometry provided by Wuhan silicon technology.
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| CN114031531A (en) * | 2021-11-27 | 2022-02-11 | 山东省烟台市农业科学研究院 | Derivatization method of dithiocarbamate compound |
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