CN108613963A - A method of decis in strawberry is detected based on gold nano surface Raman enhancement - Google Patents
A method of decis in strawberry is detected based on gold nano surface Raman enhancement Download PDFInfo
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- 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
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Abstract
The present invention discloses a kind of method detecting decis in strawberry based on gold nano surface Raman enhancement, including：Step 1, after mixing by the strawberry, acetonitrile and the sodium chloride that are attached with deltamethrin pesticide, vortex oscillation, centrifugation are carried out successively, obtains supernatant；Step 2, anhydrous magnesium sulfate, propyl ethylenediamine, C18 and Graphon are mixed with supernatant, and carries out vortex oscillation, centrifugation, filtering successively, obtain prepare liquid；Step 3, gold nano colloidal sol substrate is prepared；Step 4, after mixing by gold nano colloidal sol substrate, prepare liquid and sodium-chloride water solution, Raman spectrum acquisition is carried out；Step 5, the residual quantity of deltamethrin pesticide in strawberry is calculated according to formula.Deltamethrin pesticide method for detecting residue provided by the invention provides quick, cheap, easy, accurate detection scheme for Detecting Pesticide.
Description
Technical field
The present invention relates to plant pesticide residue detection technical fields, and in particular to one kind being based on gold nano surface Raman enhancement
The method for detecting decis in strawberry.
Background technology
Red-color strawberries seedling (also known as red cheek strawberry, Japan 99, cheek of blushing) is the maximum strawberry series of existing market plantation,
Red-color strawberries growth potential is strong, and plant is higher (25 centimetres), and as a result strain diameter is big, and mitogenetic new stem ability is medium, blade thick, petiole greatly
Light green color, base portion leaf sheath slightly take on a red color, stem thickness of crawling, and pumping ability is medium, and peduncle is thick, and bifurcation that raw small one and large one is two complete
Full leaf.Decis is a kind of benzimidazoles derivative, belongs to absorbability wide-spectrum bactericide, is widely used in the red spider of strawberry
Spider, aphid, grub control, Long Term Contact or eat by mistake be easy cause cancerous swelling, blood strangury disease and immune system disorder, seriously affect consumption
The physical and mental health of person.(GB 2763-2014) is provided according to China's Pesticide maximum residue limit, and decis is in the oil
Residual quantity must not exceed 1mg/kg.Currently, deltamethrin pesticide detection method mainly has gas chromatography-mass spectrography, liquid phase color
Spectrometry etc., accurate, high sensitivity that these methods have the characteristics that, but complex pretreatment, of high cost, detection time is long, detector
Device is expensive, it is difficult to meet extensive online, low cost, the testing requirements of high speed.
Raman spectrum (Raman spectra) is a kind of scattering spectrum, and Raman spectrum analysis method is to be based on India scientist
C.V. the Raman scattering effect that Raman (Raman) is found, principle are：Pair scattering spectrum different from incident light frequency carries out
Analysis is to obtain molecular vibration, rotation aspect information.Surface enhanced Raman spectroscopy (surface-enhanced Raman
Spectroscopy, SERS) technology refers to Molecular Adsorption to the surface of certain nanoscale rough metals (such as gold, gold, copper) or molten
In glue, make the Raman signal of adsorbent at the enhancing of geometry multiple.SERS technologies can be realized to micro-example and monomolecular
Quickly detection, meanwhile and a kind of Fingerprint of high sensitivity, there is instrument to be easy to carry about with one, is easy to operate, pre-treatment it is convenient
The features such as.In recent years, lot of domestic and international scholar application surface enhances Raman spectrum to micro-example and monomolecular quick detection
It is studied.
Surface enhanced Raman spectroscopy technology refers to table of the Molecular Adsorption to certain nanoscale rough metals (such as gold, gold, copper)
In face or colloidal sol, make the Raman signal of adsorbent at the enhancing of geometry multiple, is suitble to carry out the remains of pesticide in agricultural product
Rapid screening.Chetan etc. makes gold size capillary column and carried out post detection to orange juice, and in conjunction with SERS technologies, detection is minimum dense
Degree is 50 μ g/L.Li et al. is research pair with organophosphorus pesticide (thimet and Entex) using gold nanoparticle as enhancing substrate
As choosing 2cm2Apple epidermis simulates pesticide residue, is detected with SERS, chooses 728cm respectively-1And 1215cm-1For mesh
It marks peak and carries out quantitative analysis, the results showed that detection limit is respectively 0.05 and 0.4mg/L.It opens duckweed etc. and uses Surface enhanced Raman spectroscopy
Detection technique combination Accelerated solvent extraction pre-treating method establishes the quick inspection of basic element of cell division 6-BA residuals in bean sprouts
Survey method.Kim etc. acquires the Surface enhanced Raman spectroscopy of solution to be measured under different pH value using benzimidazole as research object,
Raman spectra is belonged to.He etc. combines a quick and easy method to realize apple surface bromine cyanogen using SERS technologies
The detection of pyrethrin pesticide, detection time only need 10min.Although the studies above can be reached using Surface enhanced Raman spectroscopy technology
To the purpose that pesticide molecular signal in agricultural product enhances, but fail fully to remove the influence of stroma ground substance, the detection limit of method has
It waits further increasing, accuracy, the stability of method are poor, and detection method is also to be further improved, in addition, about utilization
Surface enhanced Raman spectroscopy technology detects the remaining research of decis bactericide agricultural chemicals in strawberry, and there is not been reported.
Invention content
The present invention provides a kind of methods detecting decis in strawberry based on gold nano surface Raman enhancement, are pesticide
Residue detection provides quick, cheap, easy, accurate detection scheme.
Specific technical solution of the present invention is as follows：
A method of decis in strawberry is detected based on gold nano surface Raman enhancement, including：
Step 1, after mixing by the strawberry, acetonitrile and the sodium chloride that are attached with deltamethrin pesticide, it is vortexed successively
Oscillation, centrifugation, obtain supernatant；
Step 2, anhydrous magnesium sulfate, propyl ethylenediamine, C18 and Graphon are mixed with supernatant, and carried out successively
Vortex oscillation, centrifugation, filtering, obtain prepare liquid；
Step 3, gold nano colloidal sol substrate is prepared；
Step 4, after mixing by gold nano colloidal sol substrate, prepare liquid and sodium-chloride water solution, Raman spectrum is carried out to adopt
Collection；
Step 5, the residual quantity of deltamethrin pesticide in strawberry is calculated according to following formula：
Y=0.0632x-14.103
In formula：Y is the residual quantity of deltamethrin pesticide, unit mg/kg；
X is 1000cm-1Locate Raman absorption peak intensity, unit a.u..
The present invention is using strawberry as carrier, and using benzimidazole germicide pesticide deltamethrin as research object, use is anhydrous
Magnesium sulfate, propyl ethylenediamine, C18 and graphitized charcoal black track producing particle remove the glimmering of the substances such as leaf, protein, fat, carbohydrate
Shadow is rung, and is used for quickly detecting to deltamethrin residues in strawberry using SERS technologies, to realize that Detecting Pesticide provides one
Quick, cheap, easy, the accurate detection scheme of kind.
In order to ensure being fully dissolved out for decis, it is preferable that in step 1, be attached with strawberry, the second of deltamethrin pesticide
The amount ratio of nitrile and sodium chloride is 2g：2mL：1g.In step 1, after vortex oscillation 1min, centrifuged under 10000r/min rotating speeds
2min obtains supernatant.
In order to ensure anhydrous magnesium sulfate, propyl ethylenediamine, C18 and graphitized charcoal black track producing particle removal protein, fat, carbon water
The effect of the substances such as compound, it is preferable that in step 2, anhydrous magnesium sulfate, propyl ethylenediamine, C18 and graphitized charcoal black track producing particle with
The amount ratio of supernatant is 300mg：1mL.It is further preferred that supplement：Anhydrous magnesium sulfate 150mg, propyl ethylenediamine 50mg,
C18 and Graphon 30mg；In step 2, after vortex oscillation 1min, 2min is centrifuged under 10000r/min rotating speeds, after centrifugation
Supernatant cross 0.22 μm of organic filter membrane after, obtain prepare liquid.
Preferably, step 3 prepares gold nano colloidal sol substrate using trisodium citrate heating reduction method.Gold nano colloidal sol base
Bottom can also use other modes to prepare, and can play Raman spectrum humidification, and do not influence target analyte detection.
Preferably, in step 4, the mass fraction of sodium-chloride water solution is 1%, gold nano colloidal sol substrate, prepare liquid and
The volume ratio of sodium-chloride water solution is 5：1：1.
Preferably, in step 4, the parameter of Raman spectrum acquisition is set as：Excitation wavelength 785nm, power 200mW, sweeps
Retouch 200~3300cm of range-1, optical resolution 2cm-1, time of integration 10s at least integrates and takes average spectral value 3 times.
Preferably, pre-processed to original spectral data using polynary scatter correction, needle position misalignment, random is eliminated
The interference of noise and background.
Compared with prior art, the present invention has the following advantages：
(1) surface Raman enhancement technology is applied to the remaining detection of deltamethrin pesticide in strawberry for the first time, be compared to
In traditional strawberry for the remaining detection of deltamethrin pesticide, accuracy of detection is high, and the time is short, easy to operate；
(2) model of the remaining actual value of deltamethrin pesticide in Raman absorption peak intensity and strawberry is established, it is quantitative to detect
Deltamethrin pesticide remains.
Description of the drawings
Fig. 1 is that the present invention is based on the flow charts that gold nano surface Raman enhancement detects the method for decis in strawberry；
Fig. 2 is decis schematic arrangement；
Fig. 3 is the micrograph of the gold nano substrate of TEM transmission electron microscopes characterization；
Fig. 4 is the remaining Surface enhanced Raman spectroscopy of deltamethrin pesticide in strawberry；
Scatter plots of the Fig. 5 between PLS predicted values and measured value, collects wherein (a) is modeling, is (b) forecast set；
Fig. 6 is the linear regression graph of deltamethrin pesticide concentration in Raman absorption peak and strawberry.
Specific implementation mode
With reference to embodiment and attached drawing, the present invention will be described in detail, but the present invention is not limited to this.
Flow chart according to figure 1, the method for decis includes the following steps in detection strawberry in the present embodiment：
Step 1,10g strawberries sample is weighed in 50mL centrifuge tubes, 10mL acetonitriles, 5g sodium chloride is sequentially added, after shaking up
Vortex oscillation mixes 1min, then centrifuges 2min under 10000r/min rotating speeds, obtains red supernatant.
Step 2,2mL green supernatants is taken to be put into equipped with anhydrous magnesium sulfate, propyl ethylenediamine, C18 and Graphon
In 15mL centrifuge tubes, after vortex oscillation mixes 1min, centrifuge 2min under 10000r/min rotating speeds, supernatant cross 0.22 μm it is organic
It is spare as prepare liquid after filter membrane.
In this step using anhydrous magnesium sulfate, propyl ethylenediamine, C18 and graphitized charcoal black track producing particle removal strawberry protein,
The fluorescence of the substances such as fat, carbohydrate influences.
Step 3, gold nano colloidal sol substrate is prepared, concrete operations are as follows：
Reduction method is heated using trisodium citrate, (10mg high gold chlorides are dissolved in by certain density high chlorauric acid solution
In 200mL ultra-pure waters) it pours into flask, it is placed in constant temperature blender with magnetic force, temperature control is heated to boiling 1200C is constant
Afterwards, it is rapidly added certain density citric acid three sodium solution (20mg trisodium citrates are dissolved in 4mL ultra-pure waters), while with 100rpm
Rotating speed quickly stirs, and the color of the aurosol being prepared into is claret after room temperature cooling, and above-mentioned appropriate gold size solution is poured into
A small amount of supernatant is outwelled in centrifuge tube, after centrifugation, then appropriate ultra-pure water is added into centrifuge tube, with sonic oscillation mixing, gold size
After repeatedly purifying, it is kept in dark place.The micrograph of the gold nano substrate of TEM transmission electron microscopes characterization is as shown in Figure 3.
Step 4, the gold nano substrate of 500 μ L steps 3 preparation is sequentially added in 2mL quartz bottles, prepared by 100 μ L steps 2
Prepare liquid, 100 μ L mass fractions be 1% sodium-chloride water solution, be put into mating liquid sample pool acquisition SERS spectra.
Before acquiring Raman spectrum data, rectified an instrument using acetonitrile.
The parameter of Raman spectrum acquisition is set as：Excitation wavelength 785nm, power 200mW, 200~3300cm of scanning range-1, optical resolution 2cm-1, time of integration 10s, integral takes average spectral value 3 times.
Step 5, the residual quantity of deltamethrin pesticide in strawberry is calculated according to following formula：
Y=0.0632x-14.103
In formula：Y is the residual quantity of deltamethrin pesticide, and unit is that (kg is the weight of strawberry to mg/kg, and mg is decis
The residual mass of pesticide)；
X is 1000cm-1Locate Raman absorption peak intensity, unit a.u..
Above-mentioned formula to establish process as follows：
(1) decis standard solution is prepared
950ml ultra-pure waters are added after 1000mg decis standard items are dissolved in 50mL acetonitriles, are made into 1000mg/
The decis standard solution of L is placed in 4 DEG C of light protected environments and stores, and decis schematic arrangement is as shown in Figure 2.
(2) deltamethrin pesticide in strawberry is simulated to remain
It chooses without pesticide strawberry, the decis standard solution of the 1000mg/L in step 1 is diluted to various concentration
Decis solution is sprayed, and concentration range is 0~100mg/L, concentration gradient 1mg/L, and simulation nature sprays 24 hours
Afterwards, picking strawberry is as experiment sample.
Experiment sample is 101 total, wherein 70 sample composition modeling collection, remaining 31 sample form forecast set.
(3) sample to be tested is prepared
By experiment sample using the processing of the method for step 1 and step 2, prepare liquid is obtained.
(4) method for utilizing step 3 prepares gold nano colloidal sol substrate, tests to obtain table using the parameter and method of step 4
Face enhances Raman spectrum, and for Surface enhanced Raman spectroscopy as shown in figure 4, x-axis is wave number in Fig. 4, y-axis is Raman absorption peak intensity.
(5) the remaining actual value of deltamethrin pesticide in high performance liquid chromatography detection strawberry is used
Prepare liquid prepared by 2mL steps (3) is added equipped with 150mg magnesium sulfate, 50mg N- propyl ethylenediamine (i.e.
Primary secondary amine, abbreviation PSA), in the 15mL centrifuge tubes of 10mg Graphons and 50mgC18 chromatographic columns,
After vortex oscillation mixes 2min, 2min is centrifuged under 10000r/min rotating speeds, takes supernatant 1mL in 10mL teat glass, nitrogen
After air-blowing is dry, 1mL ethyl acetate is added, vortex oscillation is crossed 0.22 μm of organic filter membrane, is positioned in 2mL sample injection bottles, using efficient
The remaining actual value of deltamethrin pesticide in liquid chromatographic detection strawberry.
(6) Pretreated spectra
The initial surface enhancing Raman spectrum that step (4) acquires is handled using preprocessing procedures, using more
First scatter correction pre-processes original spectral data, eliminates the interference of needle position misalignment, random noise and background.
(7) the true of deltamethrin pesticide in Raman spectrum absorption peak and strawberry is established using partial least-square regression method
The relationship model of value
Fig. 5 is modeling collection and the scatter plot between the predicted value and measured value of forecast set sample after first derivative processing.Fig. 5
In (a) be modeling collect, (b) be forecast set；X-axis is wave number, and y-axis is Raman absorption peak intensity.
Relationship model is the formula employed in step 6, the linear regression graph of formula as shown in fig. 6, formula correlation
Coefficients R2=0.98.
According to the disclosure and teachings of the above specification, those skilled in the art in the invention can also be to above-mentioned embodiment party
Formula carries out change and modification appropriate.Therefore, the invention is not limited in specific implementation modes disclosed and described above, to this
Some modifications and changes of invention should also be as falling into the scope of the claims of the present invention.In addition, although this specification
In used some specific terms, these terms are merely for convenience of description, does not limit the present invention in any way.
Claims (8)
1. a kind of method detecting decis in strawberry based on gold nano surface Raman enhancement, which is characterized in that including：
Step 1, strawberry, acetonitrile and the sodium chloride of deltamethrin pesticide will be attached with after mixing, carry out successively vortex oscillation,
Centrifugation, obtains supernatant；
Step 2, anhydrous magnesium sulfate, propyl ethylenediamine, C18 and Graphon are mixed with supernatant, and are vortexed successively
Oscillation, centrifugation, filtering, obtain prepare liquid；
Step 3, gold nano colloidal sol substrate is prepared；
Step 4, after mixing by gold nano colloidal sol substrate, prepare liquid and sodium-chloride water solution, Raman spectrum acquisition is carried out；
Step 5, the residual quantity of deltamethrin pesticide in strawberry is calculated according to following formula：
Y=0.0632x-14.103
In formula：Y is the residual quantity of deltamethrin pesticide, unit mg/kg；
X is 1000cm-1Locate Raman absorption peak intensity, unit a.u..
2. the method for detecting decis in strawberry based on gold nano surface Raman enhancement as described in claim 1, feature
It is, in step 1, the amount ratio for being attached with the strawberry of deltamethrin pesticide, acetonitrile and sodium chloride is 2g：2mL：1g.
3. the method for detecting decis in strawberry based on gold nano surface Raman enhancement as described in claim 1, feature
It is, in step 2, anhydrous magnesium sulfate, propyl ethylenediamine, C18 and the amount ratio of Graphon and supernatant are 300mg：
1mL。
4. the method for detecting decis in strawberry based on gold nano surface Raman enhancement as claimed in claim 3, feature
It is, anhydrous magnesium sulfate 150mg, propyl ethylenediamine 50mg, C18 and Graphon 30mg.
5. the method for detecting decis in strawberry based on gold nano surface Raman enhancement as described in claim 1, feature
It is, gold nano colloidal sol substrate is prepared using trisodium citrate heating reduction method in step 3.
6. the method for detecting decis in strawberry based on gold nano surface Raman enhancement as described in claim 1, feature
It is, in step 4, the mass fraction of sodium-chloride water solution is 1%, gold nano colloidal sol substrate, prepare liquid and sodium-chloride water solution
Volume ratio be 5：1：1.
7. the method for detecting decis in strawberry based on gold nano surface Raman enhancement as described in claim 1, feature
It is, in step 4, the parameter of Raman spectrum acquisition is set as：Excitation wavelength 785nm, power 200mW, scanning range 200~
3300cm-1, optical resolution 2cm-1, time of integration 10s at least integrates and takes average spectral value 3 times.
8. the method for detecting decis in strawberry based on gold nano surface Raman enhancement as described in claim 1, feature
Be, in step 4, original spectral data pre-processed using polynary scatter correction, eliminate needle position misalignment, random noise and
The interference of background.
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| CN109540866A (en) * | 2018-11-30 | 2019-03-29 | 泉州师范学院 | A kind of compound gold nano-material and preparation method thereof for Detecting Pesticide |
| CN109827948A (en) * | 2019-03-20 | 2019-05-31 | 苏州天际创新纳米技术有限公司 | A kind of rapid detection method of dithiocarbamate pesticide |
| CN110231329A (en) * | 2019-05-27 | 2019-09-13 | 河北伊诺光学科技股份有限公司 | Utilize the method for Fungicide residue in Raman enhanced spectrum detection food |
| CN111289491A (en) * | 2020-03-17 | 2020-06-16 | 浙江中烟工业有限责任公司 | Method for detecting triadimefon and triadimenol in tobacco based on surface enhanced Raman spectroscopy |
| CN111380850A (en) * | 2018-12-27 | 2020-07-07 | 普拉瑞思科学仪器（苏州）有限公司 | Surface enhanced Raman spectroscopy rapid detection method for chlorpyrifos and acetamiprid in vegetables |
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| CN111289491A (en) * | 2020-03-17 | 2020-06-16 | 浙江中烟工业有限责任公司 | Method for detecting triadimefon and triadimenol in tobacco based on surface enhanced Raman spectroscopy |
| CN111289491B (en) * | 2020-03-17 | 2023-03-10 | 浙江中烟工业有限责任公司 | Method for detecting triadimefon and triadimenol in tobacco based on surface enhanced Raman spectroscopy |
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