CN111380850A - Surface enhanced Raman spectroscopy rapid detection method for chlorpyrifos and acetamiprid in vegetables - Google Patents
Surface enhanced Raman spectroscopy rapid detection method for chlorpyrifos and acetamiprid in vegetables Download PDFInfo
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- CN111380850A CN111380850A CN201811612181.8A CN201811612181A CN111380850A CN 111380850 A CN111380850 A CN 111380850A CN 201811612181 A CN201811612181 A CN 201811612181A CN 111380850 A CN111380850 A CN 111380850A
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- 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
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Abstract
The invention discloses a surface-enhanced Raman spectroscopy rapid detection method of chlorpyrifos and acetamiprid in vegetables, which belongs to the technical field of food safety detection. The detection method provided by the invention prepares the pesticide residue purification powder, detects chlorpyrifos and acetamiprid in vegetables by using the surface enhanced Raman spectroscopy, and has the detection limits of 0.2ppm and 0.1ppm respectively, the sample pretreatment process is simple and convenient, the sample and reagent consumption is small, the detection is rapid and simple, the precision is high, and the cost is low.
Description
Technical Field
The invention belongs to the technical field of food safety detection, and particularly relates to a surface-enhanced Raman spectroscopy rapid detection method for chlorpyrifos and acetamiprid in vegetables.
Background
The chlorpyrifos is named as chlorpyrifos, lesonian, termite clear, chlorpyrifos and the like, has the triple effects of stomach toxicity, contact killing and fumigation, has better control effect on various chewing and piercing-sucking mouthpart pests on rice, wheat, cotton, fruit trees, vegetables and tea trees, and has wide insecticidal spectrum; belongs to toxic pesticide, and has high toxicity to fish and aquatic organisms.
Acetamiprid belongs to a nicotine chloride compound, is a novel pesticide, is named as acetamiprid, quick-acting pesticide and the like, has the characteristics of wide insecticidal spectrum, high activity, small dosage, long lasting effect, quick effect and the like, has the effects of contact poisoning and stomach poisoning, and has excellent systemic activity.
Chlorpyrifos and acetamiprid are commonly used pesticides in agricultural planting, are remained in agricultural products and food, and threaten health of people after eating, and the existing research and report mentions that the detection methods of the chlorpyrifos and the acetamiprid mainly comprise a resonance light scattering method, an enzyme linked immunosorbent assay kit, a nanogold colorimetric method, a fluorescence spectroscopy method and the like.
Therefore, a fast and simple method for detecting chlorpyrifos and acetamiprid, which can solve the above problems, is needed.
Disclosure of Invention
In order to overcome the defects of the existing detection method, the invention provides the surface enhanced Raman spectroscopy rapid detection method of chlorpyrifos and acetamiprid in vegetables.
The technical scheme provided by the invention is as follows.
A surface enhanced Raman spectroscopy rapid detection method for chlorpyrifos and acetamiprid in vegetables specifically comprises the following steps:
(1) adding 1g of sample to be detected into a 10mL centrifuge tube, adding 3mL of acetonitrile, oscillating for 20 s, and then carrying out ultrasonic treatment for 2 min;
(2) taking out 1mL of supernatant to a pesticide residue purification tube, oscillating until the supernatant is colorless, centrifuging for 10s, and layering, wherein the supernatant is a solution to be detected;
(3) 500ul of the enhanced reagent A, 50ul of the solution to be detected and 100ul of the enhanced reagent B are sequentially and uniformly mixed in a detection bottle, and the mixture is placed in a detection cell of a Raman spectrometer to start detection.
Preferably, the sample to be tested in the step (1) is the vegetable to be tested which is cut into a proper size.
Preferably, in the step (2), the pesticide residue purification tube is made of magnetic bead-magnesium sulfate-GCB graphitized carbon black mixed powder, and the mass ratio is 1: 4: 0.1, the centrifugal speed is 10000 r/min.
Preferably, in the step (3), the enhancing reagent A is self-made nanogold sol, and the enhancing reagent B is 0.2mol/L sodium chloride solution.
Preferably, in the step (3), the scanning parameters during detection by the Raman spectrometer are 200mW of laser power, 5 s of scanning time, 2 scanning times and 4 smooth parameters, and the chlorpyrifos positive spectrogram is 606/674cm-1The displacement has obvious Raman peak, the positive spectrogram of the acetamiprid is 630cm-1There is a distinct raman peak at the shift.
Preferably, the acetonitrile, water and the like used in the detection process are all chromatographically pure.
The invention has the beneficial effects that: the detection method provided by the invention is characterized in that the pesticide residue purification powder is prepared, a vegetable sample to be detected is extracted by acetonitrile, the supernatant is taken and put in a pesticide residue purification tube for oscillation, purification and centrifugation, the obtained supernatant to be detected is uniformly mixed with a proper amount of nano enhanced reagent A and enhanced reagent B, and then the mixture is detected by a Raman spectrometer, the detection limits of chlorpyrifos and acetamiprid are 0.2ppm and 0.1ppm respectively, and compared with the existing detection method, the detection method has the obvious advantages of simple and convenient sample pretreatment process, small sample and reagent dosage, quick and simple detection, high precision, low cost and the like.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention.
FIG. 1 is a surface enhanced Raman spectrum of chlorpyrifos in an example of the present invention.
Wherein, the grey dotted line spectrogram is a chlorpyrifos negative sample, and the black solid line spectrogram is a chlorpyrifos positive sample with the concentration of 0.5 ppm.
Detailed Description
The present invention will be described in further detail with reference to examples, but the present invention is not limited to the following examples.
A surface enhanced Raman spectroscopy rapid detection method for chlorpyrifos and acetamiprid in vegetables specifically comprises the following steps:
(1) preparing a chlorpyrifos negative vegetable sample, and preparing a proper amount of chlorpyrifos positive vegetable sample with the concentration of 0.5 ppm;
(2) adding 1g of sample to be detected into a 10mL centrifuge tube, adding 3mL of acetonitrile, oscillating for 20 s, and then carrying out ultrasonic treatment for 2 min;
(3) taking out 1mL of supernatant to a pesticide residue purification tube, oscillating until the supernatant is colorless, centrifuging at 10000 r/min for 10s for layering, and taking the supernatant as a solution to be detected;
(4) 500ul of the enhanced reagent A, 50ul of the solution to be detected and 100ul of the enhanced reagent B are sequentially and uniformly mixed in a detection bottle, the mixture is placed in a detection pool of a Raman spectrometer, and detection is started, wherein scanning parameters comprise 200mW of laser power, 5 s of scanning time, 2 scanning times and 4 smoothing parameters.
The detection result is shown in FIG. 1, wherein the grey dotted line spectrogram is a chlorpyrifos negative sample, the black solid line spectrogram is a chlorpyrifos positive sample with the concentration of 0.5ppm, and the chlorpyrifos positive spectrogram is 606cm-1The displacement has obvious Raman peak, which is obviously distinguished from the negative sample spectrogram.
Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art will understand that various changes, modifications and substitutions can be made without departing from the spirit and scope of the invention as defined by the appended claims. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (6)
1. A surface enhanced Raman spectroscopy rapid detection method for chlorpyrifos and acetamiprid in vegetables is characterized by comprising the following steps:
(1) adding 1g of sample to be detected into a 10mL centrifuge tube, adding 3mL of acetonitrile, oscillating for 20 s, and then carrying out ultrasonic treatment for 2 min;
(2) taking out 1mL of supernatant to a pesticide residue purification tube, oscillating until the supernatant is colorless, centrifuging for 10s, and layering, wherein the supernatant is a solution to be detected;
(3) 500ul of the enhanced reagent A, 50ul of the solution to be detected and 100ul of the enhanced reagent B are sequentially and uniformly mixed in a detection bottle, and the mixture is placed in a detection cell of a Raman spectrometer to start detection.
2. The method for rapidly detecting chlorpyrifos and acetamiprid in vegetables by surface enhanced Raman spectroscopy according to claim 1, wherein the sample to be detected in step (1) is a vegetable to be detected which is cut into pieces with appropriate size.
3. The surface-enhanced Raman spectroscopy rapid detection method for chlorpyrifos and acetamiprid in vegetables according to claim 1, wherein in the step (2), the pesticide residue purification tube is mixed powder of magnetic beads, magnesium sulfate and GCB graphitized carbon black, and the mass ratio is 1: 4: 0.1, the centrifugal speed is 10000 r/min.
4. The surface-enhanced Raman spectroscopy rapid detection method for chlorpyrifos and acetamiprid in vegetables according to claim 1, wherein the enhancing reagent A in step (3) is self-made nanogold sol, and the enhancing reagent B is 0.2mol/L sodium chloride solution.
5. The method for rapidly detecting chlorpyrifos and acetamiprid in vegetables by surface enhanced Raman spectroscopy according to claim 1, wherein scanning parameters of the Raman spectrometer in the step (3) are 200mW of laser power, 5 s of scanning time, 2 times of scanning and 4 of smoothing parameter, and a chlorpyrifos positive spectrogram is 606/674cm-1The displacement has obvious Raman peak, the positive spectrogram of the acetamiprid is 630cm-1There is a distinct raman peak at the shift.
6. The surface-enhanced Raman spectroscopy method for rapidly detecting chlorpyrifos and acetamiprid in vegetables according to claim 1, wherein acetonitrile, water and the like used in the detection process are all chromatographically pure.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104931483A (en) * | 2015-06-30 | 2015-09-23 | 北京工商大学 | Raman spectrum detection method for pesticide residues in fruits and vegetables |
| CN108613963A (en) * | 2018-05-17 | 2018-10-02 | 浙江大学 | A method of decis in strawberry is detected based on gold nano surface Raman enhancement |
| CN108693003A (en) * | 2018-04-26 | 2018-10-23 | 许昌学院 | A kind of method of leafy vegetable Detecting Pesticide sample pre-treatments |
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2018
- 2018-12-27 CN CN201811612181.8A patent/CN111380850A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104931483A (en) * | 2015-06-30 | 2015-09-23 | 北京工商大学 | Raman spectrum detection method for pesticide residues in fruits and vegetables |
| CN108693003A (en) * | 2018-04-26 | 2018-10-23 | 许昌学院 | A kind of method of leafy vegetable Detecting Pesticide sample pre-treatments |
| CN108613963A (en) * | 2018-05-17 | 2018-10-02 | 浙江大学 | A method of decis in strawberry is detected based on gold nano surface Raman enhancement |
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Application publication date: 20200707 |