CN110511745A - A kind of preparation method of water soluble fluorescence silicon quantum dot and its application in selective enumeration method paranitrophenol - Google Patents

A kind of preparation method of water soluble fluorescence silicon quantum dot and its application in selective enumeration method paranitrophenol Download PDF

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CN110511745A
CN110511745A CN201910791551.7A CN201910791551A CN110511745A CN 110511745 A CN110511745 A CN 110511745A CN 201910791551 A CN201910791551 A CN 201910791551A CN 110511745 A CN110511745 A CN 110511745A
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quantum dot
paranitrophenol
silicon quantum
fluorescence
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CN110511745B (en
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叶存玲
王远飞
武莹
王全坤
王治科
范顺利
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Henan Normal University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/02—Silicon
    • C01B33/021—Preparation
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/59—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing silicon
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • 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
    • G01N21/64—Fluorescence; Phosphorescence
    • G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
    • G01N21/643—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes" non-biological material
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • 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
    • G01N21/64—Fluorescence; Phosphorescence
    • G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
    • G01N2021/6432—Quenching

Abstract

The invention belongs to fluorescent functional Material Fields, and in particular to a kind of water-soluble silicon quantum dot and preparation method thereof, and the application in the highly selective detection of high sensitivity of paranitrophenol.Technical solution of the present invention main points are as follows: 3- aminopropyl triethoxysilane is added in ultrapure water under 85 DEG C and intense agitation and reacts 10min, adds acetaminophen solution, is persistently stirred to react 5h.Silicon quantum dot simple synthetic method of the invention, reaction condition is mild, and quantum yield is high, good water solubility, and saves for a long time, or even be still able to maintain excellent fluorescence property under different pH, different ionic strength conditions.The silicon quantum dot emits 495nm fluorescence under the fluorescence excitation of 398nm, and paranitrophenol can the specific fluorescence for quenching silicon quantum dot.Silicon quantum dot of the present invention shows good application prospect rapidly and efficiently, in terms of highly selective, highly sensitive detection paranitrophenol.

Description

A kind of preparation method of water soluble fluorescence silicon quantum dot and its in selective enumeration method to nitre Application in base phenol
Technical field
The invention belongs to fluorescent functional field of material technology, and in particular to a kind of preparation side of water soluble fluorescence silicon quantum dot Method and its application in selective enumeration method paranitrophenol.
Background technique
Paranitrophenol property is stable and can be dissolved in water, thus it can long-term existence in the natural environment, and because it is used extensively In the preparation of the chemical articles such as pesticide, medicine, rubber, explosive and dyestuff, often through water body and soil pollution and then serious shadow Ring the physical and mental health of people.Currently, the method for detecting paranitrophenol mainly has electrochemical method, capillary electrophoresis, color Spectrometry etc..However, more or less there are some defects in these methods.Fluorescence analysis method is low cost, efficient, Sensitive Detection pair Nitrophenols provides new approaches.
Summary of the invention
The technical problem to be solved by the present invention is to provide a kind of simple synthetic method, mild condition and fluorescence property are excellent The preparation method of water soluble fluorescence silicon quantum dot, this method are used using 3- aminopropyl triethoxysilane as silicon precursor, to acetyl Amino phenols is reducing agent, has prepared the bright cyan water soluble fluorescence silicon quantum dot of generation.The quantum yield of the silicon quantum dot is 12.8%, and possess water-soluble and good photoluminescent property well.And under strong acid, highly basic or high ionic strength, still It is able to maintain stable fluorescence property.This fluorescence chemical sensor has good selectivity and sensitivity, is used successfully to practical water The detection of paranitrophenol in sample.
A kind of technical solution of the present invention main points are as follows: preparation method of water soluble fluorescence silicon quantum dot, it is characterised in that tool Body step are as follows: 5mL ultrapure water is added in collet beaker, three ethoxy of 1mL 3- aminopropyl is added under 85 DEG C of intense agitations Base silane, in 10min after the acetaminophen solution of 2mL, 50mM is added, be persistently stirred to react 5h, it is final that water solubility is made Hanced cyan fluorescent silicon quantum dot.
Water soluble fluorescence silicon quantum dot of the present invention is in highly selective, answering in Sensitive Determination paranitrophenol concentration With, it is characterised in that detailed process are as follows: the PBS for sequentially adding 0.5mL silicon quantum dot and 0.2mL, pH=11 in the reaction vessel is slow Solution is rushed, paranitrophenol to be measured, constant volume 4.00mL, in 25 DEG C of reaction 40min, in excitation wavelength 398nm, launch wavelength are added 495nm measures mixed system fluorescence intensity, obtains further according to the fluorescence intensity measured and in conjunction with linear equation calculation to be measured to nitre Base phenol concentration；Paranitrophenol concentration is within the scope of 1-80 μM, with fluorescent quenching efficiency (F0- F)/F0Between exist it is preferable linear Relationship, R2=0.9944, linear equation is (F0- F)/F0=0.007C+0.036, wherein F0、F is added before and after paranitrophenol respectively The fluorescence intensity of system, C are the concentration of paranitrophenol, and unit μM is repeated 11 times measurement, relative standard to 40 μM of paranitrophenols Deviation is 0.9%, and detection is limited to 0.87 μM.
Water-soluble silicon quantum dot produced by the present invention emits 495nm fluorescence under the fluorescence excitation of 398nm, and to nitro Phenol can the specific fluorescence for quenching silicon quantum dot.Water-soluble silicon quantum dot produced by the present invention rapidly and efficiently, it is highly selective, high Good application prospect is shown in terms of sensitivity technique paranitrophenol.
Detailed description of the invention
Fig. 1 is the stability of silicon quantum dot.
Fig. 2 is influence of the pH to silicon quantum dot fluorescence property.
Fig. 3 is influence of the ionic strength to silicon quantum dot fluorescence property.
Fig. 4 is the excitation and emission spectra figure of silicon quantum dot.
Fig. 5 is 3- aminopropyl triethoxysilane (APTS), paracetamol (APAP), silicon quantum dot (SiQDs) are red External spectrum.
Fig. 6 is the selectivity and interference free performance of measuring method.
Specific embodiment
Above content of the invention is described in further details by the following examples, but this should not be interpreted as to this The range for inventing above-mentioned theme is only limitted to embodiment below, and all technologies realized based on above content of the present invention belong to this hair Bright range.
Embodiment
Synthesizing water-solubility hanced cyan fluorescent silicon quantum dot
5mL ultrapure water is added in collet beaker, lower addition 1mL 3- aminopropyl triethoxysilane is vigorously stirred at 85 DEG C, 2mL, 50mM acetaminophen solution are added after in 10min, is persistently stirred to react 5h, it is final that water-soluble hanced cyan fluorescent silicon is made Quantum dot.
The fluorescence property and characterization of silicon quantum dot
Fig. 1 is influence of the silicon quantum dot holding time to its fluorescence property.It is saved at 4 DEG C 70 days, the fluorescence of silicon quantum dot is strong Degree still reaches the 98.6% of its initial fluorescent intensity, this demonstrate that silicon quantum dot has good stability.
Fig. 2 is influence of the pH value to its fluorescence intensity.In the pH value range of investigation, the fluorescence property of silicon quantum dot does not have Significant change.
Fig. 3 is influence of the ionic strength to silicon quantum dot fluorescence property.Sodium chloride concentration increases to 300mM, silicon quantum dot Fluorescence property it is still not significantly affected.
Fig. 4 is the excitation and emission spectra figure of silicon quantum dot.The best excitation of silicon quantum dot and the position of emission peak are distinguished At 398nm and 495nm.
Fig. 5 is 3- aminopropyl triethoxysilane (APTS), paracetamol (APAP), silicon quantum dot (SiQDs) are red External spectrum.Silicon quantum dot is in 1021cm-1The absorption peak at place is caused by being stretched due to Si-O key chattering, compared with the peak of silane herein It is wide；In 2930cm-1It is due to-CH that absorption peak, which occurs, in place3The stretching vibration of middle c h bond.1590cm-1The absorption peak at place is N-H curved Caused by Qu Zhendong, 3300cm-1It is caused by the stretching vibration of N-H that, which there is absorption in left and right, and absorption herein is compared with paracetamol It is weak, and silane is here substantially without absorption.This proves that water-soluble silicon quantum dot successfully synthesizes.
Highly selective, Sensitive Determination paranitrophenol
0.5mL silicon quantum dot and the PBS buffer solution of 0.2mL, pH=11 are sequentially added in the reaction vessel, are added a certain amount of Paranitrophenol, constant volume 4.00mL measures mixture in excitation wavelength 398nm, launch wavelength 495nm in 25 DEG C of reaction 40min The fluorescence intensity of system.Paranitrophenol concentration is within the scope of 1-80 μM, with fluorescent quenching efficiency (F0- F)/F0Between exist it is preferable Linear relationship (R2=0.9944), linear equation is (F0- F)/F0=0.007C+0.036, wherein F0, F respectively be added to nitro The fluorescence intensity of phenol fore-and-aft architecture, C are the concentration (μM) of paranitrophenol.Measurement is repeated 11 times to 40 μM of paranitrophenols, relatively Standard deviation is 0.9%, and the detection of this method is limited to 0.87 μM.
The highly selective and high anti-interfering performance of measuring method
Sequentially add 0.5mL silicon quantum dot and 0.2mL PBS buffer solution (pH=11) in the reaction vessel, other interfering substances, Constant volume 4.00mL, in 25 DEG C of reaction 40min, in excitation wavelength 398nm, the fluorescence that launch wavelength 495nm measures mixed system is strong Degree.Experimental result measures system to beta naphthal, o-aminophenol, bisphenol-A, 2- nitro as shown in fig. 6, other than paranitrophenol The compounds such as phenol, 3- nitrophenols, para-aminophenol, m-aminophenol, paracetamol, benzoic acid are almost without response.This Show that measuring method can highly selective measurement paranitrophenol.
0.5mL silicon quantum dot and 0.2mL PBS buffer solution (pH=11), same concentrations are sequentially added in the reaction vessel Paranitrophenol and other interfering compounds for example beta naphthal, o-aminophenol, bisphenol-A, 2- nitrophenols, 3- nitrophenols, to amino Phenol, m-aminophenol, paracetamol, benzoic acid etc., constant volume 4.00mL, in 25 DEG C of reaction 40min, in excitation wavelength 398nm, launch wavelength 495nm measure its fluorescence intensity.As shown in fig. 6, the interfering compound investigated hardly is interfered to nitro The measurement of phenol.
Application of the measuring method in measurement water sample in paranitrophenol
The water sample of acquisition has tap water, river water and spring, and water sample is filtered through filter paper, the present invention construct based on water soluble fluorescence silicon The fluorescence analysis of quantum dot does not detect paranitrophenol.Standard addition method the results are shown in Table 1.The rate of recovery that paranitrophenol is added exists Between 97.09%-99.86%, relative standard deviation (RSD) is 0.08%-1.51%.This shows that the silicon quantum dot of this method synthesis is glimmering The detection that light probe is applied to actual water sample paranitrophenol is feasible reliable.
The advantages of water soluble fluorescence silicon quantum dot produced by the present invention and measuring method
Silicon quantum dot simple synthetic method of the invention, reaction condition is mild, and saves (70 days) for a long time still with good Good fluorescence property, or even the fluorescence under different pH(pH=3,4,5,6,7,9,10,11) ionic strength conditions, different It can stablize.
Water soluble fluorescence silicon quantum dot fluorescence probe produced by the present invention is used to detect the content of paranitrophenol in water sample, fastly Fast efficient, selectivity height, high sensitivity.Water-soluble silicon quantum dot fluorescence probe of the invention is only needed with the paranitrophenol reaction time 40min is wanted, it can effective fluorescent quenching.Measurement system to beta naphthal, o-aminophenol, bisphenol-A, 2- nitrophenols, 3- nitrophenols, The compounds such as para-aminophenol, m-aminophenol, paracetamol, benzoic acid are almost without response, it was demonstrated that measuring method Selectivity is high.And beta naphthal, o-aminophenol, bisphenol-A, 2- nitrophenols, 3- nitrophenols, para-aminophenol, m-aminophenol, Paracetamol, benzoic acid etc. do not interfere with silicon quantum dot fluorescence probe of the present invention substantially.Measuring method detection of the present invention Concentration range is 1-80 μM, and detection is limited to 0.87 μM.
1 water soluble fluorescence silicon quantum dot fluorescence probe of table detects paranitrophenol in earth's surface water sample
Basic principle of the invention, main feature and advantage has been shown and described above, is not departing from spirit and scope of the invention Under the premise of, there are also various changes and modifications, these changes and improvements to both fall within the range of claimed invention by the present invention.

Claims (2)

1. a kind of preparation method of water soluble fluorescence silicon quantum dot, it is characterised in that specific steps are as follows: be added in collet beaker 1mL 3- aminopropyl triethoxysilane is added in 5mL ultrapure water under 85 DEG C of intense agitations, in 10min after be added 2mL, The acetaminophen solution of 50mM, is persistently stirred to react 5h, final that water-soluble hanced cyan fluorescent silicon quantum dot is made.
2. water soluble fluorescence silicon quantum dot is in highly selective, Sensitive Determination pair made from the method according to claim 11 Application in nitrophenols concentration, it is characterised in that detailed process are as follows: sequentially add in the reaction vessel 0.5mL silicon quantum dot and The PBS buffer solution of 0.2mL, pH=11, add paranitrophenol to be measured, and constant volume 4.00mL is being excited in 25 DEG C of reaction 40min Wavelength 398nm, launch wavelength 495nm measure mixed system fluorescence intensity, further according to the fluorescence intensity measured and combine linear side Paranitrophenol concentration to be measured is calculated in journey；Paranitrophenol concentration is within the scope of 1-80 μM, with fluorescent quenching efficiency (F0- F)/F0 Between there are preferable linear relationship, R2=0.9944, linear equation is (F0- F)/F0=0.007C+0.036, wherein F0、F difference It is the fluorescence intensity that paranitrophenol fore-and-aft architecture is added, C is the concentration of paranitrophenol, unit μM, to 40 μM of paranitrophenol weight Multiple 11 measurements, relative standard deviation 0.9%, detection are limited to 0.87 μM.
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