CN110346344A - A kind of detection method of pesticide residue containing Cyano chrysanthemate - Google Patents
A kind of detection method of pesticide residue containing Cyano chrysanthemate Download PDFInfo
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- CN110346344A CN110346344A CN201811352885.6A CN201811352885A CN110346344A CN 110346344 A CN110346344 A CN 110346344A CN 201811352885 A CN201811352885 A CN 201811352885A CN 110346344 A CN110346344 A CN 110346344A
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- detection method
- residue containing
- pesticide residue
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- cyano chrysanthemate
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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
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
- G01N21/658—Raman scattering enhancement Raman, e.g. surface plasmons
Abstract
The invention discloses a kind of detection methods of pesticide residue containing Cyano chrysanthemate, comprising the following steps: (1) takes sample to be tested to be placed in a beaker, shred, ultrasonic extraction after organic solvent is added；Extracting solution is transferred in sample cell, is vibrated, is stood to layering；It takes supernatant to be transferred in another sample cell, alkaline solution is added, vibrate, stand；Aqueous solution is added into another sample cell, vibrates, stratification takes lower layer's solution for standby；(2) it takes the 50 above-mentioned lower layer's solution examples of the μ of μ L~200 L in Raman sample pool, the 10 μ L metal-sols of μ L~200 is added, mix, the Raman sample pool is then placed on portable Raman spectrometer detection interior and is detected.The detection method high sensitivity, it is swift to operate, it is at low cost.
Description
Technical field
The present invention relates to a kind of detection methods of pesticide residue containing Cyano chrysanthemate, belong to Detecting Pesticide field.
Background technique
The pesticide of class containing Cyano chrysanthemate has the characteristics that insecticidal spectrum is wide, quick-acting is good, less toxic, in early days in terms of pernicious pests control
Important function is played.But after large-scale popularization is using quasi- deinsectization class containing Cyano chrysanthemate pesticide, cause to occur in poisoning and food
The case where residual is detected by foreign countries is more and more, and safety increasingly causes the concern of people with residual.
Pyrethrins residuces quantity measuring method mainly has gas-chromatography (GC), high performance liquid chromatography (HPLC) etc. at present.Gas
Phase chromatography (GC) requires strictly the purification of sample using highly sensitive electron capture detector (ECD), thus increases
The time of analysis process.Since pyrethroids has thermal instability, and gas chromatography (GC) needs higher vapourizing temperature, is examining
Pyrethroids is destroyed during surveying, accuracy in detection is not high.High performance liquid chromatography (HPLC), which analyzes chrysanthemum ester type compound, to be had centainly
Advantage, its requirement to sample purification process is opposite to want low, does not need higher vapourizing temperature.But it is measured using HPLC method
When pesticide residue containing Cyano chrysanthemate, the main problem encountered is that the sensitivity of detector is lower.Moreover, gas-chromatography (GC) and height
The instrument of effect liquid phase chromatogram (HPLC) is costly, at high cost.
" highly sensitive conical fiber SERS probe and its application in the residual detection of agriculture " of the Lei Xing and " surface of Sun Xudong
The progress of enhancing Raman spectroscopy detection pesticide residue " describe detection of the SERS to part agriculture residual standard product.Surface increases
Strong Raman spectroscopy (SERS) be interaction between a kind of very effective molecular detection, characterization surface molecular adsorption behavior and
The tool of molecular structure.SERS signal is 106 times higher than raman spectral signal before enhancing, due to its high detection sensitivity, high-resolution
Rate, water interference is small, can quench the advantages that fluorescence, stability are good, has very big application potential in terms of Detecting Pesticide.But
It is that application of the Raman spectroscopy of existing literature report in Detecting Pesticide is mainly also only limitted to standard items detection and few
Residual actually detected, the specific detection method of pesticide residue containing Cyano chrysanthemate of not registering also of several agricultures of number.
Summary of the invention
It is an object of the invention in place of overcome the deficiencies in the prior art, provide a kind of inspection of pesticide residue containing Cyano chrysanthemate
Survey method, the detection method is swift to operate, at low cost.
The technical solution adopted by the present invention to solve the technical problems is:
A kind of detection method of pesticide residue containing Cyano chrysanthemate, comprising the following steps:
(1) it takes 1-5g sample to be tested to be placed in a beaker, shreds, ultrasonic extraction after 5-10mL organic solvent is added；By 3-
5mL extracting solution is transferred in sample cell, and the alkaline solution of 0.2-1mL is added, and vibrates 10-20s, stands 1-5min；It is another toward this
0.2-2mL aqueous solution is added in sample cell, vibrates 10-20s, stratification takes lower layer's solution for standby；
(2) it takes the 50 above-mentioned lower layer's solution examples of the μ of μ L~200 L in Raman sample pool, it is molten that the 10 μ L metals of μ L~200 is added
Glue mixes, and the Raman sample pool is then placed on portable Raman spectrometer detection interior and is detected.
Preferably, the organic solvent described in step (1) be acetonitrile, methylene chloride, acetone, ethylene glycol, ethyl acetate,
Hexane, petroleum ether or its mixed solution.
Preferably, it is added before alkaline solution in step (1), suitable adsorbent is first added into sample cell, vibrated
After absorption, supernatant is transferred in another sample cell, then carries out subsequent step.
Preferably, above-mentioned adsorbent be N- propyl ethylenediamine, phosphoenolpyruvate, graphitized carbon, anhydrous calcium chloride,
Or mixtures thereof anhydrous magnesium sulfate.
Preferably, the additional amount of adsorbent is 0.05-1g.
Preferably, the alkaline solution described in step (1) is sodium hydroxide, potassium hydroxide or barium hydroxide, concentration
For 1mM to saturation.
Preferably, the aqueous solution described in step (1) is sodium chloride, sodium sulphate, sodium hydroxide, sodium nitrate or its mixing
Solution.
Preferably, the metal-sol described in step (2) is nanogold or nano silver.
The pesticide of class containing Cyano chrysanthemate of the present invention, including but not limited to taufluvalinate, cyfloxylate, efficient fluorine chlorine
Cyano chrysanthemate, flucythrinate, Fenpropathrin, decis, S- fenvalerate, fenvalerate, gamma cyhalothrin, chlorine fluorine cyanogen
Pyrethroids, effective cypermethrin, cypermethrin etc..
The technical program compared with the background art, it has the following advantages:
1, the method for the present invention will contain Cyano chrysanthemate under alkaline condition and decomposite cyanogen root, and adopts under alkaline condition in sample
Effective detection to the cyanogen root in the pesticide of class containing Cyano chrysanthemate is realized with Raman spectroscopy, and high sensitivity, method safety is reliable, no
Expensive instrument is needed, it is at low cost.
2, the entire detection time of the method for the present invention is in 10min-15min, and convenient and efficient, the method is to operator's safety nothing
Injury is well suited for the quick detection at scene.
3, the detection in the pesticide residues such as veterinary antibiotics and tealeaves containing Cyano chrysanthemate may be implemented in the method for the present invention, using model
It encloses wide.
4, detection limit of the present invention can be down to 0.2mg/kg.
Detailed description of the invention
Below with reference to figure, the invention will be further described with embodiment.
Fig. 1 is the Surface enhanced Raman spectroscopy of mark-on 5ppm cypermethrin in green vegetables.
Fig. 2 is the Surface enhanced Raman spectroscopy of mark-on 5ppm Fenpropathrin in tealeaves.
Fig. 3 is the Surface enhanced Raman spectroscopy of mark-on 5ppm flucythrinate in apple.
Specific embodiment
The contents of the present invention are illustrated below by embodiment:
Nanogold the preparation method comprises the following steps: 250mL round-bottomed flask is added in the aqueous solution of chloraurate of the 0.01wt% of 100mL
In, it is heated to after acutely boiling, is vigorously stirred down the 1wt% trisodium citrate aqueous solution for rapidly joining 1mL, continue heating stirring
After 60min, stop heating, continues to stand after stirring 30min, room temperature natural cooling.
Nano silver the preparation method comprises the following steps: the 1mM silver nitrate aqueous solution of 100mL is added in 250mL round-bottomed flask, be heated to
Acutely after boiling, it is vigorously stirred down the 1wt% trisodium citrate aqueous solution for rapidly joining 1mL, after continuing heating stirring 60min,
Stop heating, continues to stand after stirring 30min, room temperature natural cooling.
Embodiment 1: taking 2g green vegetables, shred, mark-on 5ppm cypermethrin, and 5mL acetonitrile ultrasonic extraction is added, 3mL is taken to extract
Liquid vibrates 10s in sample cell, stands 5min layering.It takes 2mL supernatant in another sample cell, 500 μ L0.5M hydrogen is added
Potassium oxide vibrates 10s, stands 2min, and 500 μ L2M sodium chloride are being added, are vibrating 10s, stratification, lower layer's solution for standby.It takes
100 μ L prepare liquids are added 200 μ L nanogold and mix in Raman sample pool, and it is indoor to be then placed on portable Raman spectrometer detection
Detected (Raman spectrometer power 280mw, optical maser wavelength 785nm, scanning range 200-3200cm-1), obtain the surface such as Fig. 1
Enhance Raman spectrum.As shown in Figure 1, the detection of cypermethrin may be implemented in the method.
Embodiment 2: taking 1g tealeaves, shred, mark-on 5ppm Fenpropathrin, and 5mL ethyl acetate ultrasonic extraction is added, takes 3mL
0.1gN- propyl ethylenediamine and 0.5g anhydrous sodium sulfate is added in sample cell in extracting solution, vibrates 20s, stands 1min layering.It takes
200 μ L0.1M sodium hydroxides are added in another sample cell in 2mL supernatant, vibrate 20s, stand 2min, and 500 μ L 2M are being added
Potassium sulfate vibrates 20s, stratification, lower layer's solution for standby.It takes 200 μ L prepare liquids in Raman sample pool, 100 μ L is added and receive
Rice gold mixes, and is then placed on portable Raman spectrometer detection interior and is detected (Raman spectrometer power 280mw, optical maser wavelength
785nm, scanning range 200-3200cm-1), obtain the Surface enhanced Raman spectroscopy such as Fig. 2.As shown in Figure 2, the method can be real
The detection of existing Fenpropathrin.
Embodiment 3: taking 5g apple, shred, mark-on 5ppm flucythrinate, and 10mL acetone ultrasonic extraction is added, takes 5mL
0.5g phosphoenolpyruvate is added in sample cell in extracting solution, vibrates 10s, stands 1min layering.Take 3mL supernatant in
In another sample cell, 1mL 0.1M sodium hydroxide is added, vibrates 10s, stands 2min, 500 μ L 5M sodium hydroxides, vibration is being added
Swing 10s, stratification, lower layer's solution for standby.It takes 200 μ L prepare liquids in Raman sample pool, 50 μ L nano silvers is added and mix, so
After be placed on portable Raman spectrometer detection interior and detected (Raman spectrometer power 280mw, optical maser wavelength 785nm, scanning
Range 200-3200cm-1), obtain the Surface enhanced Raman spectroscopy such as Fig. 3.From the figure 3, it may be seen that penta chrysanthemum of fluorine cyanogen may be implemented in the method
The detection of ester.
The above is only the preferred embodiment of the present invention, the range implemented of the present invention that therefore, it cannot be limited according to, i.e., according to
Equivalent changes and modifications made by the invention patent range and description, should still be within the scope of the present invention.
Claims (9)
1. a kind of detection method of pesticide residue containing Cyano chrysanthemate, it is characterised in that: the following steps are included:
(1) it takes 1-5g sample to be tested to be placed in a beaker, shreds, ultrasonic extraction after 5-10mL organic solvent is added；3-5mL is mentioned
It takes liquid to be transferred in sample cell, the alkaline solution of 0.2-1mL is added, vibrate 10-20s, stand 1-5min；Toward another sample cell
Middle addition 0.2-2mL aqueous solution, vibrates 10-20s, and stratification takes lower layer's solution for standby；
(2) it takes the 50 above-mentioned lower layer's solution examples of the μ of μ L~200 L in Raman sample pool, the 10 μ L metal-sols of μ L~200 is added, mix
It is even, the Raman sample pool is then placed on portable Raman spectrometer detection interior and is detected.
2. the detection method of pesticide residue containing Cyano chrysanthemate according to claim 1, it is characterised in that: the institute in step (1)
The organic solvent stated is acetonitrile, methylene chloride, acetone, ethylene glycol, ethyl acetate, hexane, petroleum ether or its mixed solution.
3. the detection method of pesticide residue containing Cyano chrysanthemate according to claim 1, it is characterised in that: add in step (1)
Before entering alkaline solution, suitable adsorbent is first added into sample cell, supernatant is transferred to another sample after oscillation absorption
Guan Zhong, then carry out subsequent step.
4. the detection method of pesticide residue containing Cyano chrysanthemate according to claim 3, it is characterised in that: the institute in step (1)
The adsorbent stated be N- propyl ethylenediamine, phosphoenolpyruvate, graphitized carbon, anhydrous calcium chloride, anhydrous magnesium sulfate or its
Mixture.
5. the detection method of pesticide residue containing Cyano chrysanthemate according to claim 3 or 4, it is characterised in that: adsorbent adds
Entering amount is 0.05-1g.
6. the detection method of pesticide residue containing Cyano chrysanthemate according to claim 1, it is characterised in that: the institute in step (1)
The alkaline solution stated is sodium hydroxide, potassium hydroxide or barium hydroxide, and concentration is that 1mM is extremely saturated.
7. the detection method of pesticide residue containing Cyano chrysanthemate according to claim 1, it is characterised in that: the institute in step (1)
The aqueous solution stated is sodium chloride, sodium sulphate, sodium hydroxide, sodium nitrate or its mixed solution.
8. the detection method of pesticide residue containing Cyano chrysanthemate according to claim 1, it is characterised in that: the institute in step (2)
The metal-sol stated is nanogold or nano silver.
9. the detection method of pesticide residue containing Cyano chrysanthemate according to claim 1, it is characterised in that: described contains Cyano chrysanthemate
Class pesticide include taufluvalinate, cyfloxylate, betacyfluthrin, flucythrinate, Fenpropathrin, decis,
S- fenvalerate, fenvalerate, gamma cyhalothrin, lambda-cyhalothrin, effective cypermethrin, at least one in cypermethrin
Kind.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113092438A (en) * | 2021-03-26 | 2021-07-09 | 陕西理工大学 | Gel, nano material Raman substrate construction and pyrethroid pesticide residue detection method |
| CN114088687A (en) * | 2021-11-29 | 2022-02-25 | 云南省烟草质量监督检测站 | Displacement differential Raman-based rapid detection method for dithiocarbamate pesticides in tobacco |
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| CN114088687A (en) * | 2021-11-29 | 2022-02-25 | 云南省烟草质量监督检测站 | Displacement differential Raman-based rapid detection method for dithiocarbamate pesticides in tobacco |
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