CN111220602A - Quick detection device of carbamate pesticide residue - Google Patents
Quick detection device of carbamate pesticide residue Download PDFInfo
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- CN111220602A CN111220602A CN201910952626.5A CN201910952626A CN111220602A CN 111220602 A CN111220602 A CN 111220602A CN 201910952626 A CN201910952626 A CN 201910952626A CN 111220602 A CN111220602 A CN 111220602A
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Abstract
The invention discloses a rapid detection device for carbamate pesticide residues, which comprises a preliminary mixing pool, a color development pool, a waste liquid pool, a sample liquid supply device, a buffer liquid supply device, a first color development agent supply device, a second color development agent supply device, a cleaning liquid supply device, a spectrum testing device, a temperature control module, a valve pump module, a liquid flow control module, a testing module, a display module and a control unit, wherein the preliminary mixing pool is used for mixing the waste liquid pool and the sample liquid pool; the dosage of the sample solution, the buffer solution and the 4-aminoantipyrine solution entering the primary mixing tank is accurately controlled, and carbamate in the sample solution is hydrolyzed under an alkaline environment to generate phenolic compounds; then, the mixed solution enters a color development pool, and a second color development agent enters the color development pool and reacts with the phenolic compound in the mixed solution to generate a red complex; and then, controlling the liquid in the color development pool to enter a spectrum testing device, and testing the pesticide residue in the sample solution. The device is simple to operate, high in detection speed and accurate in detection result.
Description
Technical Field
The invention relates to the technical field of analysis and detection of pesticide residues, in particular to a device for rapidly detecting carbamate pesticide residues.
Background
In the production process of agricultural products, exogenous substances such as pesticides, antibiotics, hormones and the like are widely used at present. The first pesticides used were organochlorine and organophosphorus pesticides, which can kill a large number of pests, but these pesticides have good stability and can exist in the environment for a long time and accumulate in animals, plants and human bodies, and thus are gradually eliminated. The carbamate pesticide which is widely used at present has the advantages of strong selectivity, high efficiency, low toxicity to human and livestock, easy decomposition, less residue and the like, thereby being widely applied. However, researches show that the carbamate pesticide has certain carcinogenic, teratogenic and mutagenic effects, and the carbamate pesticide residue monitoring on agricultural products is particularly important because the carbamate pesticide can affect human health after being contacted with the carbamate pesticide for a long time through diet.
In the existing market, the pesticide residue is rapidly detected by mostly using a kit and a simple pesticide residue rapid detection card through a cholinesterase inhibition method, so that the cost is high, and the detection precision is low; although large-scale instruments such as gas phase or liquid phase chromatography have high accuracy and sensitivity, the instruments are expensive, complex in operation process and long in detection time, and need professional personnel to carry out the detection, so that the requirements of daily food safety and large-scale rapid detection cannot be met.
Therefore, there is an urgent need to develop a carbamate pesticide residue detection device with simple operation, fast detection speed and high accuracy, which can perform on-site fast nondestructive detection on agricultural products and food.
Disclosure of Invention
The invention aims to provide a device for quickly detecting carbamate pesticide residues, which is simple to operate, high in detection speed and accurate in detection result.
In order to achieve the purpose, the invention adopts the following technical scheme:
a rapid detection device for carbamate pesticide residues comprises a preliminary mixing pool, a color development pool, a waste liquid pool, a sample liquid supply device, a buffer liquid supply device, a first color development agent supply device, a second color development agent supply device, a cleaning liquid supply device and a spectrum testing device;
the buffer solution supply device is used for accommodating a buffer solution for providing an alkaline environment in the pesticide residue detection process, the buffer solution is an ammonia-ammonium chloride buffer solution, the first color developing agent supply device is used for accommodating a first color developing agent 4-aminoantipyrine solution, and the second color developing agent supply device is used for accommodating a second color developing agent potassium ferricyanide solution;
the sample liquid supply device, the buffer liquid supply device, the first color developing agent supply device and the cleaning liquid supply device are respectively communicated with an inlet of the preliminary mixing tank through a first pipeline, a second pipeline, a third pipeline and a fourth pipeline, the second color developing agent supply device is communicated with an inlet of the color developing tank through a fifth pipeline, and an electromagnetic flowmeter, a liquid inlet pump and an electromagnetic valve are sequentially arranged on each of the first pipeline to the fifth pipeline;
the outlet of the preliminary mixing tank is communicated with a three-way valve through a sixth pipeline, and the three-way valve is respectively connected with the waste liquid tank and the inlet of the color developing tank through branch pipelines; the outlet of the color developing tank is communicated with a three-way valve through a seventh pipeline, one end of the three-way valve is communicated with the waste liquid tank through a branch pipeline, the other end of the three-way valve is communicated with the inlet of a colorimetric channel in the spectrum testing device through a branch pipeline, the outlet of the colorimetric channel is communicated with the waste liquid tank through an eighth pipeline, and an electromagnetic valve is arranged on the eighth pipeline close to the outlet of the colorimetric channel;
one side of color comparison passageway is provided with the emitter group that is used for sending the laser beam of different wavelengths to the color comparison passageway among the spectrum testing arrangement, the opposite side of color comparison passageway is provided with the detector group that is used for gathering the spectral signal who sees through from the color comparison passageway surface.
In a further technical scheme, the spectrum testing device further comprises a processing unit, an analysis unit and a result display unit, wherein the processing unit is electrically connected with the detector group and is used for receiving the spectrum signals transmitted by the detector and converting the spectrum signals into spectrum images; the analysis unit is electrically connected with the processing unit and is used for processing and comparing the spectral image formed by the processing unit with a standard map image in a system to obtain detection result data; and the result display unit is electrically connected with the analysis unit and is used for receiving and displaying the detection structure data.
Further, the primary mixing pool and the color developing pool are both provided with a temperature sensor and a heating device.
Further technical scheme, quick detection device is still including the PLC controller, the PLC controller includes temperature control module, valve pump module, liquid flow control module, test module, display module and the control unit, open valve pump module and liquid flow control module through the control unit and will await measuring sample solution, buffer solution, first colour developing agent and second colour developing agent are added preliminary mixing pond or colour development pond through corresponding valve ration respectively, open temperature control module through control and keep mixing liquid in preliminary mixing pond and colour development pond to be at the constant temperature, test module changes light signal into the signal of telecommunication, finally present the final result after the department compares through the analysis through display module.
According to the technical scheme, a filter screen is arranged at an inner liquid inlet of the sample liquid supply device, and a honeycomb-shaped filter mechanism coated with an adsorbent on the surface is fixed in the sample liquid supply device.
According to the rapid detection device for the carbamate pesticide residues, the preliminary mixing tank is arranged, the use amounts of the sample solution, the buffer solution and the 4-aminoantipyrine solution entering the preliminary mixing tank are automatically and accurately controlled, the pH of the mixed solution is adjusted to be about 10 by the buffer solution, carbamate in the sample solution is hydrolyzed under an alkaline environment to generate a phenolic compound, and the temperature of the carbamate is controlled within a proper range; then, the mixed solution enters a color development pool, and a potassium ferricyanide solution in a second color development device enters the color development pool and reacts with a phenolic compound in the mixed solution to generate a red complex; and then, controlling a part of liquid in the color development pool to enter a spectrum testing device, testing the pesticide residue in the sample solution, discharging the liquid in the preliminary mixing pool and the color development pool to a waste liquid pool after the test is finished, and cleaning the preliminary mixing pool and the color development pool by a cleaning liquid device.
The device for quickly detecting the carbamate pesticide residue can quickly and accurately detect the pesticide residue on the surface of the agricultural product, judges the pesticide content by comparing the intensity of spectral absorption with a detection model established in equipment, and has the advantages of high detection efficiency, high sensitivity and high measurement precision.
Drawings
The invention is described in further detail below with reference to specific embodiments and with reference to the following drawings.
FIG. 1 is a schematic structural diagram of a rapid detection device according to the present invention;
FIG. 2 is a schematic view showing the structure of a sample liquid supply apparatus according to the present invention;
FIG. 3 is a flowchart illustrating the steps of a method for testing a spectrum testing device according to the present invention;
FIG. 4 is a schematic block diagram of the PLC control system control of the rapid detection device of the present invention;
wherein the specific reference numerals are as follows: the device comprises a cleaning liquid supply device 1, a sample liquid supply device 2, a filter screen 3, a honeycomb-shaped filter mechanism 4, a buffer liquid supply device 5, a first color developing agent supply device 6, a second color developing agent supply device 7, a preliminary mixing pool 8, a color developing pool 9, a spectrum testing device 10, a colorimetric channel 11, an emitter group 12, a detector group 13, a waste liquid pool 14, an electromagnetic flowmeter 15, an electromagnetic valve 16, a liquid inlet pump 17 and a three-way valve 18.
Detailed Description
The reagent preparation method used in the examples of the present invention is as follows:
sample solution: grinding and filtering agricultural products such as vegetables and fruits to be detected, and dissolving 20mL of vegetable and fruit juice in 80mL of water;
ammonia-ammonium chloride buffer at pH 10: weighing 20g of ammonium chloride, dissolving in 100mL of concentrated ammonia water, and storing at 3-5 ℃;
first developer (2 g/L4-aminoantipyrine aqueous solution): sucking 10mL of 20g/L potassium ferricyanide solution, dissolving in water, adding water to dilute to 100mL, and preparing the solution on site;
second developer (8g/L potassium ferricyanide solution): sucking 10mL of 80g/L potassium ferricyanide solution, dissolving in water, adding water to dilute to 100mL, and storing at 3-5 ℃ for one week;
as shown in fig. 1, the present invention provides a device for rapidly detecting carbamate pesticide residues, which comprises a preliminary mixing tank 8, a color development tank 9, a waste liquid tank 14, a sample liquid supply device 2, a buffer liquid supply device 5, a first color developing agent supply device 6, a second color developing agent supply device 7, a cleaning liquid supply device 1 and a spectrum testing device 10. As shown in fig. 2, inlet opening department is provided with filter screen 3 in the appearance liquid feeding device 2 for impurity and particulate matter in to the sample solution carry out prefilter, avoid its influence later stage spectral test, appearance liquid feeding device 2 internal fixation has the honeycomb filter mechanism 4 that coats on the surface and have the adsorbent, adsorbs the pigment in the sample solution, avoids the colour influence test result of sample solution. Temperature sensors and heating devices are arranged in the primary mixing tank 8 and the color development tank 9. A buffer solution supply device 5 for accommodating a buffer solution for providing an alkaline environment in the pesticide residue detection process, the buffer solution being an ammonia-ammonium chloride buffer solution, a first developer supply device 6 for accommodating a first developer 4-aminoantipyrine solution, a second developer supply device 7 for accommodating a second developer potassium ferricyanide solution; the color development mechanism is as follows: the carbamate pesticide is hydrolyzed in an alkaline environment to generate a phenolic compound, the phenolic compound reacts with 4-aminoantipyrine in an environment with the pH value of about 10 and in the presence of potassium ferricyanide to generate red antipyrine dye, the color of the finally generated antipyrine dye shows different changes according to the reaction degree, and the content of the pesticide is judged according to the intensity of spectral absorption.
The sample liquid supply device 2, the buffer liquid supply device 5, the first color developing agent supply device 6 and the cleaning liquid supply device 1 are respectively communicated with an inlet of the primary mixing pool 8 through a first pipeline, a second pipeline, a third pipeline and a fourth pipeline, the second color developing agent supply device 7 is communicated with an inlet of the color developing pool 9 through a fifth pipeline, and an electromagnetic flowmeter 15, a liquid inlet pump 17 and an electromagnetic valve 16 are sequentially arranged on the first pipeline to the fifth pipeline; the outlet of the preliminary mixing tank 8 is communicated with a three-way valve 18 through a sixth pipeline, and the three-way valve 18 is respectively connected with the waste liquid tank 14 and the inlet of the color developing tank 9 through branch pipelines; the outlet of the color developing pool 9 is communicated with a three-way valve 18 through a seventh pipeline, one end of the three-way valve 18 is communicated with the waste liquid pool 14 through a branch pipeline, the other end of the three-way valve 18 is communicated with the inlet of a colorimetric channel 11 in the spectrum testing device 10 through a branch pipeline, the outlet of the colorimetric channel 11 is communicated with the waste liquid pool 14 through an eighth pipeline, and an electromagnetic valve 16 is arranged on the eighth pipeline close to the outlet of the colorimetric channel 11.
As shown in fig. 3, one side of the colorimetric channel 11 in the spectrum testing apparatus 10 is provided with an emitter group 12 for emitting laser beams with different wavelengths to the colorimetric channel 11, the other side of the colorimetric channel 11 is provided with a detector group 13 for collecting spectral signals transmitted from the surface of the colorimetric channel 11, the spectrum testing apparatus 10 further includes a processing unit, an analyzing unit and a result displaying unit, the processing unit is electrically connected with the detector group 13, and is configured to receive the spectral signals transmitted by the detector and convert the spectral signals into spectral images; the analysis unit is electrically connected with the processing unit and is used for processing and comparing the spectral image formed by the processing unit with the standard map image in the system to obtain detection result data; and the result display unit is electrically connected with the analysis unit and is used for receiving and displaying the detection structure data.
As shown in fig. 4, quick detection device is still including the PLC controller, the PLC controller includes temperature control module, the valve pump module, liquid flow control module, test module, display module and the control unit, open valve pump module and liquid flow control module through the control unit and will await measuring sample solution, buffer solution, first developer and second developer add preliminary mixing pond 8 or color development pond 9 through corresponding valve ration respectively, open temperature control module through control and keep mixing liquid in preliminary mixing pond 8 and color development pond 9 to be at the constant temperature, test module changes light signal into the signal of telecommunication, final result after the analysis is compared in the department of presenting through display module.
The method automatically and accurately controls the dosage of the sample solution, the buffer solution and the first color developing agent (4-aminoantipyrine solution) entering the primary mixing tank 8, the pH of the buffer solution is adjusted to be about 10, carbamate in the sample solution is hydrolyzed under an alkaline environment to generate a phenolic compound, and the temperature of the carbamate is controlled within a proper range; then, the mixed solution enters a color development pool 9, and a potassium ferricyanide solution in a second color development device enters the color development pool 9 to react with a phenolic compound in the mixed solution to generate a red complex; then, part of the liquid in the color development pool 9 enters the spectrum testing device 10, pesticide residue in the sample solution is tested, after the test is finished, the liquid in the preliminary mixing pool 8 and the liquid in the color development pool 9 are discharged to the waste liquid pool 14, and the preliminary mixing pool 8 and the color development pool 9 are cleaned through a cleaning liquid device.
The present invention has been described in terms of specific examples, which are provided to aid understanding of the invention and are not intended to be limiting. For a person skilled in the art to which the invention pertains, several simple deductions, modifications or substitutions may be made according to the idea of the invention.
Claims (5)
1. A device for rapidly detecting carbamate pesticide residues is characterized by comprising a preliminary mixing pool, a color development pool, a waste liquid pool, a sample liquid supply device, a buffer liquid supply device, a first color development agent supply device, a second color development agent supply device, a cleaning liquid supply device and a spectrum testing device;
the buffer solution supply device is used for accommodating a buffer solution for providing an alkaline environment in the pesticide residue detection process, the buffer solution is an ammonia-ammonium chloride buffer solution, the first color developing agent supply device is used for accommodating a first color developing agent 4-aminoantipyrine solution, and the second color developing agent supply device is used for accommodating a second color developing agent potassium ferricyanide solution;
the sample liquid supply device, the buffer liquid supply device, the first color developing agent supply device and the cleaning liquid supply device are respectively communicated with an inlet of the preliminary mixing tank through a first pipeline, a second pipeline, a third pipeline and a fourth pipeline, the second color developing agent supply device is communicated with an inlet of the color developing tank through a fifth pipeline, and an electromagnetic flowmeter, a liquid inlet pump and an electromagnetic valve are sequentially arranged on each of the first pipeline to the fifth pipeline;
the outlet of the preliminary mixing tank is communicated with a three-way valve through a sixth pipeline, and the three-way valve is respectively connected with the waste liquid tank and the inlet of the color developing tank through branch pipelines; the outlet of the color developing tank is communicated with a three-way valve through a seventh pipeline, one end of the three-way valve is communicated with the waste liquid tank through a branch pipeline, the other end of the three-way valve is communicated with the inlet of a colorimetric channel in the spectrum testing device through a branch pipeline, the outlet of the colorimetric channel is communicated with the waste liquid tank through an eighth pipeline, and an electromagnetic valve is arranged on the eighth pipeline close to the outlet of the colorimetric channel;
one side of color comparison passageway is provided with the emitter group that is used for sending the laser beam of different wavelengths to the color comparison passageway among the spectrum testing arrangement, the opposite side of color comparison passageway is provided with the detector group that is used for gathering the spectral signal who sees through from the color comparison passageway surface.
2. The device for rapidly detecting the carbamate pesticide residues according to claim 1, wherein the spectrum testing device further comprises a processing unit, an analyzing unit and a result displaying unit, wherein the processing unit is electrically connected with the detector group and is used for receiving the spectrum signals transmitted by the detector and converting the spectrum signals into spectrum images; the analysis unit is electrically connected with the processing unit and is used for processing and comparing the spectral image formed by the processing unit with a standard map image in a system to obtain detection result data; and the result display unit is electrically connected with the analysis unit and is used for receiving and displaying the detection structure data.
3. The device for rapidly detecting carbamate pesticide residues according to claim 1, wherein a temperature sensor and a heating device are arranged in each of the preliminary mixing tank and the color developing tank.
4. The device for rapidly detecting the carbamate pesticide residues according to claim 3, wherein the device further comprises a PLC controller, the PLC controller comprises a temperature control module, a valve pump module, a liquid flow control module, a test module, a display module and a control unit, the valve pump module and the liquid flow control module are started through the control unit, a sample solution to be detected, a buffer solution, a first color developing agent and a second color developing agent are respectively added into the primary mixing pool or the color developing pool through corresponding valve quantification, the temperature control module is started through control to keep the mixed liquid in the primary mixing pool and the color developing pool at a constant temperature, the test module converts an optical signal into an electric signal, and finally the final result after analysis and comparison is displayed through the display module.
5. The device for rapidly detecting carbamate pesticide residues according to claim 1, wherein a filter screen is arranged at an inlet of the sample liquid supply device, and a honeycomb filter mechanism coated with an adsorbent on the surface is fixed in the sample liquid supply device.
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| CN2018114257974 | 2018-11-27 | ||
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Cited By (1)
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Application publication date: 20200602 |