CN105784669A - Method for rapid in-situ detection of object surface pollutants - Google Patents
Method for rapid in-situ detection of object surface pollutants Download PDFInfo
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- 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
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Abstract
A method for rapid in-situ detection of object surface pollutants is characterized in that a flexible and semi-transparent surface enhanced Raman substrate is used and is composed of a Raman active nanoparticle assembly body and a flexible polymer; by a way that the substrate is directly affixed to the surface of an object to be detected, or the substrate is rubbed back and forth on the surface of the object to be detected, or the substrate is coiled into a capillary, the adsorption and enrichment capacity of the substrate on the pollutants on the surface of the object to be detected is enhanced, then the on-site rapid in-situ detection of the pollutants on the surface of the object is achieved by a surface enhancing Raman technique. Compared with other detection methods, the method is simple, rapid, low in cost, and beneficial for on-site casual inspection, and has wide application prospects in the fields of environmental monitoring, food safety, medical treatment and health care and the like.
Description
Technical field
A kind of detection method is related to, the method especially relating to a kind of quick in situ detection body surface pollutant in invention.
Background technology
In recent years, environmental pollution is day by day serious, and wherein residue problem poisonous, harmful pollutants is especially prominent.The pesticide of fruit and Folium Camelliae sinensis remained on surface in agricultural product, the illegal malachite green oxalate added and crystal violet etc., all health of the serious threat mankind in aquaculture.At present, the detection method of residual contaminants mainly has high performance liquid chromatography, gas chromatography and inhibiting AChE etc..Although, these method accuracy of detection are high, identify accurately, but the cost of loaded down with trivial details sample pre-treatments, detection cycle consuming time and costliness, all seriously hinder their popularization and application, especially difficult for on-the-spot quickly sampling observation.Therefore, a kind of simplicity of development, low cost, high-sensitive pollutant quick in situ detection method have great importance.
Raman spectrum is as a kind of molecular vibration spectrum technology, different material can be differentiated on a molecular scale, there is numerous advantage (as without labelling, without complex sample pretreatment, precisely provide molecular chemistry information, detection cycle short and water interference is little etc.) in pollutant monitoring, but normal Raman spectrum is weak due to signal, the Raman signal of a lot of materials is difficult to detect, and causes that its application is extremely limited.When surface enhanced raman spectroscopy (Surface-EnhancedRamanScattering, SERS) refers to when test substance absorption or is close to the metallic nanostructured surface such as gold, silver, copper, its Raman signal can obtain the enhancing of more than million times.Therefore, SERS not only has the advantage of normal Raman spectrum, and has superelevation detection sensitivity, even up to Single Molecule Detection level.
At present, the body surface contamination detection method based on SERS is relatively cumbersome, is usually first with the pollutant on organic solvent extraction detected material surface, is then added drop-wise to by extract in SERS substrate, detects after solvent volatilizees again.This is because existing SERS substrate is mostly the supporting layer adopting some hard materials, such as silicon chip, quartz and electro-conductive glass etc..These hard substrates do not have flexibility, it is difficult to carry out in situ detection directly against being combined in irregularity surface.Although there being a small amount of SERS substrate to adopt the supporting layer of flexible material, such as cellulose paper, light tight polymer and CNT etc., but owing to these flexible support layers are light tight, laser is difficult to pass through supporting layer, it is impossible to excite the Raman signal of pollutant.Therefore, it is impossible to realize the quick in situ detection of body surface pollutant.
Development has flexibility, semi-transparent SERS substrate, is realize SERS technology to be applied to the key of body surface pollutant quick in situ detection.Flexible SERS substrate can make it be close to the body surface of irregular pattern so that body surface pollutant and SERS substrate as close possible to, to obtain higher Raman enhancement effect；Semi-transparency then can make laser pass through SERS supporting layer, arrives SERS active layer and pollutant surface, it is achieved the activation of pollutant Raman signal and enhancing.
In order to promote this technology extensive use, research and development low cost, highly sensitive, the flexibility of high intensity, semi-transparent SERS substrate are cores.Additionally, for the sensitivity improving detection further, the detection mode of Development of Novel also has great importance.
Summary of the invention
Solve above-mentioned technical problem, the method that the invention discloses a kind of quick in situ detection body surface pollutant, the method can without sample pretreatment, easy, quickly, the detection realizing body surface pollutant of original position, low cost, it is very suitable for on-the-spot quickly sampling observation, in environmental monitoring, there is extremely wide application prospect in the field such as food safety and health care.
The present invention utilizes flexibility and the semi-transparency of surface enhanced Raman substrate, is placed directly against body surface, or increases the substrate adsorption and enrichment to pollutant by friction back and forth, improves detection sensitivity, it is achieved the quick in situ detection of body surface pollutant.
The present invention utilizes flexibility and the semi-transparency of surface enhanced Raman substrate, it is rolled into capillary tube, by capillary force or additional suction, the pollutant of adsorption and enrichment body surface, produce higher SERS enhancement effect by curling Raman substrate simultaneously, improve detection sensitivity, it is achieved the quick in situ detection of body surface pollutant.
The present invention utilizes the stability and intensity that surface enhanced Raman substrate is good, by substrate is carried out, reduces its background signal, by substrate is modified, strengthens its adsorption and enrichment ability to pollutant, improves its detection sensitivity.
Surface enhanced Raman substrate of the present invention, it is made up of Raman-active nano-particles assembly and flexible polymer, by simply changing experiment parameter, it may be achieved the regulation and control to nanoparticle assemblies structure and polymer content so that it is meet the different demands in application.
Described surface enhanced Raman substrate preparation method has following two:
The first prepares scheme:
1) building profit system, wherein oil phase is the organic solvent containing polymer, and aqueous phase is Raman-active nano-particles aqueous solution.Polymer includes that polyamide, Merlon, polymethyl methacrylate, polydimethylsiloxane, polyurethane, urethaneureas, polrvinyl chloride, polyethylene terephthalate, polystyrene, poly-D-lysine, polysulfones and polyether sulfone etc. are therein a kind of or their mixture, and modifier.Organic solvent includes one therein or its mixed liquors such as benzene, hexamethylene, Ketohexamethylene, amylalcohol, ether, carbon tetrachloride, chloroform.Raman-active nano-particles is that nanometer gold, silver, copper etc. is therein a kind of or their mixture, and composite construction；
2) stirred by stirrer or ultrasonic, promote Raman-active nano-particles to be self-assembly of Nanoscale assemblies at oil-water interfaces；
3) after organic solvent volatilizees, the polymer in organic solvent will form a thin film, and nanoparticle assemblies is fixed, and ultimately form and have flexibility, semi-transparent surface enhanced Raman substrate.
The second prepares scheme:
1) profit system is built, the polymer wherein contained in oil phase or aqueous phase.Polymer includes that polyamide, Merlon, polymethyl methacrylate, polydimethylsiloxane, polyurethane, urethaneureas, polrvinyl chloride, polyethylene terephthalate, polystyrene, poly-D-lysine, Polyetherimide, polysulfones, polyether sulfone, Polyethylene Glycol, chitosan and polyvinyl alcohol etc. are therein a kind of or their mixture, and polymer-modified；Organic solvent includes one therein or its mixed liquors such as toluene, hexamethylene, Ketohexamethylene, amylalcohol, ether, carbon tetrachloride, chloroform；
2) will the Raman-active nano-particles solution of concentration, be expelled to oil-water interfaces, and form nanoparticle assemblies, wherein Raman-active nano-particles is that nanometer gold, silver, copper etc. is therein a kind of or their mixture, and composite construction；
3) after oil phase or aqueous phase volatilize, oil phase or the polymer in aqueous phase will form a thin film in interface, and nanoparticle assemblies is fixed, and ultimately form and have flexibility, semi-transparent surface enhanced Raman substrate.
The invention have the advantage that
1) present invention can realize the on-the-spot quick in situ detection of body surface pollutant.
2) compared to other detection method, the method is simple, quickly, low cost, be easy to spot sampling check.
Accompanying drawing explanation
Fig. 1 is under embodiment 1 condition, obtained flexibility, the optical photograph figure of semi-transparent surface enhanced Raman substrate.
Fig. 2 is under embodiment 2 condition, at the optical photograph figure of the nanometer gold assembly that oil-water interfaces are self-assembly of.
Fig. 3 is under embodiment 3 condition, is rubbed back and forth at apple surface by flexible, semi-transparent surface enhanced Raman substrate, the optical photograph figure of detection remained on surface pesticide.
Fig. 4 is under embodiment 4 condition, and flexible, semi-transparent surface enhanced Raman substrate is curled into capillary tube, the optical photograph figure of detection apple surface residual pesticide.
Specific implementation method:
Technical scheme is further described below in conjunction with embodiment below in conjunction with reality (executing case) example.
Embodiment 1:
1) first take the nanometer silver gold filled particle solution of the fresh preparation of 15ml in 25mL beaker, and put into rotor；
2) then 3ml is contained toluene and the cyclohexanone mixed solution of 5% polystyrene, is added on nanometer silver gold filled particle solution, form oil-water interfaces；
3) by rotor gentle agitation nanometer silver gold filled particle solution, make nanometer silver gold filled particle float to oil-water interfaces, and be self-assembled into assembly；
4), after treating upper strata organic solvent volatilization, the polystyrene film containing Nanoscale assemblies is taken out, finally gives flexibility, semi-transparent surface enhanced Raman substrate.
Embodiment 2:
1) 15ml aqueous solution is first taken in 25mL beaker；
2) then 3ml is contained the cyclohexane solution of 5% polymethyl methacrylate, is added on aqueous solution, form oil-water interfaces；
3) then the nanometer gold alcoholic solution of concentration is slowly expelled to oil-water interfaces place, forms nanometer gold assembly；
4), after treating upper strata thiacyclohexane volatilization, the polymethyl methacrylate film containing nanometer gold assembly is taken out, finally gives flexibility, semi-transparent surface enhanced Raman substrate.
Embodiment 3:
1) first by flexibility prepared in embodiment 1, semi-transparent surface enhanced Raman substrate, it is immersed in 1mM sulfhydrylation beta-schardinger dextrin-solution 5 hours；
2) then clean substrate with deionized water, be attached to apple surface after cleaning, and rub back and forth, increase the substrate accumulation ability to pollutant；
3) it is then used by Portable Raman spectrometer, to the Fructus Mali pumilae place posting surface enhanced Raman substrate, carries out Raman spectroscopy scans；
4) Raman signal obtained finally by detection, it is judged that whether apple surface exists the pollutant such as pesticide.
Embodiment 4:
1) first by flexibility prepared in embodiment 1, semi-transparent surface enhanced Raman substrate, it is immersed in 1mM sulfhydrylation beta-schardinger dextrin-solution 5 hours；
2) then clean substrate with deionized water, after cleaning, be curled into capillary tube, the pollutant of adsorption and enrichment apple surface；
3) it is then used by Portable Raman spectrometer, the most advanced and sophisticated place to capillary tube, carry out Raman spectroscopy scans；
4) Raman signal obtained finally by detection, it is judged that whether apple surface exists the pollutant such as pesticide.
Although specifically showing in conjunction with preferred embodiment and describing the present invention; but those skilled in the art should be understood that; in the spirit and scope without departing from appended claims invention defined; the present invention can be made a variety of changes in the form and details, be protection scope of the present invention.
Claims (9)
1. the method for quick in situ detection body surface pollutant, it is characterized in that using flexible, semi-transparent surface enhanced Raman substrate, this substrate is made up of Raman-active nano-particles assembly and flexible polymer, by this substrate is directly affixed on detected material surface, maybe substrate is rubbed back and forth by this on detected material surface, maybe substrate is rolled into the modes such as capillary tube by this, strengthen the substrate adsorption and enrichment ability to detected material surface contaminant, then pass through surface enhanced Raman technique, it is achieved the on-the-spot quick in situ detection of body surface pollutant.
2. the method for a kind of quick in situ as claimed in claim 1 detection body surface pollutant, it is characterised in that the preparation method of described surface enhanced Raman substrate flexible, semi-transparent is as follows:
1) building profit system, wherein oil phase is the organic solvent containing polymer, and aqueous phase is Raman-active nano-particles aqueous solution；Polymer includes that polyamide, Merlon, polymethyl methacrylate, polydimethylsiloxane, polyurethane, urethaneureas, polrvinyl chloride, polyethylene terephthalate, polystyrene, poly-D-lysine, polysulfones and polyether sulfone etc. are therein a kind of or their mixture, and modifier；Organic solvent includes one therein or its mixed liquors such as benzene, hexamethylene, Ketohexamethylene, amylalcohol, ether, carbon tetrachloride, chloroform；Raman-active nano-particles is that nanometer gold, silver, copper etc. is therein a kind of or their mixture, and composite construction；
2) stirred by stirrer or ultrasonic, promote Raman-active nano-particles to be self-assembly of Nanoscale assemblies at oil-water interfaces；
3) after organic solvent volatilizees, the polymer in organic solvent will form a thin film, and nanoparticle assemblies is fixed, and ultimately form and have flexibility, semi-transparent surface enhanced Raman substrate.
3. the method for a kind of quick in situ as claimed in claim 1 detection body surface pollutant, it is characterised in that the preparation method of described surface enhanced Raman substrate flexible, semi-transparent also can be as follows:
1) profit system is built, the polymer wherein contained in oil phase or aqueous phase；Polymer includes that polyamide, Merlon, polymethyl methacrylate, polydimethylsiloxane, polyurethane, urethaneureas, polrvinyl chloride, polyethylene terephthalate, polystyrene, poly-D-lysine, Polyetherimide, polysulfones, polyether sulfone, Polyethylene Glycol, chitosan and polyvinyl alcohol etc. are therein a kind of or their mixture, and polymer-modified；Organic solvent includes one therein or its mixed liquors such as toluene, hexamethylene, Ketohexamethylene, amylalcohol, ether, carbon tetrachloride, chloroform；
2) will the Raman-active nano-particles solution of concentration, be expelled to oil-water interfaces, and form nanoparticle assemblies, wherein Raman-active nano-particles is that nanometer gold, silver, copper etc. is therein a kind of or their mixture, and composite construction；
3) after oil phase or aqueous phase volatilize, oil phase or the polymer in aqueous phase will form a thin film in interface, and nanoparticle assemblies is fixed, and ultimately form and have flexibility, semi-transparent surface enhanced Raman substrate.
4. the method for a kind of quick in situ as claimed in claim 1 detection body surface pollutant, it is characterized in that in flexible, semi-transparent surface enhanced Raman substrate, Raman-active nano-particles assembly is to be shunk by polymer physics to fix, there is good stability and intensity, various cleaning, modification etc. can be carried out, and do not destroy its structure.
5. the method for a kind of quick in situ as claimed in claim 1 detection body surface pollutant, it is characterized in that in flexible, semi-transparent surface enhanced Raman substrate, the structure of Raman-active nano-particles assembly and the content of polymer are prone to regulation and control, it is simple to meet different detection demand.
6. the method for a kind of quick in situ as claimed in claim 1 detection body surface pollutant, it is characterized in that before detection, flexible, semi-transparent surface enhanced Raman substrate can be carried out plasma treatment, strengthen the degree of exposure of Raman-active nano-particles assembly and the roughness of substrate, improve detection sensitive.
7. the method for a kind of quick in situ as claimed in claim 1 detection body surface pollutant, it is characterized in that in detection process, flexible, semi-transparent surface enhanced Raman substrate can be rolled into capillary tube, by capillary force or additional suction, the pollutant of adsorption and enrichment body surface, improve detection sensitive.
8. the method for a kind of quick in situ as claimed in claim 1 detection body surface pollutant, it is characterized in that before detection, it is prone to flexible, semi-transparent surface enhanced Raman substrate is modified, strengthen the Raman substrate adsorption and enrichment ability to pollutant, improve detection sensitivity, wherein decorating molecule comprises cyclodextrin and derivant thereof, enzyme, aptamers etc..
9. the method for a kind of quick in situ as claimed in claim 4 detection body surface pollutant, it is characterised in that the preparation process of flexible, semi-transparent surface enhanced Raman substrate, it is not necessary to add ethanol, simplifies step, reduces cost.
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| CN108982466A (en) * | 2018-06-06 | 2018-12-11 | 上海应用技术大学 | A method of for antibiotic field quick detection in Amoxicillin in water body |
| CN109142319A (en) * | 2018-10-31 | 2019-01-04 | 大连民族大学 | A kind of field fast detection method of shellfish aquatic products surface malachite green |
| CN109294234A (en) * | 2018-09-26 | 2019-02-01 | 北京市政建设集团有限责任公司 | It is a kind of reusable based on graphene-noble metal nano particles compound hybrid film and preparation method thereof |
| CN109799223A (en) * | 2019-03-09 | 2019-05-24 | 湖北工业大学 | For detecting the Raman substrate and detection method of Acrylamide in Foods and bisphenol-A |
| CN109813692A (en) * | 2019-01-02 | 2019-05-28 | 北京科技大学 | A kind of capillary analysis detection method based on ultrasound aggregation |
| CN109900674A (en) * | 2019-03-15 | 2019-06-18 | 深圳华中科技大学研究院 | A kind of nanogold array surface enhancing Raman chip and the preparation method and application thereof |
| TWI678527B (en) * | 2017-09-08 | 2019-12-01 | 鴻海精密工業股份有限公司 | Method for detecting molecular |
| US10533948B2 (en) | 2017-09-08 | 2020-01-14 | Tsinghua University | Carrier for use in single molecule detection |
| US10641699B2 (en) | 2017-09-08 | 2020-05-05 | Tsinghua University | Method of making a carrier for molecular detection |
| CN111289493A (en) * | 2020-03-27 | 2020-06-16 | 电子科技大学 | Surface-enhanced Raman substrate and preparation method thereof |
| US10859501B2 (en) | 2017-09-08 | 2020-12-08 | Tsinghua University | Carrier for use in single molecule detection |
| US11112364B2 (en) | 2017-09-08 | 2021-09-07 | Tsinghua University | Molecular detection device |
| CN113970538A (en) * | 2021-09-16 | 2022-01-25 | 深圳网联光仪科技有限公司 | Pathogen detection method |
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| US10852241B2 (en) | 2017-09-08 | 2020-12-01 | Tsinghua University | Method for detecting molecular |
| US11112364B2 (en) | 2017-09-08 | 2021-09-07 | Tsinghua University | Molecular detection device |
| US10859501B2 (en) | 2017-09-08 | 2020-12-08 | Tsinghua University | Carrier for use in single molecule detection |
| TWI678527B (en) * | 2017-09-08 | 2019-12-01 | 鴻海精密工業股份有限公司 | Method for detecting molecular |
| US10533948B2 (en) | 2017-09-08 | 2020-01-14 | Tsinghua University | Carrier for use in single molecule detection |
| US10641699B2 (en) | 2017-09-08 | 2020-05-05 | Tsinghua University | Method of making a carrier for molecular detection |
| CN108982466A (en) * | 2018-06-06 | 2018-12-11 | 上海应用技术大学 | A method of for antibiotic field quick detection in Amoxicillin in water body |
| CN109294234A (en) * | 2018-09-26 | 2019-02-01 | 北京市政建设集团有限责任公司 | It is a kind of reusable based on graphene-noble metal nano particles compound hybrid film and preparation method thereof |
| CN109142319A (en) * | 2018-10-31 | 2019-01-04 | 大连民族大学 | A kind of field fast detection method of shellfish aquatic products surface malachite green |
| CN109813692A (en) * | 2019-01-02 | 2019-05-28 | 北京科技大学 | A kind of capillary analysis detection method based on ultrasound aggregation |
| CN109799223A (en) * | 2019-03-09 | 2019-05-24 | 湖北工业大学 | For detecting the Raman substrate and detection method of Acrylamide in Foods and bisphenol-A |
| CN109900674A (en) * | 2019-03-15 | 2019-06-18 | 深圳华中科技大学研究院 | A kind of nanogold array surface enhancing Raman chip and the preparation method and application thereof |
| CN111289493A (en) * | 2020-03-27 | 2020-06-16 | 电子科技大学 | Surface-enhanced Raman substrate and preparation method thereof |
| CN111289493B (en) * | 2020-03-27 | 2021-08-06 | 电子科技大学 | Surface-enhanced Raman substrate and preparation method thereof |
| CN113970538A (en) * | 2021-09-16 | 2022-01-25 | 深圳网联光仪科技有限公司 | Pathogen detection method |
| CN113970538B (en) * | 2021-09-16 | 2024-09-13 | 深圳网联光仪科技有限公司 | Pathogen detection method |
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