CN104535601A - Dual-mode sensor for detecting Cd<2+> based on magnetic nanoparticles and preparation method of dual-mode sensor - Google Patents
Dual-mode sensor for detecting Cd<2+> based on magnetic nanoparticles and preparation method of dual-mode sensor Download PDFInfo
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Abstract
The invention belongs to the technical field of rapid detection, and particularly relates to a dual-mode sensor for detecting Cd<2+> based on magnetic nanoparticles and a preparation method of the dual-mode sensor. The method comprises the following steps: firstly, preparing a specific receptor unit, preparing Au-Fe3O4 nanoparticles, and finally dissolving the specific receptor unit, mPEG-SH and anhydrous sodium carbonate into water; and adding the mixture to an Au-Fe3O4 nanoparticle solution, and carrying out shaking table oscillating reaction for 10-20 hours. According to the dual-mode sensor disclosed by the invention, the disperse state of the nanoparticles changes into an aggregation state from a dispersed state in the presence of Cd<2+> ions. The relaxation time of water protons around the nanoparticles is changed by the change of the state; and due to the presence of gold nanoparticles, ultraviolet absorption spectrums of the nanoparticles change, so that the Cd<2+> is detected by two methods, namely an ultraviolet absorption detection method and a nuclear magnetic resonance method; and the dual-mode sensor has the advantages of high accuracy, high anti-jamming capability and high selectivity.
Description
Technical field
The invention belongs to rapid detection technical field, particularly one detects Cd based on magnetic nano-particle
2+double mode sensor and preparation method thereof.
Background technology
Environmental pollution and food security directly jeopardize public health safety, all can cause serious impact to social and economic development.Pollute unexpected environmental accident recent years and food pollution event takes place frequently, threaten the safety of people, processing each emergency event in time, is steadily the task of top priority.And emergency monitoring is the process prerequisite of similar incidents and foundation, the most key is just monitors the concentration change of pollutant in the early stage even budding period of event evolves.Thus, field quick detection technology is developed very important.Heavy metal pollution is a kind of important pollutant needing priority acccess control.Heavy metal toxicity pollutant mainly refers to lead, chromium, cadmium, mercury, copper etc.Smelt, the burning of fossil fuel, dig up mine and be the main pollution source of heavy metal.
In zoopery, cadmium can affect growth, causes a series of negative results, such as: the metabolism of young deformity, the interference young and infringement neurodevelopment.The acute effects (short-term) of cadmium enters the lungs such as major effect lung cancer, bronchiolitis and pulmonary emphysema to stimulate by exposed suction.Chronic (long-term) suction or oral contact cadmium, make cadmium in the accumulation of kidney and cause kidney trouble, and affecting liver, lung, bone, immune system, blood and nervous system simultaneously.Shown by zooscopy, be chronically exposed in the environment containing cadmium, greatly can increase the occurrence probability of lung cancer.Realize Cd
2+ion detects easily and quickly, can greatly facilitate the life of people, ensures that the public's is healthy and safe, has good social effect.
Exploitation Fast Detection Technique, realizing in shorter detection time, reach higher accuracy in detection, realize higher detection sensitivity, with guarantee environment and food security, is the developing direction of following detection technique.Fast Detection Technique newly developed in recent years has biology sensor detection technique, enzyme level detection technique, immunoassay technology, chemical sensor (electrochemical sensor, spectrum sensor, nmr sensor) etc.
But traditional detection technique poor anti jamming capability, precision are low, the Cd in sample cannot be detected fast
2+.
Summary of the invention
The object of this invention is to provide a kind of based on magnetic nano-particle detection Cd
2+double mode sensor, this sensor, by the double check of relaxation time and ultraviolet spectrum, can detect Cd fast
2+existence, and degree of accuracy is high, selectivity is good.
Another object of the present invention is to provide above-mentioned based on magnetic nano-particle detection Cd
2+the preparation method of double mode sensor.
Object of the present invention can be achieved through the following technical solutions:
A kind of based on magnetic nano-particle detection Cd
2+the preparation method of double mode sensor, its step comprises:
(1), in chloracetyl catechol and Sodium azide, dimethyl sulfoxide (DMSO) is added, 5-15 hour is reacted at 18-25 DEG C, add extraction after frozen water, dry, obtain powdered samples, then add in powdered samples after water stirs and add ethyl propiolate stirring reaction 10-20 hour again, concentrated, filtration, obtains specific receptor unit;
(2), in naphthane, add oleyl amine and gold chloride, at temperature is 60-85 DEG C, reacts 4-6 hour, centrifugal, dispersion obtains golden nanometer particle;
(3) oleyl amine, oleic acid and golden nanometer particle will be added in octadecylene and be warming up to 125-135 DEG C of maintenance 0.5-1 hour, then adding Fe (CO)
5after be warming up to 220-260 DEG C, keep 0.5-1.5 hour, cooling, centrifugal, dispersion, obtain Au-Fe
3o
4;
(4) the specific receptor unit, by step (1), mPEG-SH, natrium carbonicum calcinatum are soluble in water, then add the Au-Fe in step (3)
3o
4shaking table oscillating reactions 10-20 hour.
In described step (1), in chloracetyl catechol, Sodium azide and the proportioning that adds of dimethyl sulfoxide (DMSO) be 1g:0.1-2g:10-20mL.
In described step (1), the additional proportion of powdered samples and water is 20-50mg/mL.
In described step (1), the addition ratio that adds of powdered samples and ethyl propiolate is 3-10mg:1 μ L.
In described step (2), the proportioning that adds of naphthane, oleyl amine and gold chloride is 8-12mL:1mL:0.1g.
In described step (3), golden nanometer particle and Fe (CO)
5addition proportioning be 2-25mg:0.1mL.
In described step (4), the proportioning that adds of specific receptor unit, mPEG-SH, natrium carbonicum calcinatum is 1:1-1.5:6-7; Specific receptor unit and Au-Fe
3o
4the proportioning that adds be 1:0.1-2.5.Suitable adds proportioning, is conducive to the raising dispersed in aqueous of double mode sensor, and the enhancing of detectability.
Can be prepared by above-mentioned preparation method and detect Cd based on magnetic nano-particle
2+double mode sensor.
Double mode sensor of the present invention passes through Cd
2+the specific recognition effect of ion, at Cd
2+ion is deposited in case, and the disperse state of nano particle is changed by being distributed to gathering.The change of this state, the relaxation time that can change the water proton around nano particle changes, simultaneously due to gold nano existence and there occurs gathering, also the ultra-violet absorption spectrum of nano particle is made to change, by the use of nuclear magnetic resonance POP instrument and Ultravioblet spectrophotometer, realize Cd
2+the double mode detection of ion.
Compared with prior art, beneficial effect of the present invention is:
(1) what prepared by the present invention detects Cd based on magnetic nano-particle
2+double mode sensor UV absorbance detection and nuclear magnetic resonance method two kinds of methods can be adopted jointly to detect Cd
2+, have precision high, antijamming capability is strong, and selectivity is high.
(2) the present invention is when by the detection of Ultravioblet spectrophotometer, can be realized intuitively, visual testing process by the change of color and spectrum, and detection efficiency is high, convenient.
(3) the double mode sensor operations prepared of the present invention is simple, and the degree of controllability of reaction is high, expands the range of application of nanometer technology.
Accompanying drawing explanation
Fig. 1 is the nuclear magnetic spectrogram of the specific receptor unit of preparation in embodiment 1.
Fig. 2 is the heterozygosis Au-Fe of preparation in embodiment 1
3o
4the Electronic Speculum figure of nano particle.
Fig. 3 is heterozygosis Au-Fe prepared in embodiment 1
3o
4the uv absorption spectrogram of nano particle.
Fig. 4 is heterozygosis Au-Fe prepared in embodiment 1
3o
4the infrared spectrum of nano particle.
Fig. 5 is the infrared spectrum of double mode sensor prepared by embodiment 1.
Fig. 6 is the Electronic Speculum figure of double mode sensor prepared by embodiment 1.
Fig. 7 is the hydrated diameter (DLS) of double mode sensor in 1 in embodiment.
Fig. 8 is for adding Cd
2+after double mode sensor assemble after hydrated diameter (DLS).
Fig. 9 for add variable concentrations Cd in double mode sensor
2+after uv absorption spectrogram.
Figure 10 for add variable concentrations Cd in double mode sensor
2+after T2 (T
2) variation diagram.
Figure 11 sensor nano particle is to the selectivity test comparison diagram of different metallic ions (300 μm of ol/L).
Embodiment
Below in conjunction with embodiment, the invention will be further described:
Embodiment 1
(1), the preparation of specific receptor unit
In the chloracetyl catechol of 1.0g, in the Sodium azide of 300mg, add the DMSO (dimethyl sulfoxide (DMSO)) of 15mL.At room temperature react 8h, add the frozen water of 50mL, by extracted with diethyl ether three times.Organic phase is washed and is used Na
2cO
3drying, organic phase obtains powdered samples through decompression distillation.Take 380mg powdered samples and be dissolved in 15mLH
2in O, mix; Add the ethyl propiolate of 50 μ L, add thermal agitation 12h, after reaction terminates, thickening filtration, recrystallization, i.e. specific receptor unit.Fig. 1 is the nuclear magnetic spectrogram of the specific receptor unit of preparation.
(2) heterozygosis Au-Fe
3o
4preparation
In the naphthane of 10mL, add the oleyl amine of 1mL, the gold chloride of 100mg, be warming up to 70 DEG C, reaction 5h, cooling, it is centrifugal to add ethanol, is dispersed in normal hexane, obtains golden nanometer particle.
In the octadecylene of 10mL, add the oleyl amine of 1mL, the oleic acid of 1mL, then add the golden nanometer particle (1-10mg/mL) of 2mL, be warming up to 130 DEG C and keep 30min; Add the Fe (CO) of 0.1mL
5, be slowly warming up to 240 DEG C, keep 1h; Be cooled to room temperature, it is centrifugal to add a large amount of isopropyl alcohols, and by heterozygosis Au-Fe
3o
4nanoparticle dispersion in chloroform.Fig. 2 is heterozygosis Au-Fe
3o
4the Electronic Speculum figure of nano particle, by this Electronic Speculum figure, can find out the favorable dispersibility of the nano particle of preparation.
Fig. 3 is heterozygosis Au-Fe
3o
4the uv absorption spectrogram of nano particle, this nano particle has maximum absorption band at 565nm place.
Fig. 4 is heterozygosis Au-Fe
3o
4the infrared spectrum of nano particle.
(3) Cd is detected based on magnetic nano-particle
2+the preparation of double mode sensor
Get 15mg specific receptor unit, the mPEG-SH of 20mg; Natrium carbonicum calcinatum 100mg, soluble in water, mixing mixing forms aqueous solution; Get the heterozygosis Au-Fe of 2mL
3o
4nano particle (1-10mg/mL) is diluted to 5mL, joins in above-mentioned aqueous solution, shaking table oscillating reactions 16 hours; Centrifugal, be dispersed in water.
Fig. 5 is the infrared spectrum of prepared double mode sensor, from Fig. 4 and Fig. 5 contrast, and heterozygosis Au-Fe
3o
4the success of Nanoparticle Modified specific receptor unit.
Fig. 6 is the Electronic Speculum figure of prepared double mode sensor, illustrates that obtained sensor distribution is good.
Embodiment 2
(1), the preparation of specific receptor unit
In the chloracetyl catechol of 1.0g, in the Sodium azide of 1.0g, add the DMSO (dimethyl sulfoxide (DMSO)) of 20mL.At room temperature react 12h, add the frozen water of 60mL, by extracted with diethyl ether three times.Organic phase is washed and is used Na
2cO
3drying, organic phase obtains powdered samples through decompression distillation.Take 380mg powdered samples and be dissolved in 15mLH
2in O, mix; Adding the ethyl propiolate of 100 μ L, stir 12h at normal temperatures, after reaction terminates, thickening filtration, recrystallization, i.e. specific receptor unit.
(2) heterozygosis Au-Fe
3o
4preparation
In the naphthane of 100mL, add the oleyl amine of 10mL, the gold chloride of 1g, be warming up to 70 DEG C, reaction 5h, cooling, it is centrifugal to add ethanol, is dispersed in normal hexane, obtains golden nanometer particle.
The oleic acid of 1mL in the octadecylene of 20mL, then adds the golden nanometer particle (40mg) of 2.5mL, is warming up to 130 DEG C and keeps 40min; Add the Fe (CO) of 0.18mL
5, inject the oleyl amine of 0.6mL, be slowly warming up to 245 DEG C, keep 1h; Be cooled to room temperature, it is centrifugal to add a large amount of isopropyl alcohols, and by heterozygosis Au-Fe
3o
4be dispersed in chloroform.
(3) Cd is detected based on magnetic nano-particle
2+the preparation of double mode sensor
Get 20mg specific receptor unit, the mPEG-SH of 25mg; Natrium carbonicum calcinatum 110mg, soluble in water, mixing mixing forms aqueous solution; Get the heterozygosis Au-Fe of 3mL
3o
4nano particle (8-12mg) is diluted to 5mL, joins in above-mentioned aqueous solution, shaking table oscillating reactions 16 hours; Centrifugal, be dispersed in water.
Embodiment 3
(1) preparation of specific receptor unit is with embodiment 1.
(2) heterozygosis Au-Fe
3o
4preparation with embodiment 1.
(3) Cd is detected based on magnetic nano-particle
2+the preparation of double mode sensor
Get 30mg specific receptor unit, the mPEG-SH of 40mg; Natrium carbonicum calcinatum 200mg, soluble in water, mixing mixing forms aqueous solution; Get the heterozygosis Au-Fe of 4mL
3o
4nano particle (10-18mg) is diluted to 5mL, join in above-mentioned aqueous solution, shaking table oscillating reactions? hour; Centrifugal, be dispersed in water.
Cd is detected based on magnetic nano-particle by what obtain in embodiment 1
2+double mode sensor to Cd
2+detect:
(1), ultraviolet spectroscopy is utilized to detect
Be add Cd in the solution of the double mode sensor nano particle of (21.18 μ g/mL) at Fe content
2+ion, makes Cd
2+the concentration of ion is respectively 0,10,20,30,40,50,60,70,80,90,100,110 and 120 μm of ol/L, due to Cd
2+the difference of concentration, makes uv absorption spectrogram that different changes occur; Result as shown in Figure 9.Ultraviolet spectroscopy is utilized to detect, Cd
2+the detectability of ion is about 3.02 μm of ol/L.And along with the Cd in solution
2+ion increases, and color is changed to blueness by aubergine.Be convenient to people's naked eyes just can observe, very convenient, practical.
(2) nuclear magnetic resonance method is utilized to detect
Be add Cd in the solution of the double mode sensor nano particle of 0.71 μ g/mL at Fe content
2+ion, makes Cd
2+the concentration of ion is respectively 40,50,60,70,80,90,100,110,120,130,140,150,160 and 170 μm of ol/L, due to Cd
2+the difference of concentration, T2 (T
2) changing value increase gradually, until reach balance; Result as shown in Figure 10.Utilize the method for nuclear magnetic resonance, Cd
2+the detectability of ion is about 2.64 μm of ol/L.
(3) anti-interference test
Be add the different metallic ion of 300 μm of ol/L in the solution of the double mode sensor nano particle of (21.18 μ g/mL) at Fe content, the change of the uv absorption spectrogram that more similar heavy metal ion causes, for detecting the competitiveness of this sensor, as shown in figure 11, this sensor nano particle has good selectivity to result.
Contrast test
Double mode sensor prepared by magnetic nano-particle monotype sensor of the prior art and the present invention is carried out the contrast test of precision, result is as follows:
In the double mode sensor nano particle solution (Fe content is 21.18 μ g/mL) prepared with the present invention in magnetic nano-particle monotype sensor nano particle solution in the prior art, add the Cd that concentration is 0.05 μm of ol/L, 0.10 μm of ol/L, 10 μm of ol/L, 20 μm of ol/L, 50 μm of ol/L, 80 μm of ol/L respectively
2+testing sample, the Detection accuracy of double mode sensor nano particle solution is 100%, but the Detection accuracy of magnetic nano-particle monotype sensor nano particle solution is only 95%.
The above is preferred embodiment of the present invention, but the present invention should not be confined to the content disclosed in this embodiment.The equivalence completed under not departing from spirit disclosed in this invention so every or amendment, all fall into the scope of protection of the invention.
Claims (9)
1. one kind is detected Cd based on magnetic nano-particle
2+the preparation method of double mode sensor, its step comprises:
(1), in chloracetyl catechol and Sodium azide, dimethyl sulfoxide (DMSO) is added, 5-15 hour is reacted at 18-25 DEG C, add extraction after frozen water, dry, obtain powdered samples, then add in powdered samples after water stirs and add ethyl propiolate stirring reaction 10-20 hour again, concentrated, filtration, obtains specific receptor unit;
(2), in naphthane, add oleyl amine and gold chloride, at temperature is 60-85 DEG C, reacts 4-6 hour, centrifugal, dispersion obtains golden nanometer particle;
(3), oleyl amine, oleic acid and golden nanometer particle will be added in octadecylene and be warming up to 125-135 DEG C of maintenance 0.5-1 hour, then adding Fe (CO)
5after be warming up to 220-260 DEG C, keep 0.5-1.5 hour, cooling, centrifugal, dispersion, obtain Au-Fe
3o
4;
(4) the specific receptor unit, by step (1), mPEG-SH, natrium carbonicum calcinatum are soluble in water, then add the Au-Fe in step (3)
3o
4shaking table oscillating reactions 10-20 hour.
2. according to claim 1 based on magnetic nano-particle detection Cd
2+the preparation method of double mode sensor, it is characterized in that: in described step (1), in chloracetyl catechol, Sodium azide and the proportioning that adds of dimethyl sulfoxide (DMSO) be 1g:0.1-2g:10-20mL.
3. according to claim 1 based on magnetic nano-particle detection Cd
2+the preparation method of double mode sensor, it is characterized in that: in described step (1), the additional proportion of powdered samples and water is 20-50mg/mL.
4. according to claim 1 based on magnetic nano-particle detection Cd
2+the preparation method of double mode sensor, it is characterized in that: in described step (1), powdered samples and ethyl propiolate add addition than being 3-10mg:1 μ L.
5. according to claim 1 based on magnetic nano-particle detection Cd
2+the preparation method of double mode sensor, it is characterized in that: in described step (2), the proportioning that adds of naphthane, oleyl amine and gold chloride is 8-12mL:1mL:0.1g.
6. according to claim 1 based on magnetic nano-particle detection Cd
2+the preparation method of double mode sensor, it is characterized in that: in described step (3), golden nanometer particle and Fe (CO)
5addition proportioning be 2-25mg:0.1mL.
7. according to claim 1 based on magnetic nano-particle detection Cd
2+the preparation method of double mode sensor, it is characterized in that: in described step (4), the proportioning that adds of specific receptor unit, mPEG-SH, natrium carbonicum calcinatum is 1:1-1.5:6-7.
8. according to claim 1 based on magnetic nano-particle detection Cd
2+the preparation method of double mode sensor, it is characterized in that: in described step (4), specific receptor unit and Au-Fe
3o
4the proportioning that adds be 1:0.1-2.5.
9. one kind is detected Cd based on magnetic nano-particle
2+double mode sensor, it is characterized in that: by any one of claim 1-8 claim preparation.
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Cited By (1)
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