CN102874774B - Fluorescent nanometer CdSe quantum dot probe for phorate pesticide and application thereof - Google Patents
Fluorescent nanometer CdSe quantum dot probe for phorate pesticide and application thereof Download PDFInfo
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- CN102874774B CN102874774B CN201210364912.8A CN201210364912A CN102874774B CN 102874774 B CN102874774 B CN 102874774B CN 201210364912 A CN201210364912 A CN 201210364912A CN 102874774 B CN102874774 B CN 102874774B
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Abstract
The invention discloses a fluorescent nanometer CdSe quantum dot probe for a phorate pesticide and an application thereof. The preparation of the fluorescent nanometer quantum dot probe for a phorate pesticide comprises the following steps: (a) preparing a selenium stock solution; (b) preparing a cadmium stock solution; (c) preparing the fluorescent nanometer CdSe quantum dot probe for a phorate pesticide by the cadmium stock solution and the selenium stock solution. When the fluorescent nanometer CdSe quantum dot probe for a phorate pesticide is used as a fluorescent probe for detecting a phorate pesticide, the detection limit for the phorate pesticide can reach 7.4*10-8 mol/L. The probe of the invention is simple in operation method, rapid in detection, high in sensitivity, and good in selectivity, and has the characteristics of high sensitivity and high selective identification when used for detecting phorate in a mixed sample.
Description
Technical field
The invention belongs to Pesticides Testing technical field, be specifically related to a kind of fluorescence nano CdSe quantum dot probe and application thereof of phorate agricultural chemicals.
Background technology
Phorate is the interior absorption insecticidal/acaricidal agent of a kind of high poison, efficient, wide spectrum, have tag, stomach toxicity, fumigation action, all effective to piercing-sucking mouthparts and pests with chewing mouthparts, as aphid, plant hopper, thrips, red spider, Liriomyza, plan walking first, weevil, flea beetle, mole cricket, wireworm etc.Poor to lepidopterous larvae drug effect.Phorate enters after plant materials, be subject to the impact of plant metabolism and change into the oxide compound that toxicity is larger (sulfoxide, sulfone), after insect's food-taking, in body, the activity of the acetylcholinesterase in nervous tissue is suppressed, thereby destroyed normal nerve impulse conduction, and cause poisoning, until dead.Due to the more malicious oxide compound that phorate and metabolite thereof form, in plant materials, can keep the longer time (individual month of about 1-2, even longer), therefore the drug effect phase long, but also to pay special attention to residual toxicity problem.Up to now, the detection method of phorate agricultural chemicals mainly contains high performance liquid chromatography, vapor-phase chromatography and immunization etc.But these methods have, and pretreatment process is loaded down with trivial details, analysis time is long, instrument and the high deficiency of cost of drugs.Therefore, set up simple, quick and highly sensitive phorate Pesticides Testing method and become gradually research emphasis.
In recent years, fluorescence nano quantum dot, as a kind of novel fluorescence probe, causes the extensive concern of multiple research fields.Compare with fluorescin with traditional organic fluorescent dye, quantum dot has very superior spectral quality, as: exciting light spectrum width, emmission spectrum is narrow and symmetrical, fluorescence quantum yield is high, wavelength of fluorescence is adjustable, anti-photobleaching performance is strong etc.These superior spectral qualities make quantum dot fluorescence probe be widely used in biochemical analysis detection field, have brought into play huge application potential.But up to now, quantum dot fluorescence probe is had not yet to see for the relevant report of phorate Pesticides Testing.
For above problem, we have studied a kind of novel method of fluorescence nano quantum dot probe in detecting phorate agricultural chemicals, and the method is simple to operate, it is quick and highly sensitive to detect, and can carry out the highly sensitive identification of phorate in biased sample.
Summary of the invention
The object of the present invention is to provide a kind of fluorescence nano CdSe quantum dot probe and application thereof of phorate agricultural chemicals.
The technical scheme that the present invention solves the problems of the technologies described above is as follows:
1. the preparation method of the fluorescence nano CdSe quantum dot probe of phorate agricultural chemicals is as follows:
(a) in glove box, take 0.18g selenium powder and join in the flask that 0.56g tri-n-butyl phosphine and 3.8g dioctylamine are housed, make selenium storing solution;
(b) get 0.03g Cadmium oxide and 0.38g stearic acid in three mouthfuls of Schlenk reaction vessels, adopt Schlenk technology, after vacuumizing with vacuum pump, be filled with argon gas, six times so that be full of argon gas in reaction vessel so repeatedly, then be heated to 180 ° of C and be incubated 30min, Cadmium oxide fully being dissolved, after having reacted, solution is down to room temperature, makes cadmium storing solution;
(c) in the cadmium storing solution making, add 3.8g trioctylphosphine and 3.8g cetylamine, adopt Schlenk technology, after vacuumizing with vacuum pump, be filled with argon gas, six times so that be full of argon gas in reaction vessel so repeatedly, stir and be heated to 320 ° of C, then the selenium storing solution taking out from glove box is injected into rapidly in reaction vessel, at 290 ° of C left and right reaction 1min, then remove rapidly heating unit and make product be cooled to room temperature, add 20mL chloroform, add again the centrifugation of 50mL methyl alcohol, remove supernatant liquor, the precipitation finally obtaining is dispersed in 15mL normal hexane again, make the fluorescence nano CdSe quantum dot probe of phorate agricultural chemicals, under the ultraviolet lamp of 365nm, fluorescence nano CdSe quantum dot sends stronger green fluorescence, under 388nm wavelength excites, at 460～650nm, there is very strong fluorescence emission spectrum.
2. the fluorescence nano CdSe quantum dot probe of phorate agricultural chemicals is detecting the application of phorate agricultural chemicals:
When the fluorescence nano CdSe quantum dot probe of application phorate agricultural chemicals detects phorate agricultural chemicals as fluorescent probe, fluorescent nano probe solution after diluting 500 times is mixed with phorate the pesticide solution, wherein, the fluorescence nano CdSe quantum dot probe solution of phorate agricultural chemicals and phorate the pesticide solution mol ratio are 1: 30～1500; The fluorescence intensity that can learn fluorescence nano CdSe quantum dot probe from fluorescence spectrum figure weakens with the increase of the concentration of phorate the pesticide solution, and fluorescence intensity and phorate the pesticide solution concentration have good linear relationship, therefore, the fluorescence nano CdSe quantum dot probe of phorate agricultural chemicals can be used as the content of phorate agricultural chemicals in the quick also detection by quantitative organic solvent of probe that detects phorate agricultural chemicals, to the detectability of phorate agricultural chemicals, can reach 7.4 × 10
– 8mol/L.
Advantage of the present invention:
1. phorate agricultural chemicals fluorescence nano CdSe quantum dot fluorescence probe intensity provided by the invention is high, fluorescent stability good.
2. adopt the present invention prepared phorate agricultural chemicals fluorescence nano CdSe quantum dot probe to carry out the detection of phorate agricultural chemicals, testing process is simple and convenient, highly sensitive, detectability is low, can realize the rapid detection of phorate agricultural chemicals in actual sample.
Accompanying drawing explanation
Fig. 1 is in phorate agricultural chemicals fluorescence nano CdSe quantum dot probe in detecting phorate agricultural chemicals process of the present invention, after different phorate pesticide concentrations and fluorescence nano CdSe quantum dot probe reaction, and the fluorescence spectrum figure that excitation wavelength obtains during for 388nm;
In figure, a～e is the different phorate pesticide concentrations that add in embodiment, and the mol ratio that makes probe and phorate agricultural chemicals is 1: 30～1500 fluorescence spectrum figure.
Embodiment
For a better understanding of the present invention, below in conjunction with specific embodiment, the present invention is done further and elaborated.Should be understood that following examples are preferred implementations more of the present invention, object is to set forth better content of the present invention, rather than protection scope of the present invention is produced to any restriction.
Embodiment 1
The preparation of the fluorescence nano CdSe quantum dot probe of phorate agricultural chemicals:
(a) in glove box, take 0.18g selenium powder and join in the flask that 0.56g tri-n-butyl phosphine and 3.8g dioctylamine are housed, make selenium storing solution;
(b) get 0.03g Cadmium oxide and 0.38g stearic acid in three mouthfuls of Schlenk reaction vessels, adopt Schlenk technology, after vacuumizing with vacuum pump, be filled with argon gas, six times so that be full of argon gas in reaction vessel so repeatedly, then be heated to 180 ° of C and be incubated 30min, Cadmium oxide fully being dissolved, after having reacted, solution is down to room temperature, makes cadmium storing solution;
(c) in the cadmium storing solution making, add 3.8g trioctylphosphine and 3.8g cetylamine, adopt Schlenk technology, after vacuumizing with vacuum pump, be filled with argon gas, six times so that be full of argon gas in reaction vessel so repeatedly, stir and be heated to 320 ° of C, then the selenium storing solution taking out from glove box is injected into rapidly in reaction vessel, at 290 ° of C left and right reaction 1min, then remove rapidly heating unit and make product be cooled to room temperature, add 20mL chloroform, add again the centrifugation of 50mL methyl alcohol, remove supernatant liquor, the precipitation finally obtaining is dispersed in 15mL normal hexane again, make the fluorescence nano CdSe quantum dot probe of phorate agricultural chemicals, under the ultraviolet lamp of 365nm, fluorescence nano CdSe quantum dot sends stronger green fluorescence, under 388nm wavelength excites, at 460～650nm, there is very strong fluorescence emission spectrum.
Embodiment 2
The fluorescence nano CdSe quantum dot probe of phorate agricultural chemicals is detecting the application of sensitivity of phorate agricultural chemicals:
1. the fluorescence nano CdSe quantum dot probe of application phorate agricultural chemicals detects as fluorescent probe in the process of phorate agricultural chemicals in phorate standard sample of pesticide, fluorescent nano probe solution after diluting 500 times is mixed with phorate the pesticide solution, making the fluorescence nano CdSe quantum dot probe solution of phorate agricultural chemicals and the mol ratio of phorate the pesticide solution is 1: 30, obtains fluorescence spectrum a.
2. all the other conditions are all identical with step 1, and only the fluorescence nano CdSe quantum dot probe solution of phorate agricultural chemicals and the mol ratio of phorate the pesticide solution change 1: 130 into, obtain fluorescence spectrum b;
3. all the other conditions are all identical with step 1, and only the fluorescence nano CdSe quantum dot probe solution of phorate agricultural chemicals and the mol ratio of phorate the pesticide solution change 1: 320 into,, obtain fluorescence spectrum c;
4. all the other conditions are all identical with step 1, and only the fluorescence nano CdSe quantum dot probe solution of phorate agricultural chemicals and the mol ratio of phorate the pesticide solution change 1: 750 into, obtain fluorescence spectrum d;
5. all the other conditions are all identical with step 1, and only the fluorescence nano CdSe quantum dot probe solution of phorate agricultural chemicals and the mol ratio of phorate the pesticide solution change 1: 1500 into, obtain fluorescence spectrum e;
The fluorescence intensity that can learn the fluorescence nano CdSe quantum dot probe of phorate agricultural chemicals from fluorescence spectrum figure increases and weakens with the concentration of phorate the pesticide solution, and the reduction value of fluorescence intensity and phorate the pesticide solution concentration have good linear relationship, R
2=0.9943.
Claims (1)
1. the fluorescence nano CdSe quantum dot probe of phorate agricultural chemicals, detecting the application of phorate agricultural chemicals, is characterized in that,
When the fluorescence nano CdSe quantum dot probe of application phorate agricultural chemicals detects phorate agricultural chemicals as fluorescent probe, fluorescent nano probe solution after diluting 500 times is mixed with phorate the pesticide solution, wherein, the fluorescence nano CdSe quantum dot probe solution of phorate agricultural chemicals and phorate the pesticide solution mol ratio are 1: 30～1500; The fluorescence intensity that can learn fluorescence nano CdSe quantum dot probe from fluorescence spectrum figure weakens with the increase of the concentration of phorate the pesticide solution, and fluorescence intensity and phorate the pesticide solution concentration have good linear relationship, therefore, the fluorescence nano CdSe quantum dot probe of phorate agricultural chemicals can be used as the content of phorate agricultural chemicals in the quick also detection by quantitative organic solvent of probe that detects phorate agricultural chemicals, to the detectability of phorate agricultural chemicals, can reach 7.4 × 10
– 8mol/L.
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| CN201210364912.8A CN102874774B (en) | 2012-09-26 | 2012-09-26 | Fluorescent nanometer CdSe quantum dot probe for phorate pesticide and application thereof |
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| CN201210364912.8A CN102874774B (en) | 2012-09-26 | 2012-09-26 | Fluorescent nanometer CdSe quantum dot probe for phorate pesticide and application thereof |
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| CN111208077B (en) * | 2020-02-18 | 2021-01-22 | 中国科学院地质与地球物理研究所 | Device for on-line testing of ferrous iron and total iron content in sample and use method |
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Non-Patent Citations (2)
| Title |
|---|
| Control of Photoluminescence Properties of CdSe Nanocrystals in Growth;Lianhua Qu, et al.;《Journal of the American Chemical Society》;20020206;第124卷(第9期);第2049-2055页 * |
| Lianhua Qu, et al..Control of Photoluminescence Properties of CdSe Nanocrystals in Growth.《Journal of the American Chemical Society》.2002,第124卷(第9期),第2049-2055页. |
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