CN105136773A - Method of rapidly detecting cyflumetofen by utilizing Raman spectra - Google Patents
Method of rapidly detecting cyflumetofen by utilizing Raman spectra Download PDFInfo
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- CN105136773A CN105136773A CN201510589705.6A CN201510589705A CN105136773A CN 105136773 A CN105136773 A CN 105136773A CN 201510589705 A CN201510589705 A CN 201510589705A CN 105136773 A CN105136773 A CN 105136773A
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- cyflumetofen
- raman spectrum
- spectrum analysis
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Abstract
The invention discloses a method of rapidly detecting cyflumetofen in food on the basis of Raman spectra, i.e. sample diluent and silver sol are mixed according to the volume ratio of 1 to 3, and an Raman spectrum analysis is performed, so that the cyflumetofen content in the food can be conveniently and rapidly detected by comparing with a standard curve. The detection method has the advantages of rapidity and simplicity in operation; in addition, onsite and outdoor real-time analyses can be realized by matching a handheld Raman analyzer.
Description
Technical field
The present invention relates to a kind of method utilizing Raman spectrum to detect cyflumetofen fast, specifically, is a kind of method adopting Surface enhanced raman spectroscopy to detect cyflumetofen fast.The invention belongs to organic substance detection technique field.
Background technology
Since the 1950's, chemical synthetic pesticide is widespread use worldwide, effectively decrease the loss that the harmful organisms such as disease, worm, grass bring to grain and other agricultural product, alleviate the mankind increase the staple food supply deficiency of generation rapidly pressure because of population.But, along with the application of chemical pesticide, inevitably create Pesticide Residue.Be present in the residues of pesticides in food and environment, together with other Harmful chemicals, cause food security and problems of ecological security, affect the healthy of the mankind, become the principal element affecting international agriculture trade, receive most attention and the concern of countries in the world government and consumer.
Cyflumetofen is the novel acaricide of benzoyl acetonitrile class developed by this great of mound chemical company, chemical name is (RS)-2-(4-t-butyl-phenyl)-2-itrile group-3-oxo-3-(a, a, the fluoro-o-tolyl of a-tri-) propionic acid-2-methoxyethyl ester, English name: cyflumetofen, is mainly used in the harmful mite preventing and treating the plants such as fruit tree, vegetables, tea, with existing pesticide without cross resistance, effective to two-spotted spider mite, especially higher to the activity of young mite.Due to its broad spectrum activity, be widely used in Japan at present.Due to its good insecticidal effect and not easily produce the feature such as resistance, be also about to be used by China's registration.But along with a large amount of uses of cyflumetofen, may exist residual to target crop and environment thus environment and human health are impacted.Especially cyflumetofen metabolic conversion can become complicated metabolic product in the environment.Because o-trifluoromethyl benzamide (B-3) in main metabolites is large to mammalian toxicity, o-trifluoromethyl benzoic acid (B-1) difficult degradation, has potential risks to environment and the mankind.
Current pesticide residue detection method is mainly divided three classes: biometric techniques, Physico-chemical tests method and fast detection method.Biometric techniques requires higher to indicator organism, and measurement result can not determine pesticide species; Though Physico-chemical tests method precision is high, but the loaded down with trivial details and length consuming time of operating process, the needs of on-line checkingi can not be met.The mensuration of cyflumetofen commonly uses the method such as gas phase, liquid-phase chromatographic analysis, time-consuming and can not realize on-line determination, and needs complicated sample pretreatment process.Fast detection method is as very fast in the development such as inhibiting AChE, immune fast detection method, biosensor technology in recent years, but these methods also exist the low or high in cost of production problem of sensitivity.Therefore, realizing cyflumetofen residual quick, harmless, real-time online detection is our problem demanding prompt solution.
This invention exploits one and utilize Raman spectrum, the method for cyflumetofen in express-analysis food.Raman spectrum analysis because of economical, simply, feature fast, apply more and more extensive in recent years in the analysis of pesticide sample.Because Raman spectrum is vibrational spectrum, the nuance of the structure of matter can both reflect from the difference of its vibrational spectrum, detects pesticide residue therefore, it is possible to analyze accurately.At present, according to our understanding, also do not apply the research report of Raman spectrum express-analysis cyflumetofen.In addition, do not find to ask identical publication or granted patent with this patent protection with U.S.Patent & Trademark Office (www.uspto.gov) through retrieval data center of State Intellectual Property Office (www.sipo.gov.cn), World Intellectual Property Organization (www.wipo.int), EUROPEAN PATENT OFFICE (www.espacenet.com) yet.
Summary of the invention
The object of this invention is to provide a kind of method adopting Raman spectrum to detect cyflumetofen in food fast.Compare with existing technology, this method measures quick, simple to operate.In addition utilize handheld Raman spectrometer, adopt real-time, quick, the Accurate Determining that method of the present invention can realize scene easily, outdoor cyflumetofen remains.
The present invention is a kind of method utilizing Raman spectrum to detect cyflumetofen fast, it is characterized in that, has following process and step:
A, the preparation of nano silver colloidal sol
By 200ml, 0.02% liquor argenti nitratis ophthalmicus be heated to 140 DEG C in advance, then add fast 2ml, 1% trisodium citrate aqueous solution, 140 DEG C, reaction after 15 minutes under the condition that stirs, be cooled to rapidly room temperature obtain needed for Nano sol; The Nano sol prepared becomes faint yellow, and Nano sol keeps in Dark Place at being put in 4 DEG C before use, for subsequent use;
B, by experiment production standard curve
The cyflumetofen solution of various criterion concentration (0.02-200ppm) is carried out Raman spectrum analysis (500-1800cm
-1wave number); Obtain the cyflumetofen characteristic peak (1029cm of various criterion cyflumetofen solution
-1) with the normal linearity relation curve of corresponding cyflumetofen concentration;
C, carries out Raman spectrum analysis by pretreating specimen
After 1:3 mixes by volume with silver sol (3mL) by fluid sample (1mL), carry out Raman spectrum analysis, then obtain the content of cyflumetofen in sample according to the peak height reference standard curve of cyflumetofen characteristic peak quickly and accurately;
Described Raman spectrum analysis condition is: Raman spectroscopy scans scope is 500-1800cm
-1wave-number range; Obtain Raman spectrum raw data, deduction is except the quantitative test for cyflumetofen content after fluorescence background;
The characteristic peak of described cyflumetofen is 1029cm
-1.
Accompanying drawing explanation
Fig. 1 is normal Raman and the surface-enhanced Raman collection of illustrative plates of different cyflumetofen.Wherein a is the normal Raman spectroscopy figure of 200ppm cyflumetofen; B is 200ppm cyflumetofen Surface enhanced raman spectroscopy figure; C is the normal Raman spectroscopy figure of 20% cyflumetofen.
Fig. 2 is the Surface enhanced raman spectroscopy figure of the cyflumetofen of variable concentrations.(concentration is followed successively by from top to bottom: 200,100,20,2,0.2,0.02,0ppm).
Fig. 3 is the linear relationship chart of cyflumetofen concentration and surface-enhanced Raman characteristic peak peak height.Figure cathetus is the linear regression line of cyflumetofen concentration and its feature peak height.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail.
Embodiment
In embodiment, detecting step is as described below:
1, the preparation of nano silver colloidal sol
By 200ml, 0.02% liquor argenti nitratis ophthalmicus be heated to 140 DEG C in advance, then add fast 2ml, 1% trisodium citrate aqueous solution, 140 DEG C, reaction after 15 minutes under the condition that stirs, be cooled to rapidly room temperature obtain needed for Nano sol.The Nano sol prepared becomes faint yellow, and Nano sol keeps in Dark Place at being put in 4 DEG C before use, for subsequent use.Under 4 DEG C of conditions that keep in Dark Place, in three months, silver nanoparticle colloidal sol Absorbable organic halogens uses.
2, the detection of cyflumetofen
The cyflumetofen solution of various criterion concentration (0.02-200ppm) is carried out Raman spectrum analysis (500-1800cm
-1wave number).Obtain the cyflumetofen characteristic peak (1029cm of various criterion cyflumetofen solution
-1) with the normal linearity relation curve of corresponding cyflumetofen concentration.Pretreatment sample and silver sol solution are pressed 1:3 volume mixture evenly after, carry out Raman spectrum analysis, then obtain the content of cyflumetofen according to cyflumetofen characteristic peak peak height reference standard curve quickly and accurately.
Described pretreatment sample can adopt Different treatments according to determinand difference, and the processes such as fruits and vegetables etc. can grind, centrifugal obtain supernatant; Liquid food directly dilutes sampling.
feature for the present invention
1,1029cm
-1for the characteristic peak of cyflumetofen.
2, the cyflumetofen concentration in solution and the peak height of its characteristic peak have extraordinary linear relationship.
accompanying drawing for the present invention and Raman spectrum spectrum elucidation
A, interpretation about Fig. 1
As shown in Figure 1, Fig. 1 is normal Raman and the surface-enhanced Raman collection of illustrative plates of different cyflumetofen.Wherein a is the normal Raman spectroscopy figure of 200ppm cyflumetofen; B is 200ppm cyflumetofen Surface enhanced raman spectroscopy figure; C is 20% cyflumetofen normal Raman spectroscopy figure.Each solution is in 500-1800cm above
-1the Raman spectrum spectrogram obtained in scope.Can find out in accompanying drawing 1c, although cyflumetofen has many peaks, 1029cm
-1characteristic peak signal is the strongest; Further as can be seen from the result of accompanying drawing 1b also, the 1029cm of cyflumetofen
-1characteristic peak not by background interference, can be directly used in the content analysis of cyflumetofen completely in Raman enhancing matrix; And contrast accompanying drawing 1a and 1b, the 1029cm of silver sol to cyflumetofen can be found out
-1it is very remarkable that characteristic peak strengthens effect.
B, about the drafting of Fig. 2, Fig. 3 and interpretation
The aqueous solution of preparation variable concentrations cyflumetofen.Wherein the concentration of cyflumetofen be respectively 0.02,0.2,2,20,100,200ppm.Get above-mentioned 6 kinds of solution respectively to mix, in 500-1800cm with the volume ratio of 1:3 with silver sol
-1obtain Surface enhanced raman spectroscopy in wave-number range, after spectral data deduction fluorescence background, see accompanying drawing 2.Cyflumetofen concentration in the peak height of cyflumetofen characteristic peak in each solution surface enhancing Raman spectrum and solution is mapped and sees accompanying drawing 3.
As can be seen from accompanying drawing 3, the peak height of cyflumetofen characteristic peak (
y) with solution in cyflumetofen concentration (
x) there is good correlativity.Dependent equation is
y=2E+06
x+ 2051, related coefficient is 0.9698.The cyflumetofen of the method detects and is limited to 0.01ppm.
Claims (1)
1. utilize Raman spectrum to detect a method for cyflumetofen fast, it is characterized in that, there is following process and step:
A, the preparation of nano silver colloidal sol
By 200ml, 0.02% liquor argenti nitratis ophthalmicus be heated to 140 DEG C in advance, then add fast 2ml, 1% trisodium citrate aqueous solution, 140 DEG C, reaction after 15 minutes under the condition that stirs, be cooled to rapidly room temperature obtain needed for Nano sol; The Nano sol prepared becomes faint yellow, and Nano sol keeps in Dark Place at being put in 4 DEG C before use, for subsequent use;
B, by experiment production standard curve
The cyflumetofen solution of various criterion concentration (0.02-200ppm) is carried out Raman spectrum analysis (500-1800cm
-1wave number); Obtain the cyflumetofen characteristic peak (1029cm of various criterion cyflumetofen solution
-1) with the normal linearity relation curve of corresponding cyflumetofen concentration;
C, carries out Raman spectrum analysis by pretreating specimen
After 1:3 mixes by volume with silver sol (3mL) by fluid sample (1mL), carry out Raman spectrum analysis, then obtain the content of cyflumetofen in sample according to the peak height reference standard curve of cyflumetofen characteristic peak quickly and accurately;
Described Raman spectrum analysis condition is Raman spectroscopy scans scope is 500-1800cm
-1wave-number range; Obtain Raman spectrum raw data, deduction is except the quantitative test for cyflumetofen content after fluorescence background;
The characteristic peak of described cyflumetofen is 1029cm
-1.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108548805A (en) * | 2018-03-05 | 2018-09-18 | 华南理工大学 | The method that nano silver colloidal sol quenching fluorescence is used in Raman spectrum |
| CN110231326A (en) * | 2018-03-06 | 2019-09-13 | 江苏师范大学 | The residual detection qualitative-and-quantitative method of Amitraz agriculture in a kind of efficiently honey |
| CN112213292A (en) * | 2020-08-19 | 2021-01-12 | 杭州健澄科技有限公司 | Method for detecting hydroxylamine content in oximation reaction process |
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|---|---|---|---|---|
| US20110285992A1 (en) * | 2008-12-17 | 2011-11-24 | Board Of Trustees Of The University Of Arkansas | Methods of fabricating surface enhanced raman scattering substrates |
| CN102313730A (en) * | 2011-08-11 | 2012-01-11 | 江南大学 | Surface enhanced Raman scattering rapid screening method for methamidophos in vegetable |
| US20120028372A1 (en) * | 2010-07-27 | 2012-02-02 | Thomas Yong-Jin Han | Rapid detection and identification of energetic materials with surface enhanced raman spectrometry (sers) |
| CN104101591A (en) * | 2014-07-24 | 2014-10-15 | 江西农业大学 | Fast detection method for surface enhanced Raman scattering of trace pesticide residues in oranges |
| CN104142321A (en) * | 2014-07-24 | 2014-11-12 | 江西农业大学 | Method for fast detecting surface enhancing Raman spectrums of pesticide residues in tea leaves |
-
2015
- 2015-09-17 CN CN201510589705.6A patent/CN105136773A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110285992A1 (en) * | 2008-12-17 | 2011-11-24 | Board Of Trustees Of The University Of Arkansas | Methods of fabricating surface enhanced raman scattering substrates |
| US20120028372A1 (en) * | 2010-07-27 | 2012-02-02 | Thomas Yong-Jin Han | Rapid detection and identification of energetic materials with surface enhanced raman spectrometry (sers) |
| CN102313730A (en) * | 2011-08-11 | 2012-01-11 | 江南大学 | Surface enhanced Raman scattering rapid screening method for methamidophos in vegetable |
| CN104101591A (en) * | 2014-07-24 | 2014-10-15 | 江西农业大学 | Fast detection method for surface enhanced Raman scattering of trace pesticide residues in oranges |
| CN104142321A (en) * | 2014-07-24 | 2014-11-12 | 江西农业大学 | Method for fast detecting surface enhancing Raman spectrums of pesticide residues in tea leaves |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108548805A (en) * | 2018-03-05 | 2018-09-18 | 华南理工大学 | The method that nano silver colloidal sol quenching fluorescence is used in Raman spectrum |
| CN110231326A (en) * | 2018-03-06 | 2019-09-13 | 江苏师范大学 | The residual detection qualitative-and-quantitative method of Amitraz agriculture in a kind of efficiently honey |
| CN112213292A (en) * | 2020-08-19 | 2021-01-12 | 杭州健澄科技有限公司 | Method for detecting hydroxylamine content in oximation reaction process |
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Application publication date: 20151209 |