CN113720835A - Soil pesticide residue detection method - Google Patents

Soil pesticide residue detection method Download PDF

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Publication number
CN113720835A
CN113720835A CN202111016502.XA CN202111016502A CN113720835A CN 113720835 A CN113720835 A CN 113720835A CN 202111016502 A CN202111016502 A CN 202111016502A CN 113720835 A CN113720835 A CN 113720835A
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soil
sample
detection
reagent
shaking
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CN202111016502.XA
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石晓秋
解焱艳
闫妍
柏中波
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Liaoning General Fair Testing Co ltd
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Liaoning General Fair Testing Co ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • G01N21/78Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour

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  • Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Plasma & Fusion (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)

Abstract

A soil pesticide residue detection method comprises the following detection steps: sampling soil at different depths in different areas, and crushing each soil sample by using a wall breaking machine; taking an electronic balance, weighing the soil sample after the crushing treatment, and then introducing different weighed soil samples into each reaction tube for use; proportioning reagents, vibrating and shaking uniformly, and waiting for use; adding a soil sample, centrifuging, shaking uniformly, standing, filtering, adding a magnesium solution reagent and a color developing agent reagent, covering a sample cover, shaking uniformly and reacting; and starting a pesticide residue detector for detection. Owing to adopt the broken wall machine, can realize carrying out the purpose of broken handle to the soil after the sample, reach the condition of avoiding appearing soil caking influence detection effect, owing to adopt and weigh the sample to soil, can weigh the soil sample of suitable quality portion according to the needs of detecting and specification and detect, reached the purpose that the guarantee detected the precision.

Description

Soil pesticide residue detection method
Technical Field
The invention relates to the technical field of pesticide residues, in particular to a soil pesticide residue detection method.
Background
Pesticide residue is a general term for trace amounts of pesticide protomer, toxic metabolite, degradation product and impurity which are not decomposed and remain in organisms, harvested products, soil pesticide residue soil, water body and atmosphere after the pesticide is used, and at present, strict detection is needed for the condition of pesticide residue to be in compliance.
At present, the detection method that uses now adopts test paper or check out test set to detect mostly, test paper exists detection efficiency low, the drawback that the accuracy is low, be unfavorable for guaranteeing detection effect, some traditional check out test set can't carry out quick contrast and information storage to the testing result mostly, and then lead to the condition of being not convenient for look over the testing result, and the detection method that uses now only singly uses single reactant to detect, reactant reaction effect is poor, can't carry out corresponding multiple reactant to the detection needs and carry out the ratio use, and then bring very big inconvenience for the detection.
Disclosure of Invention
Technical problem to be solved
In view of the above disadvantages and shortcomings of the prior art, the present invention provides a method for detecting pesticide residue in soil, which solves the technical problems of low detection efficiency, poor effect and inconvenient use.
(II) technical scheme
In order to achieve the purpose, the invention adopts the main technical scheme that:
the embodiment of the invention provides a soil pesticide residue detection method, which comprises the following detection steps:
s1 sample preparation
Sampling the soil at different depths in different areas through sampling equipment, and then crushing each sample soil;
s2, sampling
Taking an electronic balance, weighing and sampling the soil crushed in the S1, and then introducing different sampled soil samples into each reaction tube for use;
s3 reagent preparation
Taking 500ml of distilled water to be mixed into buffer solution for standby, then taking 20ml of substrate to be added into 10ml to 20ml of distilled water for standby, taking 10ml of magnesium solution to be mixed into 10ml to 20ml of distilled water for standby, taking 15ml of color developing agent to be mixed into 10ml to 20ml of distilled water, then shaking and shaking the reagents after each proportioning to wait for use;
s4, purifying and extracting sample
Adding 10 ml-20 ml buffer solution into the soil sample in each reaction tube in S2, centrifuging, shaking uniformly, standing, filtering, pouring the extracted upper flushing solution into a sample bottle, adding 100 mu g-200 mu g magnesium solution reagent and color developing agent reagent, covering the sample bottle, shaking uniformly and reacting;
s5, detection
Starting a pesticide residue detector, selecting the detection category of the pesticide residue in the soil, then transferring the sample mixed solution after shaking up reaction into a cuvette, putting the cuvette into a detection channel of the detector, and then covering a machine cover plate for confirmation detection;
s6, displaying and viewing detection result
In the testing process, the sample detection data is transmitted to the database for comparison, the comparison result is displayed in a printing mode, the result is transmitted to the database for storage, and the database is convenient to check and understand in the later period.
Optionally, in the step S3, a shaking instrument is used for shaking up the reagent in the reaction solution.
Optionally, in S4, the centrifugation and shaking of the sample are performed by using a centrifuge, and the sample filtration is performed by using a filter screen.
Alternatively, the reaction time of the sample and the reagent in S4 is 15 minutes, and the reaction temperature is 37 ℃.
Optionally, the buffer solution, the magnesium solution reagent, the color reagent and the base color reagent are quantitatively extracted and added by using a liquid gun.
Optionally, in the step S1, a wall breaking machine is used for the soil crushing treatment.
Optionally, the pesticide residue inhibition rate of less than 50% is qualified
(III) advantageous effects
The invention has the beneficial effects that: compared with the prior art, the soil pesticide residue detection method can realize the purpose of crushing the sampled soil by adopting the wall breaking machine, thereby avoiding the situation that the soil agglomeration affects the detection effect, can weigh and sample the soil by proper mass parts according to the detection requirement and specification for detection by adopting the weighing and sampling for the soil, thereby achieving the purpose of ensuring the detection precision, has more time and labor saving compared with the prior art by adopting the oscillator, can ensure the shaking precision, has high use efficiency and good effect, can ensure the effect of reacting the pesticide residue of the soil sample by adopting the matching among the buffer solution, the magnesium solution reagent, the color reagent and the ground color reagent compared with the prior art, and achieves the improvement of the reaction efficiency, the purpose of guaranteeing the detection accuracy is realized, and compared with the prior art, the database is adopted, so that the comparative analysis of the detection data can be realized, the data can be stored, the purpose of conveniently checking the detection result of each detection by a detection person is achieved, and the completeness of data retention is guaranteed.
Detailed Description
For a better understanding of the present invention, reference will now be made in detail to the present invention by way of specific embodiments thereof.
Example 1:
a soil pesticide residue detection method comprises the following detection steps:
s1 sample preparation
Sampling soil at different depths in different areas through sampling equipment, crushing each sample soil through a wall breaking machine, and crushing the sampled soil through the wall breaking machine, so that the purpose of crushing the sampled soil can be realized, and further the condition that soil agglomeration affects the detection effect is avoided;
s2, sampling
Taking an electronic balance, weighing and sampling the soil crushed in the step S1, introducing different sampled soil samples into each reaction tube for standby use, weighing and sampling the soil, weighing and detecting the soil samples with proper mass parts according to detection requirements and specifications, and ensuring the detection precision;
s3 reagent preparation
500ml of distilled water is taken and added into buffer solution for standby, then 20ml of substrate is taken and 10ml of distilled water is added for standby, 10ml of magnesium solution is taken and 10ml of distilled water is added for standby, 15ml of color developing agent is taken and 10ml of distilled water is added, then reagents after all the proportioning are shaken and shaken uniformly and then are waited for use, reagents of reaction solution are shaken and uniformly shaken by a shaker, and by adopting the shaker, compared with a transmission manual shaking manner, the shaking precision is more time-saving and labor-saving, meanwhile, the shaking precision can be guaranteed, the use efficiency is high, the effect is good, the buffer solution, the magnesium solution reagent, the color developing reagent and a bottom color reagent are quantitatively extracted and added by adopting a liquid gun, and through the matching among the buffer solution, the magnesium solution reagent, the color developing reagent and the bottom color reagent, the effect of reacting pesticide residues in a soil sample can be guaranteed, the reaction efficiency is improved, and the detection accuracy is guaranteed;
s4, purifying and extracting sample
Adding 10ml of buffer solution into soil samples in each reaction tube in S2, centrifuging, shaking uniformly, standing and filtering, wherein the centrifugation, shaking uniformly, of the samples is carried out by adopting a centrifugal machine, the filtering of the samples is carried out by adopting a filter screen, the extracted flushing solution is poured into a sample bottle, then 100 micrograms of magnesium solution reagent and color developing agent reagent are added, the sample is covered, shaking uniformly and reacting are carried out, the reaction time of the samples and the reagents is 15 minutes, the reaction temperature is 37 ℃, the cleanness of the samples can be guaranteed by purifying and extracting the samples, impurities can be clarified to a certain extent by filtering, and the influence on the detection effect is avoided;
s5, detection
Starting a pesticide residue detector, selecting the detection type of the pesticide residue in the soil, setting a detection channel, and detecting various different samples according to the selected type, so that the detection efficiency is improved, transferring the sample mixed solution after shaking up reaction into a cuvette, putting the cuvette into the detection channel of the detector, and then covering a machine cover plate for confirmation detection;
s6, displaying and viewing detection result
In the testing process, transmit sample testing data to the database and contrast, through setting up the database, can reach the contrastive analysis to the testing data, and realize the storage to data, and then make things convenient for the testing personnel to carry out the purpose of looking over to the testing result at every turn, guarantee data is saved integrality, and show the contrast result through the printing mode, it is qualified that pesticide residue inhibition rate < 50%, transmit this time result to the database simultaneously and store, make things convenient for the later stage to look over and know.
Example 2:
a soil pesticide residue detection method comprises the following detection steps:
s1 sample preparation
Sampling soil at different depths in different areas by using sampling equipment, and then breaking each sample soil by using a wall breaking machine;
s2, sampling
Taking an electronic balance, weighing and sampling the soil crushed in the S1, and then introducing different sampled soil samples into each reaction tube for use;
s3 reagent preparation
Taking 500ml of distilled water to be mixed into buffer solution for later use, then taking 20ml of substrate to be added into 15ml of distilled water for later use, taking 10ml of magnesium solution to be mixed into 15ml of distilled water for later use, taking 10ml of color developing agent to be mixed into 15ml of distilled water, then shaking and shaking uniformly the reagents after each proportioning to wait for use, shaking and shaking uniformly the reagents of the reaction solution by adopting a shaking instrument, and quantitatively extracting and adding the buffer solution, the magnesium solution reagent, the color developing reagent and the bottom color reagent by adopting a liquid gun;
s4, purifying and extracting sample
Adding 15ml of buffer solution into the soil sample in each reaction tube in S2, centrifuging, shaking uniformly, standing and filtering, wherein the centrifugation, shaking uniformly, of the sample is performed by using a centrifugal machine, the sample is filtered by using a filter screen, the extracted supernatant is poured into a sample bottle, then 150 mu g of magnesium solution reagent and color developing agent reagent are added, the sample is covered, shaking uniformly and reacting are performed, the reaction time of the sample and the reagents is 15 minutes, and the reaction temperature is 37 ℃;
s5, detection
Starting a pesticide residue detector, selecting the detection category of the pesticide residue in the soil, then transferring the sample mixed solution after shaking up reaction into a cuvette, putting the cuvette into a detection channel of the detector, and then covering a machine cover plate for confirmation detection;
s6, displaying and viewing detection result
In the testing process, the sample testing data is transmitted to the database for comparison, the comparison result is displayed in a printing mode, the pesticide residue inhibition rate is less than 50 percent, and meanwhile, the result is transmitted to the database for storage, so that the later-stage checking and understanding are facilitated.
Example 3:
a soil pesticide residue detection method comprises the following detection steps:
s1 sample preparation
Sampling soil at different depths in different areas by using sampling equipment, and then breaking each sample soil by using a wall breaking machine;
s2, sampling
Taking an electronic balance, weighing and sampling the soil crushed in the S1, and then introducing different sampled soil samples into each reaction tube for use;
s3 reagent preparation
Taking 500ml of distilled water to be mixed into buffer solution for later use, then taking 20ml of substrate to be added into 20ml of distilled water for later use, taking 10ml of magnesium solution to be mixed into 20ml of distilled water for later use, taking 15ml of color developing agent to be mixed into 20ml of distilled water, then shaking and shaking uniformly the reagents after each proportioning to wait for use, shaking and shaking uniformly the reagents of the reaction solution by adopting a shaker, and quantitatively extracting and adding the buffer solution, the magnesium solution reagent, the color developing reagent and the bottom color reagent by adopting a liquid gun;
s4, purifying and extracting sample
Adding 20ml of buffer solution into the soil sample in each reaction tube in S2, centrifuging, shaking uniformly, standing and filtering, wherein the centrifuging, shaking uniformly, filtering the sample by using a filter screen, extracting the supernatant, pouring the supernatant into a sample bottle, adding 200 mu g of magnesium solution reagent and color developing agent reagent, covering the sample bottle, shaking uniformly and reacting, wherein the reaction time of the sample and the reagents is 15 minutes, and the reaction temperature is 37 ℃;
s5, detection
Starting a pesticide residue detector, selecting the detection category of the pesticide residue in the soil, then transferring the sample mixed solution after shaking up reaction into a cuvette, putting the cuvette into a detection channel of the detector, and then covering a machine cover plate for confirmation detection;
s6, displaying and viewing detection result
In the detection process, the sample detection data is transmitted to the database for comparison, the comparison result is displayed in a printing mode, the pesticide residue inhibition rate is less than 50 percent and is qualified, and meanwhile, the result is transmitted to the database for storage, so that the later-stage examination and understanding are facilitated
In the description of the present invention, it is to be understood that the terms "first", "second" and the like are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implying any number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
In the present invention, unless otherwise expressly stated or limited, the terms "mounted," "connected," "secured," and the like are to be construed broadly and can, for example, be fixedly connected, detachably connected, or integrally formed; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium; either as communication within the two elements or as an interactive relationship of the two elements. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
In the present invention, unless otherwise expressly stated or limited, a first feature may be "on" or "under" a second feature, and the first and second features may be in direct contact, or the first and second features may be in indirect contact via an intermediate. Also, a first feature "on," "above," and "over" a second feature may be directly or obliquely above the second feature, or simply mean that the first feature is at a higher level than the second feature. A first feature being "under," "below," and "beneath" a second feature may be directly under or obliquely under the second feature, or may simply mean that the first feature is at a lower level than the second feature.
In the description herein, the description of the terms "one embodiment," "some embodiments," "an embodiment," "an example," "a specific example" or "some examples" or the like, 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 invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
Although embodiments of the present invention have been shown and described above, it should be understood that the above embodiments are illustrative and not restrictive, and that those skilled in the art may make changes, modifications, substitutions and alterations to the above embodiments without departing from the scope of the present invention.

Claims (6)

1. A soil pesticide residue detection method is characterized by comprising the following detection steps:
s1, sampling
Sampling the soil at different depths in different areas through sampling equipment, and crushing each soil sample by adopting a wall breaking machine;
s2 sample preparation
Taking an electronic balance, weighing the soil sample crushed in the step S1, and then introducing different weighed soil samples into each reaction tube for use;
s3 reagent preparation
Taking 500ml of distilled water to be mixed into buffer solution for standby, then taking 20ml of substrate to be added into 10ml to 20ml of distilled water for standby, taking 10ml of magnesium solution to be mixed into 10ml to 20ml of distilled water for standby, taking 15ml of color developing agent to be mixed into 10ml to 20ml of distilled water, then shaking and shaking the reagents after each proportioning to wait for use;
s4, purifying and extracting sample
Adding 10 ml-20 ml buffer solution into the soil sample in each reaction tube in S2, centrifuging, shaking uniformly, standing, filtering, pouring the extracted upper flushing solution into a sample bottle, adding 100 mu g-200 mu g magnesium solution reagent and color developing agent reagent, covering the sample bottle, shaking uniformly and reacting;
s5, detection
Starting a pesticide residue detector, selecting the detection category of the pesticide residue in the soil, then transferring the sample mixed solution after shaking up reaction into a cuvette, putting the cuvette into a detection channel of the detector, and then covering a machine cover plate for confirmation detection;
s6, displaying and viewing detection result
In the testing process, the sample detection data is transmitted to the database for comparison, the comparison result is displayed in a printing mode, the result is transmitted to the database for storage, and the database is convenient to check and understand in the later period.
2. The method for detecting pesticide residues in soil according to claim 1, which is characterized in that: and shaking the reagent of the reaction solution in the step S3 to be uniform by using a shaker.
3. The method for detecting pesticide residues in soil according to claim 1, which is characterized in that: and in the S4, the centrifugal shaking of the sample is performed by adopting a centrifugal machine, and the sample is filtered by adopting a filter screen.
4. The method for detecting pesticide residues in soil according to claim 1, which is characterized in that: the reaction time of the sample and the reagent in the S4 is 15 minutes, and the reaction temperature is 37 ℃.
5. The method for detecting pesticide residues in soil according to claim 1, which is characterized in that: and the buffer solution, the magnesium solution reagent, the color reagent and the bottom color reagent are quantitatively extracted and added by adopting a liquid transfer gun.
6. The method for detecting pesticide residues in soil according to claim 1, which is characterized in that: the pesticide residue inhibition rate is less than 50 percent, and the product is qualified.
CN202111016502.XA 2021-08-31 2021-08-31 Soil pesticide residue detection method Pending CN113720835A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2006333704A (en) * 2005-05-31 2006-12-14 Satake Corp Method for examining residual agrochemical and apparatus therefor
CN102628810A (en) * 2012-04-27 2012-08-08 河南省科学院生物研究所有限责任公司 Method for rapidly and quantitatively detecting organophosphorus pesticide residues in soil
CN105021436A (en) * 2015-07-18 2015-11-04 福建省测试技术研究所 Pesticide extraction liquid and application thereof
CN110487977A (en) * 2019-10-21 2019-11-22 烟台市同翔网络科技有限责任公司 A kind of Practice for Pesticide Residue in Agricultural Products accurate detecting method
CN111257076A (en) * 2020-02-24 2020-06-09 重庆中科检测技术服务有限公司 Pretreatment method for extracting organochlorine pesticide in soil
CN111398259A (en) * 2020-03-24 2020-07-10 中国科学院合肥物质科学研究院 Automatic detection device and detection method for pesticide residues in water body

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2006333704A (en) * 2005-05-31 2006-12-14 Satake Corp Method for examining residual agrochemical and apparatus therefor
CN102628810A (en) * 2012-04-27 2012-08-08 河南省科学院生物研究所有限责任公司 Method for rapidly and quantitatively detecting organophosphorus pesticide residues in soil
CN105021436A (en) * 2015-07-18 2015-11-04 福建省测试技术研究所 Pesticide extraction liquid and application thereof
CN110487977A (en) * 2019-10-21 2019-11-22 烟台市同翔网络科技有限责任公司 A kind of Practice for Pesticide Residue in Agricultural Products accurate detecting method
CN111257076A (en) * 2020-02-24 2020-06-09 重庆中科检测技术服务有限公司 Pretreatment method for extracting organochlorine pesticide in soil
CN111398259A (en) * 2020-03-24 2020-07-10 中国科学院合肥物质科学研究院 Automatic detection device and detection method for pesticide residues in water body

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