CN108444946A - A kind of Practice for Pesticide Residue in Agricultural Products detection method and device - Google Patents
A kind of Practice for Pesticide Residue in Agricultural Products detection method and device Download PDFInfo
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- CN108444946A CN108444946A CN201810443765.0A CN201810443765A CN108444946A CN 108444946 A CN108444946 A CN 108444946A CN 201810443765 A CN201810443765 A CN 201810443765A CN 108444946 A CN108444946 A CN 108444946A
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- 238000001514 detection method Methods 0.000 title claims abstract description 110
- 239000000447 pesticide residue Substances 0.000 title claims abstract description 33
- 239000000575 pesticide Substances 0.000 claims abstract description 58
- 238000001228 spectrum Methods 0.000 claims abstract description 35
- 239000007788 liquid Substances 0.000 claims abstract description 27
- 238000002235 transmission spectroscopy Methods 0.000 claims abstract description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000004615 ingredient Substances 0.000 claims abstract description 15
- 239000000126 substance Substances 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 14
- 238000004611 spectroscopical analysis Methods 0.000 claims abstract description 12
- 230000001476 alcoholic effect Effects 0.000 claims abstract description 6
- 239000000047 product Substances 0.000 claims description 54
- 239000012153 distilled water Substances 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 238000012360 testing method Methods 0.000 claims description 19
- 230000001105 regulatory effect Effects 0.000 claims description 17
- 239000000243 solution Substances 0.000 claims description 15
- 238000003860 storage Methods 0.000 claims description 14
- 230000007246 mechanism Effects 0.000 claims description 13
- 230000006835 compression Effects 0.000 claims description 12
- 238000007906 compression Methods 0.000 claims description 12
- 239000000706 filtrate Substances 0.000 claims description 12
- 150000003839 salts Chemical class 0.000 claims description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 10
- 239000007864 aqueous solution Substances 0.000 claims description 10
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 9
- 239000011229 interlayer Substances 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 7
- 239000010410 layer Substances 0.000 claims description 7
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 6
- 239000012141 concentrate Substances 0.000 claims description 5
- 239000003960 organic solvent Substances 0.000 claims description 5
- 230000000740 bleeding effect Effects 0.000 claims description 3
- 229920002678 cellulose Polymers 0.000 claims description 3
- 239000001913 cellulose Substances 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- 238000010835 comparative analysis Methods 0.000 claims description 3
- 238000001704 evaporation Methods 0.000 claims description 3
- 230000008020 evaporation Effects 0.000 claims description 3
- 239000012528 membrane Substances 0.000 claims description 3
- 230000005540 biological transmission Effects 0.000 claims 1
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 229940079593 drug Drugs 0.000 claims 1
- 239000003814 drug Substances 0.000 claims 1
- 230000008569 process Effects 0.000 abstract description 8
- 238000005259 measurement Methods 0.000 abstract description 3
- 238000002360 preparation method Methods 0.000 abstract description 2
- 239000000284 extract Substances 0.000 description 8
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- 230000006872 improvement Effects 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 4
- 230000003595 spectral effect Effects 0.000 description 4
- 230000035945 sensitivity Effects 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 125000004494 ethyl ester group Chemical group 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 description 2
- 235000011152 sodium sulphate Nutrition 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000003987 organophosphate pesticide Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 238000004808 supercritical fluid chromatography Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/359—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using near infrared light
-
- 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
-
- 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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3563—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
-
- 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
- G01N2001/386—Other diluting or mixing processes
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The invention discloses a kind of Practice for Pesticide Residue in Agricultural Products detection methods, include the following steps：Step (1) establishes detection model；(1.1) sample is prepared：(1.2) spectroscopic data is acquired；(1.3) detection model is established；Step (2) detects agricultural product spectrum to be measured：(2.1) sample is prepared：(2.2) sample treatment：Solute obtained above is taken to be dissolved in 75ml alcoholic solutions；(2.3) spectroscopic data is acquired：Obtain the NIR transmittance spectroscopy for the solute liquid for dissolving in alcohol；Step (3) judges farm chemical ingredients and content in agricultural product；Comparison step (2.3) obtains the spectrum and the comparison of pesticide concentration detection model for dissolving in that the NIR transmittance spectroscopy of alcohol solute liquid is obtained with step (1.3).The present invention realizes the accurate detection to the type and its content of pesticide, more because improving for detection device makes sample preparation obtain process of refinement, greatly improves the selective penetrated property of pesticide molecule, and then improve the precision of measurement, meets actual operation requirements.
Description
Technical field
The present invention relates to a kind of Practice for Pesticide Residue in Agricultural Products detection method and device, belong to technical field of agricultural product detection.
Background technology
Currently, the common detection methods of pesticide residue have：Thin-layered chromatography, gas chromatography, high performance liquid chromatography,
Supercritical fluid chromatography etc..Wherein, Instrumental Analysis detection method precision highest, but its detection process is complicated, detection time
Long, biochemistry detection technology is quickly grown, but early investment is big, experiment condition is harsh, also lacks the detection device of complete set.
Patent of invention (rapid detection method of trace pesticide), application number：200910236834.1 disclosing a kind of based on infrared
The Pesticides Testing method of spectrum is penetrated, there is advantage easy to operate, detection speed is fast, then this mode uses filter paper sample
Product, permeability is bad, therefore this method poor sensitivity, measurement accuracy be not high.For this reason, it may be necessary to study a kind of new technical solution
It gives and solves.
Invention content
The present invention is exactly in view of the deficienciess of the prior art, provide a kind of Practice for Pesticide Residue in Agricultural Products detection method and dress
It sets, realizes the accurate detection to the type and its content of pesticide, more improving so that sample preparation obtains essence because of detection device
Micronization processes, greatly improve the selective penetrated property of pesticide molecule, and then improve the precision of measurement, meet actual use and want
It asks.
To solve the above problems, the technical solution used in the present invention is as follows：
A kind of Practice for Pesticide Residue in Agricultural Products detection method, includes the following steps：
Step (1) establishes detection model
(1.1) sample is prepared：The pesticide that distilled water will be dissolved in is mixed with distilled water, pesticide and distilled water
Mass ratio is chosen to multiple proportionate relationships of arithmetic progression；
(1.2) spectroscopic data is acquired：Obtain pesticide aqueous solution NIR transmittance spectroscopy；
(1.3) detection model is established：It is closely red according to the ratio and corresponding pesticide aqueous solution of pesticide and distilled water
Outer transmitted spectrum establishes spectrum and pesticide concentration detection model in two-dimensional coordinate system；
Step (2) detects agricultural product spectrum to be measured
(2.1) sample is prepared：
Agricultural product cleaning to be measured is clean, it is subsequently placed in the vacuum chamber of detection device, draught head is realized by vacuum pump
Compression liquid is carried out to agricultural product to be measured to obtain, then anhydrous sodium sulfate, organic solvent acetic acid by being equipped in regulation pipe one, two
Ethyl ester and activated carbon are adjusted compression liquid, filter；
(2.2) electrode-induced：Above-mentioned compression filtrate is placed on the lower electrode dielectric of plasma device, voltage
2.2kV, electric current 1.2mA, gap 3.2mm operating condition under irradiate 3-5 seconds；
(2.3) it concentrates：Above-mentioned compression filtrate is placed in the salt bath that temperature is 65-75 degree and is heated, in filtrate to be compressed
Evaporation of the solvent it is clean, leave solute；
(2.4) sample treatment：Solute obtained above is taken to be dissolved in 75ml alcoholic solutions, shaken well；
(2.5) spectroscopic data is acquired：Obtain the NIR transmittance spectroscopy for the solute liquid for dissolving in alcohol；
Step (3) judges farm chemical ingredients and content in agricultural product
The light that comparison step (2.5) obtains the NIR transmittance spectroscopy for the solute liquid for dissolving in alcohol and step (1.3) obtains
Spectrum and pesticide concentration detection model, obtain agricultural product farm chemical ingredients and content.
As an improvement of the above technical solution, the spectrum and the pesticide concentration detection model are two-dimensional curve form,
Different pesticides draws different two-dimensional curves.
As an improvement of the above technical solution, 2 points adjacent in the two-dimensional curve are linearly connected, and the two dimension is bent
Line is obtained by multi-order function approximating method.
As an improvement of the above technical solution, it is equipped with interlayer at the top of the mechanism body, vacuum is equipped with below the interlayer
Room, the interior vacuum pump for being equipped with cooperation vacuum chamber and using of the interlayer, the vacuum chamber lower section is equipped with sample regulating reservoir, the machine
Structure ontology both sides are equipped with the regulation pipe one and regulation pipe two that cooperation sample regulating reservoir uses, and are equipped with below the sample regulating reservoir
Electrode-induced device, sample storage test tube and salt bath, the sample storage test tube are arranged on electrode-induced device, the sample storage test tube
Bottom is arranged in salt bath；The Practice for Pesticide Residue in Agricultural Products detection device further includes to dissolving in the molten of alcohol in sample storage test tube
The spectrum instrument for detecting pesticide residue through that matter liquid is detected, the mechanism body outer layer are equipped with cooperation spectrum instrument for detecting pesticide residue through
The comparative analysis mechanism used.
As an improvement of the above technical solution, it is equipped with valve and air bleeding valve at the top of the vacuum chamber, is set in the vacuum chamber
There are the clamping device being used cooperatively, the vacuum chamber bottom to be equipped with filtering port, the filtering port is equipped with the carrier of falling liquid, described
The carrier of falling liquid is mutual superimposed filter paper and cellulose membrane.
As an improvement of the above technical solution, it is equipped with and sample regulating reservoir phase in the regulation pipe one and regulation pipe two
The conduit of connection, the conduit are equipped with regulating valve, and sample regulating reservoir bottom is equipped with filter layer and coordinates the sample storage examination
The guide pipe that pipe uses.
As an improvement of the above technical solution, the electrode-induced device includes the lower electrode dielectric of plasma device,
The lower electrode dielectric of the plasma device is voltage 2.2kV, electric current 1.2mA, gap 3.2mm.
Compared with prior art, implementation result of the invention is as follows by the present invention：
Practice for Pesticide Residue in Agricultural Products detection method of the present invention, initially sets up detection model, then passes through detection device pair
The process of refinement of detected sample, the molecule selective penetrated property for improving detected sample, and then improve to detected sample
It carries out the precision of spectral detection and accurately judges that farm chemical ingredients and content (can not only be examined by spectrum in agricultural product
The type of pesticide is measured, can also judge the content of pesticide according to the power of absorption), i.e., by being compared with detection model
To its content, detection result is good, efficient, meets actually detected demand.
In addition, detection device is reasonable in design, easy to operate, easy, the convenient fining to agricultural product to be measured
Processing greatly improves the molecule selective penetrated property of detected sample, facilitates the detection to Practice for Pesticide Residue in Agricultural Products amount, wherein
The characteristic that molecule after at electrode-induced has selective penetrated property extremely strong, sensitivity is good, further improves accuracy of detection.
Description of the drawings
Fig. 1 is structure of the detecting device schematic diagram of the present invention.
Specific implementation mode
Illustrate present disclosure below in conjunction with specific embodiments.
Embodiment 1
A kind of Practice for Pesticide Residue in Agricultural Products detection method, includes the following steps：
Step (1) establishes detection model
(1.1) sample is prepared：The pesticide that distilled water will be dissolved in is mixed with distilled water, pesticide and distilled water
Mass ratio is chosen to multiple proportionate relationships of arithmetic progression；
(1.2) spectroscopic data is acquired：Obtain pesticide aqueous solution NIR transmittance spectroscopy；
(1.3) detection model is established：It is closely red according to the ratio and corresponding pesticide aqueous solution of pesticide and distilled water
Outer transmitted spectrum establishes spectrum and pesticide concentration detection model in two-dimensional coordinate system；
Step (2) detects agricultural product spectrum to be measured
(2.1) sample is prepared：
Agricultural product cleaning to be measured is clean, it is subsequently placed in the vacuum chamber of detection device, draught head is realized by vacuum pump
Compression liquid is carried out to agricultural product to be measured to obtain, then anhydrous sodium sulfate, organic solvent acetic acid by being equipped in regulation pipe one, two
Ethyl ester and activated carbon are adjusted compression liquid, filter；
(2.2) electrode-induced：Above-mentioned compression filtrate is placed on the lower electrode dielectric of plasma device, voltage
2.2kV, electric current 1.2mA, gap 3.2mm operating condition under irradiate 3-5 seconds；
(2.3) it concentrates：Above-mentioned compression filtrate is placed in the salt bath that temperature is 65-75 degree and is heated, in filtrate to be compressed
Evaporation of the solvent it is clean, leave solute；
(2.4) sample treatment：Solute obtained above is taken to be dissolved in 75ml alcoholic solutions, shaken well；
(2.5) spectroscopic data is acquired：Obtain the NIR transmittance spectroscopy for the solute liquid for dissolving in alcohol；
Step (3) judges farm chemical ingredients and content in agricultural product
The light that comparison step (2.5) obtains the NIR transmittance spectroscopy for the solute liquid for dissolving in alcohol and step (1.3) obtains
Spectrum and pesticide concentration detection model, obtain agricultural product farm chemical ingredients and content.
Specifically, the spectrum and the pesticide concentration detection model are two-dimensional curve form, and different pesticides is drawn not
Same two-dimensional curve；Adjacent 2 points are linearly connected in the two-dimensional curve, and the two-dimensional curve is fitted by multi-order function
Method obtains.
Wherein, the Practice for Pesticide Residue in Agricultural Products detection device, including mechanism body 100,100 top of mechanism body are equipped with
Interlayer 10,10 lower section of the interlayer are equipped with vacuum chamber 20, and the vacuum pump that cooperation vacuum chamber 20 uses is equipped in the interlayer 10
11,20 lower section of the vacuum chamber is equipped with sample regulating reservoir 30, and 100 both sides of the mechanism body are equipped with cooperation sample regulating reservoir 30
The regulation pipe 1 and regulation pipe 2 42 used, 30 lower section of the sample regulating reservoir are equipped with electrode-induced device 50, sample storage test tube
60 and salt bath 70, the sample storage test tube 60 is arranged on electrode-induced device 50, and 60 bottom of the sample storage test tube setting exists
In salt bath 70；The Practice for Pesticide Residue in Agricultural Products detection device further include to dissolved in sample storage test tube 60 the solute liquid of alcohol into
The spectrum instrument for detecting pesticide residue through 80 of row detection, 100 outer layer of the mechanism body are equipped with cooperation spectrum instrument for detecting pesticide residue through 80
The comparative analysis mechanism 90 used.
It is further improved ground, 20 top of the vacuum chamber is equipped with valve 21 and air bleeding valve 22, is equipped in the vacuum chamber 20
The clamping device 23 being used cooperatively, 20 bottom of vacuum chamber are equipped with filtering port 24, and filtering port 24 is equipped with the carrier of falling liquid 241, liquid
Carrier 241 is mutual superimposed filter paper and cellulose membrane.
It is further improved ground, is equipped in the regulation pipe 1 and regulation pipe 2 42 and is connected with sample regulating reservoir 30
Conduit 43, the conduit 43 be equipped with regulating valve 431,30 bottom of sample regulating reservoir be equipped with filter layer 31 and cooperation store up
The guide pipe 32 that sample test tube 60 uses.
Specifically, the electrode-induced device 50 includes the lower electrode dielectric 51 of plasma device, plasma device
Lower electrode dielectric 51 voltage be 2.2kV, electric current 1.2mA, gap 3.2mm.
Practice for Pesticide Residue in Agricultural Products detection method of the present invention, initially sets up detection model, then passes through detection device pair
The process of refinement of detected sample, the molecule selective penetrated property for improving detected sample, and then improve to detected sample
It carries out the precision of spectral detection and accurately judges that farm chemical ingredients and content (can not only be examined by spectrum in agricultural product
The type of pesticide is measured, can also judge the content of pesticide according to the power of absorption), i.e., by being compared with detection model
To its content, detection result is good, efficient, meets actually detected demand.
In addition, detection device is reasonable in design, easy to operate, easy, the convenient fining to agricultural product to be measured
Processing greatly improves the molecule selective penetrated property of detected sample, facilitates the detection to Practice for Pesticide Residue in Agricultural Products amount, wherein
The characteristic that molecule after at electrode-induced has selective penetrated property extremely strong, sensitivity is good, further improves accuracy of detection
Note：The accuracy of detection of the detection method cooperation detection device of the present invention is up to 99.3%.
Embodiment 2
A kind of Practice for Pesticide Residue in Agricultural Products detection method, includes the following steps：
Step (1) establishes detection model
(1.1) sample is prepared：The pesticide that distilled water will be dissolved in is mixed with distilled water, pesticide and distilled water
Mass ratio is chosen to multiple proportionate relationships of arithmetic progression；
(1.2) spectroscopic data is acquired：Obtain pesticide aqueous solution NIR transmittance spectroscopy；
(1.3) detection model is established：It is closely red according to the ratio and corresponding pesticide aqueous solution of pesticide and distilled water
Outer transmitted spectrum establishes spectrum and organophosphorus pesticide content detection model in two-dimensional coordinate system；
Step (2), detection agricultural product to be measured
(2.1) sample is prepared：
(2.11) it extracts：By agricultural product chopping, grinding, weigh 12g in centrifuge tube, be added 10g anhydrous sodium sulfates and
The organic solvent ethyl acetate of 18ml extracts 4min, then extract liquor is transferred in another centrifuge tube；
(2.13) electrode-induced：Above-mentioned extract liquor is placed on the lower electrode dielectric of plasma device, voltage 2.2kV,
Electric current 1.2mA, gap 3.2mm operating condition under irradiate 4 seconds；
(2.14) it concentrates：Test tube equipped with filtrate is placed in the salt bath that temperature is 65 degree and is evaporated, until leaving solute；
(2.2) sample treatment：Solute obtained above is taken to be dissolved in 75ml alcoholic solutions, shaken well；
(2.3) spectroscopic data is acquired：Obtain the NIR transmittance spectroscopy for the solute liquid for dissolving in alcohol；
Step (3) judges farm chemical ingredients and content in agricultural product
The light that comparison step (2.3) obtains the NIR transmittance spectroscopy for the solute liquid for dissolving in alcohol and step (1.3) obtains
Spectrum and pesticide concentration detection model, obtain farm chemical ingredients and content.
Specifically, the spectrum and the pesticide concentration detection model are two-dimensional curve form, and different pesticides is drawn not
Same two-dimensional curve；Adjacent 2 points are linearly connected in the two-dimensional curve, and the two-dimensional curve is fitted by multi-order function
Method obtains.
Practice for Pesticide Residue in Agricultural Products detection method of the present invention, initially sets up detection model, then passes through detection device pair
The process of refinement of detected sample, the molecule selective penetrated property for improving detected sample, and then improve to detected sample
It carries out the precision of spectral detection and accurately judges that farm chemical ingredients and content (can not only be examined by spectrum in agricultural product
The type of pesticide is measured, can also judge the content of pesticide according to the power of absorption), i.e., by being compared with detection model
To its content, detection result is good, efficient, meets actually detected demand
Note：The present embodiment is not used and is detected under any detection device only with the detection method of the present invention,
Accuracy of detection is up to 95.1%).
Embodiment 3
A kind of Practice for Pesticide Residue in Agricultural Products detection method, includes the following steps：
Step (1) establishes detection model
(1.1) sample is prepared：The pesticide that distilled water will be dissolved in is mixed with distilled water, pesticide and distilled water
Mass ratio is chosen to multiple proportionate relationships of arithmetic progression；
(1.2) spectroscopic data is acquired：Obtain pesticide aqueous solution NIR transmittance spectroscopy；
(1.3) detection model is established：It is closely red according to the ratio and corresponding pesticide aqueous solution of pesticide and distilled water
Outer transmitted spectrum establishes spectrum and pesticide concentration detection model in two-dimensional coordinate system；
Step (2), detection agricultural product to be measured
(2.1) sample is prepared：
(2.11) it extracts：By agricultural product chopping, grinding, claim 12g in centrifuge tube, 10g anhydrous sodium sulfates and 18ml is added
Organic solvent ethyl acetate, extract 4min, then extract liquor is transferred in another centrifuge tube；
(2.12) it purifies：The activated carbon of the anhydrous sodium sulfate and 0.18g of 6g is added into the centrifuge tube equipped with extract liquor,
2min is vibrated, upper solution is drawn after standing, filtering removal is suspended in the activated carbon in solution, filtrate is collected in test tube；
(2.13) it concentrates：Test tube equipped with filtrate, which is placed in temperature, is in 65 degree of salt bath, with nitrogen or air by test tube
In solvent purging it is clean, until leaving solute；
(2.2) sample treatment：Solute obtained above is taken to be dissolved in 75ml alcoholic solutions, shaken well；
(2.3) spectroscopic data is acquired：Obtain the NIR transmittance spectroscopy for the solute liquid for dissolving in alcohol；
Step (3) judges farm chemical ingredients and content in agricultural product
The light that comparison step (2.3) obtains the NIR transmittance spectroscopy for the solute liquid for dissolving in alcohol and step (1.3) obtains
Spectrum and pesticide concentration detection model, obtain farm chemical ingredients and content.
Specifically, the spectrum and the pesticide concentration detection model are two-dimensional curve form, and different pesticides is drawn not
Same two-dimensional curve；Adjacent 2 points are linearly connected in the two-dimensional curve, and the two-dimensional curve is fitted by multi-order function
Method obtains.
Practice for Pesticide Residue in Agricultural Products detection method of the present invention, initially sets up detection model, then by sample to be detected
The process of refinement of product, the molecule selective penetrated property for improving detected sample, and then improve and spectrum is carried out to detected sample
The precision of detection and accurately judge that farm chemical ingredients and content (not only can go out pesticide by spectral detection in agricultural product
Type, can also judge the content of pesticide according to the power of absorption), i.e., its content is obtained by the comparison with detection model,
Detection result is good, efficient, meets actually detected demand
Note：The present embodiment carries out depth process of refinement only with the detection method of the present invention to sample to be tested,
Not using being detected under any detection device, accuracy of detection is up to 96.7%).
In summary：The setting to sample to be tested detection device is can be seen that in conjunction with 3 different embodiments and is treated
The fine-grained management of sample directly affects detection efficiency and the precision of detection, especially to sample to be tested detection device
Setting, directly affects the precision detected to sample to be tested.
The foregoing is a detailed description of the present invention in conjunction with specific embodiments, and it cannot be said that the present invention is specific
Implementation is only limitted to these explanations.For those skilled in the art to which the present invention belongs, present inventive concept is not being departed from
Under the premise of, a number of simple deductions or replacements can also be made, all shall be regarded as belonging to the scope of protection of the invention.
Claims (7)
1. a kind of Practice for Pesticide Residue in Agricultural Products detection method, it is characterised in that：Include the following steps：
Step (1) establishes detection model
(1.1) sample is prepared：The pesticide that distilled water will be dissolved in is mixed with distilled water, the mass ratio of pesticide and distilled water
It is chosen to multiple proportionate relationships of arithmetic progression；
(1.2) spectroscopic data is acquired：Obtain pesticide aqueous solution NIR transmittance spectroscopy；
(1.3) detection model is established：According to the ratio and corresponding pesticide aqueous solution near-infrared transmission of pesticide and distilled water
Spectrum establishes spectrum and pesticide concentration detection model in two-dimensional coordinate system；
Step (2) detects agricultural product spectrum to be measured
(2.1) sample is prepared：
Agricultural product cleaning to be measured is clean, it is subsequently placed in the vacuum chamber of detection device, realizes that draught head is treated by vacuum pump
Survey agricultural product carry out compression liquid obtain, then the anhydrous sodium sulfate by being equipped in regulation pipe one, two, organic solvent ethyl acetate and
Activated carbon is adjusted compression liquid, filters；
(2.2) electrode-induced：Above-mentioned compression filtrate is placed on the lower electrode dielectric of plasma device, voltage 2.2kV, electric current
1.2mA, gap 3.2mm operating condition under irradiate 3-5 seconds；
(2.3) it concentrates：Above-mentioned compression filtrate is placed in the salt bath that temperature is 65-75 degree and is heated, it is molten in filtrate to be compressed
Agent evaporation is clean, leaves solute；
(2.4) sample treatment：Solute obtained above is taken to be dissolved in 75ml alcoholic solutions, shaken well；
(2.5) spectroscopic data is acquired：Obtain the NIR transmittance spectroscopy for the solute liquid for dissolving in alcohol；
Step (3) judges farm chemical ingredients and content in agricultural product
Comparison step (2.5) obtain spectrum that NIR transmittance spectroscopy and the step (1.3) of the solute liquid for dissolving in alcohol obtain with
Pesticide concentration detection model obtains agricultural product farm chemical ingredients and content.
2. a kind of Practice for Pesticide Residue in Agricultural Products detection method according to claim 1, it is characterised in that：The spectrum and the agriculture
Medicine content detection model is two-dimensional curve form, and different pesticides draws different two-dimensional curves.
3. a kind of Practice for Pesticide Residue in Agricultural Products detection method according to claim 2, it is characterised in that：Phase in the two-dimensional curve
Adjacent 2 points are linearly connected, and the two-dimensional curve is obtained by multi-order function approximating method.
4. according to a kind of Practice for Pesticide Residue in Agricultural Products detection device described in claim 1-3, it is characterised in that：Including mechanism body
(100), interlayer (10) is equipped at the top of the mechanism body (100), is equipped with vacuum chamber (20) below the interlayer (10), it is described every
It is equipped with the vacuum pump (11) that cooperation vacuum chamber (20) uses in layer (10), sample regulating reservoir is equipped with below the vacuum chamber (20)
(30), mechanism body (100) both sides are equipped with the regulation pipe one (41) and regulation pipe two that cooperation sample regulating reservoir (30) uses
(42), electrode-induced device (50), sample storage test tube (60) and salt bath (70) are equipped with below the sample regulating reservoir (30), it is described
Sample storage test tube (60) is arranged on electrode-induced device (50), and sample storage test tube (60) the bottom setting is in salt bath (70)；
The Practice for Pesticide Residue in Agricultural Products detection device further includes the light being detected to dissolving in the solute liquid of alcohol in sample storage test tube (60)
Instrument for detecting pesticide residue through (80) is composed, mechanism body (100) outer layer is equipped with cooperation spectrum instrument for detecting pesticide residue through (80) and uses
Comparative analysis mechanism (90).
5. a kind of Practice for Pesticide Residue in Agricultural Products detection device according to claim 4, it is characterised in that：Vacuum chamber (20) top
Portion is equipped with valve (21) and air bleeding valve (22), and the clamping device (23) being used cooperatively is equipped in the vacuum chamber (20), described true
Empty room (20) bottom is equipped with filtering port (24), and the filtering port (24) is equipped with the carrier of falling liquid (241), the carrier of falling liquid
(241) it is mutual superimposed filter paper and cellulose membrane.
6. a kind of Practice for Pesticide Residue in Agricultural Products detection device according to claim 4, it is characterised in that：The regulation pipe one (41)
Be equipped with the conduit (43) being connected with sample regulating reservoir (30) in regulation pipe two (42), the conduit (43), which is equipped with, to be adjusted
Valve (431), the guiding that sample regulating reservoir (30) bottom is equipped with filter layer (31) and the cooperation sample storage test tube (60) uses
It manages (32).
7. a kind of Practice for Pesticide Residue in Agricultural Products detection device according to claim 4, it is characterised in that：The electrode-induced device
(50) include plasma device lower electrode dielectric (51), the voltage of the lower electrode dielectric (51) of the plasma device is
2.2kV, electric current 1.2mA, gap 3.2mm.
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| CN111220601A (en) * | 2018-11-27 | 2020-06-02 | 上海尚湾信息技术有限公司 | Rapid detection method for pesticide residues in vegetables and fruits |
| CN111742931A (en) * | 2020-08-06 | 2020-10-09 | 祥霖美丰生物科技(淮安)有限公司 | Pesticide composition containing fosthiazate and cyclobutrifuram and used for preventing and treating root-knot nematodes |
| CN111771893A (en) * | 2020-08-06 | 2020-10-16 | 祥霖美丰生物科技(淮安)有限公司 | Pesticide composition containing tioxazafen and cyclobutrifluram |
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Application publication date: 20180824 |