CN113514302A - Efficient pretreatment method for pesticide residue detection sample - Google Patents
Efficient pretreatment method for pesticide residue detection sample Download PDFInfo
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- CN113514302A CN113514302A CN202110789372.7A CN202110789372A CN113514302A CN 113514302 A CN113514302 A CN 113514302A CN 202110789372 A CN202110789372 A CN 202110789372A CN 113514302 A CN113514302 A CN 113514302A
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Abstract
The invention discloses a high-efficiency pretreatment method of a pesticide residue detection sample, which comprises the following steps: taking an edible part of a to-be-detected farm and vegetable product, crushing, uniformly mixing and sealing the edible part by a crusher, placing the edible part into a sealing bag as a sample into a refrigeration drying box, placing the sample into a 100ml centrifuge tube at the refrigeration temperature of 0-20 ℃, weighing a proper amount of the sample, placing the sample into the 100ml centrifuge tube, adding 30-50 ml of water, placing the centrifuge tube on a vortex oscillator, uniformly mixing the sample by vortex for 1-2 min, taking supernatant, filtering out floating substances to obtain solution A, adding 2-5 ml of salt solution or acetic acid into the solution A, uniformly stirring, then adding 1-10 ml of acetonitrile, horizontally oscillating for 10-20 min, precipitating protein in the sample to the bottom end of the centrifuge tube, pouring the supernatant into another 100ml centrifuge tube, and obtaining solution B; the precipitated liquid was recovered by filtration. The beneficial effects are that: compared with the prior art, the method has the advantages of simple operation, good sensitivity, convenient recovery of extracted substances, environmental protection and no addition of harmful substances which generate body harm to detection personnel in the extraction process.
Description
Technical Field
The invention belongs to the technical field of pesticide residue detection, and particularly relates to an efficient pretreatment method of a pesticide residue detection sample.
Background
The pesticide residue detection generally comprises 2 parts of sample pretreatment and instrument analysis, wherein the sample pretreatment integrates comprehensive technologies such as extraction, purification, concentration and the like, and can furthest extract and enrich a target detection object and simultaneously furthest remove matrix interference components, thereby ensuring the accuracy of the instrument analysis detection.
At present, traditional pretreatment methods for detecting and analyzing pesticide residues comprise a Soxhlet extraction method, a liquid-liquid extraction method, a sulfonation method, an accelerated solvent extraction method, an ultrasonic extraction method, a microwave-assisted extraction method and the like, but the traditional methods generally have the defects of long extraction time, large organic solvent consumption, complex treatment process of an extracting solution, low sensitivity, environmental pollution, physical harm to detection personnel and the like, so that an efficient pretreatment method for a pesticide residue detection sample is provided.
Disclosure of Invention
The invention aims to provide an efficient pretreatment method of a pesticide residue detection sample, so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: an efficient pretreatment method of a pesticide residue detection sample comprises the following steps:
s1, taking the edible part of the to-be-tested agricultural and vegetable product, crushing, uniformly mixing and sealing the edible part by using a crusher, putting the crushed mixture into a sealing bag as a sample, and putting the sample into a refrigeration drying box, wherein the refrigeration temperature is 0-20 ℃;
s2, weighing a proper amount of sample, placing the sample into a 100ml centrifuge tube, adding 30 ml-50 ml of water, placing the centrifuge tube on a vortex oscillator, uniformly mixing by vortex for 1 min-2 min, taking supernatant, and filtering floating substances to obtain solution A;
s3, adding 2-5 ml of salt solution or acetic acid into the solution A, uniformly stirring, then adding 1-10 ml of acetonitrile, horizontally oscillating for 10-20 min, precipitating protein in a sample to the bottom end of a centrifuge tube, and pouring the supernatant into another 100ml centrifuge tube to obtain solution B; filtering and recovering the precipitated liquid;
s4, adding 1g to 3g of black Carb powder and 0.5g to 1g of activated carbon powder into the separated liquid B, swirling for 0.5min to 1min, mixing uniformly, taking supernatant, and filtering with a filter membrane to obtain filtrate to be detected.
Preferably, the sample in the step S2 has 10 g to 20 g, and the rotation speed of the vortex is 2000 rpm to 3000 rpm.
Preferably, the floating material in S2 is fat, and the size of the pores of the filter membrane used for filtration is 2um to 3 um.
Preferably, the object for stirring in S3 is a stirring device, and the object for horizontal oscillation in S3 is a horizontal oscillator.
Preferably, the rotation speed of the vortex in the S4 is 3000-5000 r, and the concentration of the ethanol is 80-95%.
Preferably, the salt solution has a concentration of 0.15 to 0.3 molar.
Preferably, the black Carb powder has a particle size of 10-30 um, and the activated carbon powder has a particle size of 5-20 um.
Compared with the prior art, the invention has the beneficial effects that: compared with the prior art, the method has the advantages of simple operation, good sensitivity, convenient recovery of extracted substances, environmental protection and no addition of harmful substances which generate body harm to detection personnel in the extraction process.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a technical scheme that: an efficient pretreatment method of a pesticide residue detection sample comprises the following steps:
s1, taking the edible part of the to-be-tested agricultural and vegetable product, crushing, uniformly mixing and sealing the edible part by using a crusher, putting the crushed mixture into a sealing bag as a sample, and putting the sample into a refrigeration drying box, wherein the refrigeration temperature is 0-20 ℃;
s2, weighing a proper amount of sample, placing the sample into a 100ml centrifuge tube, adding 30 ml-50 ml of water, placing the centrifuge tube on a vortex oscillator, uniformly mixing by vortex for 1 min-2 min, taking supernatant, and filtering floating substances to obtain solution A;
s3, adding 2-5 ml of salt solution or acetic acid into the solution A, uniformly stirring, then adding 1-10 ml of acetonitrile, horizontally oscillating for 10-20 min, precipitating protein in a sample to the bottom end of a centrifuge tube, and pouring the supernatant into another 100ml centrifuge tube to obtain solution B; filtering and recovering the precipitated liquid;
s4, adding 1g to 3g of black Carb powder and 0.5g to 1g of activated carbon powder into the separated liquid B, swirling for 0.5min to 1min, mixing uniformly, taking supernatant, and filtering with a filter membrane to obtain filtrate to be detected.
Specifically, the sample in the step S2 is 10 g to 20 g, the rotation speed of the vortex is 2000 rpm to 3000 rpm, the floating matter in S2 is fat, the size of the die hole of the filter membrane for filtering is 2um to 3um, the article for stirring in S3 is a stirring device, the article for horizontal oscillation in S3 is a horizontal oscillator, the rotation speed of the vortex in S4 is 3000 rpm to 5000 rpm, the concentration of ethanol is 80% to 95%, the concentration of the salt solution is 0.15 mol to 0.3 mol, black Carb powder, the particle size is 10um to 30um, and the particle size of the activated carbon powder is 5um to 20 um.
Example 1
An efficient pretreatment method of a pesticide residue detection sample comprises the following steps:
s1, crushing, uniformly mixing and sealing the bean curd floss in a sealing bag by using a crusher to obtain a sample, and placing the sample in a refrigeration drying box at the refrigeration temperature of 0-20 ℃;
s2, weighing 10 g of crushed bean and vegetable samples, placing the bean and vegetable samples into a 100ml centrifugal tube, adding 50ml of water, placing the centrifugal tube on a vortex oscillator, vortex for 1min at the vortex rotation speed of 2000 rpm, mixing uniformly, taking supernatant to obtain solution A, and filtering liquid contained in floaters in the supernatant by using a 3um filter membrane;
s3, adding 5ml of 0.3 molar salt solution into the solution A, uniformly stirring, then adding 1ml of acetonitrile, horizontally oscillating for 20min, precipitating protein in a sample to the bottom end of a centrifuge tube, and pouring the supernatant into another 100ml centrifuge tube to obtain solution B; filtering and recovering the precipitated liquid;
s4, adding 3ml of 80% ethanol 1g of black Carb powder and 0.5g of activated carbon powder into the separated liquid B, uniformly mixing at a vortex rotation speed of 3000 r/min for 0.5min, and filtering the supernatant with a filter membrane to obtain a filtrate to be detected;
and S5, placing the filtrate to be detected into a pesticide residue detector for detection, so that the pesticide residue in the sample can be judged.
According to the example, the results of the measurement showed that when water, a 0.3 molar salt solution and 80% ethanol were added to a fruit and vegetable sample to be measured, the recovery rate of protein, fat and pigment in the sample was 97% and the RSD value was 3%.
Has the advantages that: the method is convenient for recovering and extracting the protein and fat in the sample, the operation is simpler and more environment-friendly, and the efficiency of extracting the pigment is better.
Example 2
An efficient pretreatment method of a pesticide residue detection sample comprises the following steps:
s1, smashing, uniformly mixing and sealing the green vegetables by a smashing machine, putting the mixture into a sealing bag as a sample, and putting the sample into a refrigeration drying box, wherein the refrigeration temperature is 0-20 ℃;
s2, weighing 20 g of crushed bean and vegetable samples, placing the bean and vegetable samples into a 100ml centrifugal tube, adding 30ml of water, placing the centrifugal tube on a vortex oscillator, vortex for 2min at the vortex rotation speed of 3000 rpm, mixing uniformly, taking supernate to obtain solution A, and filtering liquid contained in floaters in the supernate by using a 2um filter membrane;
s3, adding 2ml of 0.15 mol salt solution into the solution A, uniformly stirring, then adding 2ml of acetonitrile, horizontally oscillating for 10min, precipitating protein in a sample to the bottom end of a centrifuge tube, and pouring the supernatant into another 100ml centrifuge tube to obtain solution B; filtering and recovering the precipitated liquid;
s4, adding 6ml of 95% ethanol 3g of black Carb powder and 1g of activated carbon powder into the separated liquid B, uniformly mixing at a vortex rotation speed of 5000 r/min for 1min, and filtering the supernatant with a filter membrane to obtain a filtrate to be detected;
and S5, placing the filtrate to be detected into a pesticide residue detector for detection, so that the pesticide residue in the sample can be judged.
According to the example, the results of the measurement showed that when water, a 0.15 molar salt solution and 95% ethanol were added to a fruit and vegetable sample to be tested, the recovery rate of protein, fat and pigment in the sample was 80.5% and the RSD value was 19.5%.
Has the advantages that: the recovery rate of protein and fat in the sample is convenient to recover and extract is good, the operation is simple and environment-friendly, and the efficiency of extracting the pigment is optimal.
Example 3
An efficient pretreatment method of a pesticide residue detection sample comprises the following steps:
s1, crushing, uniformly mixing and sealing fruits by using a crusher, putting the crushed fruits into a sealing bag as a sample, and putting the sample into a refrigeration drying box, wherein the refrigeration temperature is 0-20 ℃;
s2, weighing 15 g of fruit sample, placing the fruit sample into a 100ml centrifugal tube, adding 40ml of water, placing the centrifugal tube on a vortex oscillator, uniformly mixing the fruit sample and the water at the vortex rotation speed of 2500 rpm for 1.5min by vortex, taking supernatant to obtain solution A, and filtering liquid contained in the floating substances in the supernatant by using a 2.5um filter membrane;
s3, adding 2ml of acetic acid solution into the solution A, uniformly stirring, then adding 10ml of acetonitrile, horizontally oscillating for 15min, precipitating organic acid in a sample to the bottom end of a centrifugal tube, and pouring the supernatant into another 100ml centrifugal tube to obtain solution B; filtering and recovering the precipitated liquid;
s4, adding 4.5ml of 95% ethanol into the separated liquid B, uniformly mixing by swirling for 0.5-1 min, and filtering the supernate with a filter membrane to obtain a filtrate to be detected.
According to the embodiment, the determination result shows that the recovery rate of the organic acid and the pigment in the sample is 98.5 percent and the RSD value is 1.5 percent when water, acetic acid and 95 percent ethanol are added into the fruit and vegetable sample to be tested.
Has the advantages that: the method is convenient for recovering and extracting the organic acid in the sample, has optimal extraction effect, is simple and environment-friendly to operate without harmful substances, and has optimal pigment extraction efficiency.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (7)
1. An efficient pretreatment method of a pesticide residue detection sample comprises the following steps:
s1, taking the edible part of the to-be-tested agricultural and vegetable product, crushing, uniformly mixing and sealing the edible part by using a crusher, putting the crushed mixture into a sealing bag as a sample, and putting the sample into a refrigeration drying box, wherein the refrigeration temperature is 0-20 ℃;
s2, weighing a proper amount of sample, placing the sample into a 100ml centrifuge tube, adding 30 ml-50 ml of water, placing the centrifuge tube on a vortex oscillator, uniformly mixing by vortex for 1 min-2 min, taking supernatant, and filtering floating substances to obtain solution A;
s3, adding 2-5 ml of salt solution or acetic acid into the solution A, uniformly stirring, then adding 1-10 ml of acetonitrile, horizontally oscillating for 10-20 min, precipitating protein in a sample to the bottom end of a centrifuge tube, and pouring the supernatant into another 100ml centrifuge tube to obtain solution B; filtering and recovering the precipitated liquid;
s4, adding 1g to 3g of black Carb powder and 0.5g to 1g of activated carbon powder into the separated liquid B, swirling for 0.5min to 1min, mixing uniformly, taking supernatant, and filtering with a filter membrane to obtain filtrate to be detected.
2. The method for pretreating a sample for efficiently detecting pesticide residues as claimed in claim 1, wherein the method comprises the following steps: the sample in the step S2 is 10-20 g, and the rotation speed of the vortex is 2000-3000 r/min.
3. The method for pretreating a sample for efficiently detecting pesticide residues as claimed in claim 1, wherein the method comprises the following steps: the floater in S2 is fat, and the size of the filter membrane for filtering is 2 um-3 um.
4. The method for pretreating a sample for efficiently detecting pesticide residues as claimed in claim 1, wherein the method comprises the following steps: the material for stirring in S3 is a stirring device, and the material for horizontal oscillation in S3 is a horizontal oscillator.
5. The method for pretreating a sample for efficiently detecting pesticide residues as claimed in claim 1, wherein the method comprises the following steps: the rotation speed of the vortex in the S4 is 3000-5000 r, and the concentration of the ethanol is 80-95%.
6. The method for pretreating a sample for efficiently detecting pesticide residues as claimed in claim 1, wherein the method comprises the following steps: the concentration of the salt solution is 0.15 mol to 0.3 mol.
7. The method for pretreating a sample for efficiently detecting pesticide residues as claimed in claim 1, wherein the method comprises the following steps: the particle size of the black Carb powder is 10 um-30 um, and the particle size of the activated carbon powder is 5 um-20 um.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2016151947A1 (en) * | 2015-03-24 | 2016-09-29 | 三浦工業株式会社 | Method for preparing sample for residual pesticide analysis |
| CN107543888A (en) * | 2017-10-19 | 2018-01-05 | 伊犁师范学院 | A kind of method of sample pre-treatments during garden stuff pesticide residue detection |
| WO2018043465A1 (en) * | 2016-08-30 | 2018-03-08 | 三浦工業株式会社 | Method for preparing sample for analyzing residual agricultural chemical |
| CN108693003A (en) * | 2018-04-26 | 2018-10-23 | 许昌学院 | A kind of method of leafy vegetable Detecting Pesticide sample pre-treatments |
| CN109283280A (en) * | 2018-11-28 | 2019-01-29 | 广西壮族自治区农业科学院农产品质量安全与检测技术研究所 | A method of rapidly extracting purifies benzoyl urea pesticide residue from water fruits and vegetables |
| CN109725086A (en) * | 2019-03-13 | 2019-05-07 | 盐城市农产品质量监督检验测试中心 | It is a kind of to introduce the residual quick pretreatment method of broken wall treatment detection pesticide residues in vegetables |
-
2021
- 2021-07-13 CN CN202110789372.7A patent/CN113514302A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2016151947A1 (en) * | 2015-03-24 | 2016-09-29 | 三浦工業株式会社 | Method for preparing sample for residual pesticide analysis |
| WO2018043465A1 (en) * | 2016-08-30 | 2018-03-08 | 三浦工業株式会社 | Method for preparing sample for analyzing residual agricultural chemical |
| CN107543888A (en) * | 2017-10-19 | 2018-01-05 | 伊犁师范学院 | A kind of method of sample pre-treatments during garden stuff pesticide residue detection |
| CN108693003A (en) * | 2018-04-26 | 2018-10-23 | 许昌学院 | A kind of method of leafy vegetable Detecting Pesticide sample pre-treatments |
| CN109283280A (en) * | 2018-11-28 | 2019-01-29 | 广西壮族自治区农业科学院农产品质量安全与检测技术研究所 | A method of rapidly extracting purifies benzoyl urea pesticide residue from water fruits and vegetables |
| CN109725086A (en) * | 2019-03-13 | 2019-05-07 | 盐城市农产品质量监督检验测试中心 | It is a kind of to introduce the residual quick pretreatment method of broken wall treatment detection pesticide residues in vegetables |
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