CN103901007A - Method for detecting content of chlortoluron in farmland water by using fluorescence carbon point and cadmium telluride quantum dot energy transferring technology - Google Patents
Method for detecting content of chlortoluron in farmland water by using fluorescence carbon point and cadmium telluride quantum dot energy transferring technology Download PDFInfo
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Abstract
The invention discloses a method for detecting the content of chlortoluron in farmland water by using a fluorescence carbon point and cadmium telluride quantum dot energy transferring technology. According to the method, a fluorescence carbon point is used as an energy transferring donor and a cadmium telluride quantum dot is used as an acceptor to form an energy transferring system with stable performance; the fluorescence carbon point is used for transferring energy to the cadmium telluride quantum dot so as to cause fluorescence enhancement of the cadmium telluride quantum dot. The chlortoluron is added and electrons on the surface of the cadmium telluride quantum dot are transferred to the chlortoluron to be in non-radiation combination with the chlortoluron, so that the fluorescent light of the cadmium telluride quantum dot is regularly quenched. The concentration of the chlortoluron has a good linear relation with a fluorescence quenching degree (F0/F) in a range of 0.05-12.0 micrograms/liter; a linear regression equation is F0/F=1.0+0.138c and the linearly dependent coefficient r is equal to 0.9979; the detection limit of the method is 0.017 microgram/liter. The method disclosed by the invention is simple, high in sensitivity and good in selectivity; the detection of the chlortoluron in a farmland water sample is very convenient and rapid.
Description
Technical field
The present invention relates to a kind of method of utilizing fluorescent carbon point and cadmium telluride quantum dot energy transfer technique fast detecting farmland underwater trace chlortoluron.
Background technology
Chlortoluron is a kind of phenylurea herbicide, can high select, controls efficiently the growth of year raw Gramineae and broadleaved herb, becomes and applies to obtain one of phenylurea herbicide the most widely.Research shows, chlortoluron has certain carcinogenicity and hydrophyte is had to direct toxic action.At present, the detection method that chlortoluron is conventional has chromatography, electrochemical process and euzymelinked immunosorbent assay (ELISA) etc.Although these methods have some advantage, the instrument that these methods have is more expensive, and some complicated operations have limited its application in actual sample detects.Therefore the content that a kind of method that, develops simple, quick, sensitive, high selectivity detects chlortoluron has great importance.Energy transfer technique is a kind of novel fluorescence detection technique, has highly sensitively, compares be subject to Rayleigh scattering light to disturb the feature such as little with conventional fluorescence method with Resonance Light Scattering Method.Fluorescent carbon point has good optical characteristics, and such as absorption spectrum, fluorescence size is adjustable, and fluorescence lifetime is long, and quantum yield is high, has been applied to the analysis in the fields such as environmental contaminants, virus, biomolecule, metallic ion.So fluorescent carbon point can be used as donor or acceptor, set up more effective FRET (fluorescence resonance energy transfer) system.Utilize fluorescent carbon point as fluorescence donor herein, cadmium telluride is set up a novel energy transfering system as fluorescent receptor, and quick, sensitive, to detect the accurately chlortoluron new method of having utilized this Establishing.The different fluorescent carbon point of domestic and international application and cadmium telluride quantum dot energy transfer method there is not yet report in the detection of chlortoluron at present.
Summary of the invention
The object of this invention is to provide a kind of method of utilizing fluorescent carbon point and cadmium telluride quantum dot energy transfer technique to detect chlorotoluron content in the water of farmland.
Thinking of the present invention: shift using fluorescent carbon point as energy to body, cadmium telluride quantum dot is as acceptor, forms the energy transfer system of stable performance, energy is passed to cadmium telluride quantum dot by fluorescent carbon point, causes the fluorescence of cadmium telluride quantum dot to strengthen.Adding of chlortoluron, but makes the fluorescence generation quencher of cadmium telluride quantum dot, and the concentration of its fluorescent quenching degree and chlortoluron is good linear relationship within the scope of 0.05 ~ 12.0 micrograms per litre, thereby sets up the new method that detects chlortoluron.
The concrete mechanism of the present invention: energy is passed to cadmium telluride quantum dot by fluorescent carbon point, causes the fluorescence of cadmium telluride quantum dot to strengthen.Along with adding of chlortoluron, the electronics on cadmium telluride quantum dot surface is transferred to chlortoluron, with chlortoluron, non-radiative combination occurs, and causes the fluorescence of cadmium telluride quantum dot that regular quencher occurs.
Concrete steps are:
(1) water soluble cadmium telluride quantum point is synthetic:
In the there-necked flask of 25 milliliters, add respectively tellurium powder, 0.10-0.13 gram sodium borohydride and the 4-6 milliliter intermediate water of 0.03-0.06 gram, mix, under 60-70 ℃ of water-bath and magnetic agitation, react 10-30 minute, obtain purple transparent sodium hydrogen telluride aqueous solution, for subsequent use; Under nitrogen protection, be 2.5 × 10 at 180-220 ml concn
-3in mol/L caddy aqueous solution, add 0.08-0.12 milliliter to analyze pure mercaptoacetic acid, regulating pH with NaOH is 9-11, under strong mixing, add rapidly the above-mentioned sodium hydrogen telluride aqueous solution of 4-6 milliliter, the 1.5-2.5 hour that refluxes at 90-100 ℃, obtains the transparent cadmium telluride quantum dot solution of color.
(2) fluorescent carbon point is synthetic:
In pyroreaction still, add 0.1-0.3 gram of sodium citrate, 1-2 gram ammonium bicarbonate and 8-12 milliliter intermediate water, mix, to sodium citrate and ammonium bicarbonate dissolving; By the mixed solution of gained, as in the drying box of 180 ℃, reaction 3-5 hour, is cooled to room temperature; After having reacted, the product of gained is placed in to bag filter (1000 dalton) dialysis 22-26 hour, to purify, obtains the higher fluorescent carbon point of purity; Fluorescent carbon point after purifying is diluted to 100 milliliters and obtains fluorescent carbon point solution, keep in Dark Place in 4 ℃.
(3) detection method:
In 10 5 milliliters of color comparison tubes, adding respectively 0 microlitre, 2.5 microlitres, 7.5 microlitres, 15 microlitres, 50 microlitres, 150 microlitres, 150 microlitres, 400 microlitres, 500 microlitres, 600 microlitre concentration is 5.0 × 10
-4the chlortoluron solution of grams per liter, in these 10 color comparison tubes, adding respectively the fluorescent carbon point solution of 30 microlitre step (2) gained and the cadmium telluride quantum dot solution of 50 microlitre step (1) gained, is then that the amino liquid of 0.1 mol/L trihydroxy methyl is settled to scale by the concentration of pH=8.7 respectively again; At room temperature react after 5 minutes and carry out fluorescence intensity detection with RF-5301PC fluorophotometer, excitation wavelength is 350 nanometers, excites and launch slit width to be 5 nanometers.
(4) drafting of working curve:
In 10 5 milliliters of color comparison tubes, adding respectively 0 microlitre, 2.5 microlitres, 7.5 microlitres, 15 microlitres, 50 microlitres, 150 microlitres, 150 microlitres, 400 microlitres, 500 microlitres, 600 microlitre concentration is 5.0 × 10
-4the chlortoluron solution of grams per liter, in these 10 color comparison tubes, adding respectively the fluorescent carbon point solution of 30 microlitre step (2) gained and the cadmium telluride quantum dot solution of 50 microlitre step (1) gained, is then that 0.1 mol/L trishydroxymethylaminomethane-concentration is that the buffer solution of 0.1 mol/L hydrochloric acid is settled to scale by the concentration of pH=8.7 respectively again; At room temperature react after 5 minutes and carry out fluorescence intensity detection with RF-5301PC fluorophotometer, excitation wavelength is 350 nanometers, excites and launch slit width to be 5 nanometers; The concentration of chlortoluron in the scope of 0.05 ~ 12 micrograms per litre with the fluorescent quenching degree (F of cadmium telluride quantum dot
0/ F) be good linear relationship, its equation of linear regression is F
0/ F=1.0+0.138c, linearly dependent coefficient r=0.9979.
The inventive method is simple, highly sensitive, and selectivity is good, has overcome prior art and exist the shortcoming of reaction time length, complex operation, poor selectivity, instrument costliness in the time detecting, for the more accurate fast and easy of detection of low concentration chlortoluron in the water of farmland.
Accompanying drawing explanation
Fig. 1 is that the chlortoluron of embodiment of the present invention variable concentrations recovers spectrogram to the fluorescence of cadmium telluride quantum dot.Wherein a is respectively the chlortoluron of 0.0,0.05,0.15,0.3,1.0,3.0,6.0,8.0,10.0,12.0 micrograms per litre to the fluorescence recovery spectrogram of cadmium telluride quantum dot to j.
Fig. 2 is the graph of a relation of the fluorescent quenching of chlortoluron to cadmium telluride quantum dot in embodiment of the present invention chlorotoluron content and fluorescent carbon point-cadmium telluride quantum dot energy transfer system.
Embodiment
embodiment:
(1) water soluble cadmium telluride quantum point is synthetic:
In the there-necked flask of 25 milliliters, add respectively the tellurium powder of 0.048 gram, 0.120 gram of sodium borohydride and 5 milliliters of intermediate waters, mix, under 65 ℃ of water-baths and magnetic agitation, react 20 minutes, obtain purple transparent sodium hydrogen telluride aqueous solution, for subsequent use; Under nitrogen protection, be 2.5 × 10 at 200 ml concns
-3in mol/L caddy aqueous solution, add 0.10 milliliter to analyze pure mercaptoacetic acid, regulating pH with NaOH is 9-11, under strong mixing, add rapidly 5.0 milliliters of above-mentioned sodium hydrogen telluride aqueous solution, at 95 ℃, reflux 2 hours, obtain the transparent cadmium telluride quantum dot solution of color.
(2) fluorescent carbon point is synthetic:
In pyroreaction still, add 0.2 gram of sodium citrate, 1.5 grams of ammonium bicarbonate and 10 milliliters of intermediate waters, mix, to sodium citrate and ammonium bicarbonate dissolving; The mixed solution of gained, as in the drying box of 180 ℃, is reacted 4 hours, be cooled to room temperature; After having reacted, the product of gained is placed in to bag filter (1000 dalton) dialysis 24 hours, to purify, obtains the higher fluorescent carbon point of purity; Fluorescent carbon point after purifying is diluted to 100 milliliters and obtains fluorescent carbon point solution, keep in Dark Place in 4 ℃.
(3) detection method:
In 10 5 milliliters of color comparison tubes, adding respectively 0 microlitre, 2.5 microlitres, 7.5 microlitres, 15 microlitres, 50 microlitres, 150 microlitres, 150 microlitres, 400 microlitres, 500 microlitres, 600 microlitre concentration is 5.0 × 10
-4the chlortoluron solution of grams per liter, in these 10 color comparison tubes, adding respectively the fluorescent carbon point solution of 30 microlitre step (2) gained and the cadmium telluride quantum dot solution of 50 microlitre step (1) gained, is then that 0.1 mol/L trishydroxymethylaminomethane-concentration is that the buffer solution of 0.1 mol/L hydrochloric acid is settled to scale by the concentration of pH=8.7 respectively again; At room temperature react after 5 minutes and carry out fluorescence intensity detection with RF-5301PC fluorophotometer, excitation wavelength is 350 nanometers, excites and launch slit width to be 5 nanometers.
(4) drafting of working curve:
In 10 5 milliliters of color comparison tubes, adding respectively 0 microlitre, 2.5 microlitres, 7.5 microlitres, 15 microlitres, 50 microlitres, 150 microlitres, 150 microlitres, 400 microlitres, 500 microlitres, 600 microlitre concentration is 5.0 × 10
-4the chlortoluron solution of grams per liter, in these 10 color comparison tubes, adding respectively the fluorescent carbon point solution of 30 microlitre step (2) gained and the cadmium telluride quantum dot solution of 50 microlitre step (1) gained, is then that 0.1 mol/L trishydroxymethylaminomethane-concentration is that the buffer solution of 0.1 mol/L hydrochloric acid is settled to scale by the concentration of pH=8.7 respectively again; At room temperature react after 5 minutes and carry out fluorescence intensity detection with RF-5301PC fluorophotometer, excitation wavelength is 350 nanometers, excites and launch slit width to be 5 nanometers; The concentration of chlortoluron in the scope of 0.05 ~ 12 micrograms per litre with the fluorescent quenching degree (F of cadmium telluride quantum dot
0/ F) be good linear relationship, its equation of linear regression is F
0/ F=1.0+0.138c, linearly dependent coefficient r=0.9979.
(5) detection of chlorotoluron content in the water of farmland:
Said method is applied to field irrigation, and water sample obtains near farmland Yanshan District, hazard prevention, and hold over night, makes sediment deposition.Getting appropriate liquid to be measured measures sample by experimental technique operation, carry out standard simultaneously and add recovery test, result is as shown in table 1, its RSD≤3.48 % (n=6), recovery of standard addition is between 96.8 % ~ 102.3 %, and illustration method has higher accuracy and good precision.
Table 1: sample determination and mark-on recovery test data
Claims (1)
1. utilize fluorescent carbon point and cadmium telluride quantum dot energy transfer technique to detect a method for chlorotoluron content in the water of farmland, it is characterized in that concrete steps are:
(1) water soluble cadmium telluride quantum point is synthetic:
In the there-necked flask of 25 milliliters, add respectively tellurium powder, 0.10-0.13 gram sodium borohydride and the 4-6 milliliter intermediate water of 0.03-0.06 gram, mix, under 60-70 ℃ of water-bath and magnetic agitation, react 10-30 minute, obtain purple transparent sodium hydrogen telluride aqueous solution; Under nitrogen protection, be 2.5 × 10 at 180-220 ml concn
-3in mol/L caddy aqueous solution, add 0.08-0.12 milliliter to analyze pure mercaptoacetic acid, regulating pH with NaOH is 9-11, under strong mixing, add rapidly the above-mentioned sodium hydrogen telluride aqueous solution of 4-6 milliliter, the 1.5-2.5 hour that refluxes at 90-100 ℃, obtains the transparent cadmium telluride quantum dot solution of color;
(2) fluorescent carbon point is synthetic:
In pyroreaction still, add 0.1-0.3 gram of sodium citrate, 1-2 gram ammonium bicarbonate and 8-12 milliliter intermediate water, mix, to sodium citrate and ammonium bicarbonate dissolving; By the mixed solution of gained, as in the drying box of 180 ℃, reaction 3-5 hour, is cooled to room temperature; After having reacted, the product of gained is placed in to the bag filter 22-26 hour that dialyses, to purify, obtains the higher fluorescent carbon point of purity; Fluorescent carbon point after purifying is diluted to 100 milliliters and obtains fluorescent carbon point solution, keep in Dark Place in 4 ℃;
(3) detection method:
In 10 5 milliliters of color comparison tubes, adding respectively 0 microlitre, 2.5 microlitres, 7.5 microlitres, 15 microlitres, 50 microlitres, 150 microlitres, 150 microlitres, 400 microlitres, 500 microlitres, 600 microlitre concentration is 5.0 × 10
-4the chlortoluron solution of grams per liter, in these 10 color comparison tubes, adding respectively the fluorescent carbon point solution of 30 microlitre step (2) gained and the cadmium telluride quantum dot solution of 50 microlitre step (1) gained, is then that 0.1 mol/L trishydroxymethylaminomethane-concentration is that the buffer solution of 0.1 mol/L hydrochloric acid is settled to scale by the concentration of pH=8.7 respectively again; At room temperature react after 5 minutes and carry out fluorescence intensity detection with RF-5301PC fluorophotometer, excitation wavelength is 350 nanometers, excites and launch slit width to be 5 nanometers;
(4) drafting of working curve:
In 10 5 milliliters of color comparison tubes, adding respectively 0 microlitre, 2.5 microlitres, 7.5 microlitres, 15 microlitres, 50 microlitres, 150 microlitres, 150 microlitres, 400 microlitres, 500 microlitres, 600 microlitre concentration is 5.0 × 10
-4the chlortoluron solution of grams per liter, in these 10 color comparison tubes, adding respectively the fluorescent carbon point solution of 30 microlitre step (2) gained and the cadmium telluride quantum dot solution of 50 microlitre step (1) gained, is then that 0.1 mol/L trishydroxymethylaminomethane-concentration is that the buffer solution of 0.1 mol/L hydrochloric acid is settled to scale by the concentration of pH=8.7 respectively again; At room temperature react after 5 minutes and carry out fluorescence intensity detection with RF-5301PC fluorophotometer, excitation wavelength is 350 nanometers, excites and launch slit width to be 5 nanometers; The concentration of chlortoluron is F with the fluorescent quenching degree of cadmium telluride quantum dot in the scope of 0.05 ~ 12 micrograms per litre
0/ F is good linear relationship, and its equation of linear regression is F
0/ F
=1.0+0.138c, linearly dependent coefficient r=0.9979.
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