CN104007095B - The method of near-infrared luminous quantum dot fluorescence spectrographic determination nanometer gold concentration - Google Patents
The method of near-infrared luminous quantum dot fluorescence spectrographic determination nanometer gold concentration Download PDFInfo
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Abstract
A kind of method that the invention discloses near-infrared luminous quantum dot fluorescence spectrographic determination nanometer gold concentration.Containing near-infrared luminous Ag2S、Ag2Se or Ag2In the system of Te quantum dot, add the nanometer gold to be measured of different volumes, owing to nanometer gold to be measured makes near-infrared luminous Ag2S、Ag2Se or Ag2The fluorescence intensity of Te quantum dot produces regular change, by analyzing near-infrared luminous Ag2S、Ag2Se or Ag2The amount of Te quantum dot point fluorescence intensity change realizes treating the detection by quantitative of nanometer gold concentration；Near-infrared luminous Ag2S、Ag2Se or Ag2Te quantum dot detection range respectively 5.93-27.09 × 10 to nanometer gold-6mol/l、3.39-28.79×10-6Mol/l or 3.39-16.93 × 10-6Mol/l；Its correlation coefficient (r2) respectively 0.9956,0.9954 or 0.9865.The detection method of the present invention is simple to operate, detection is quick, cost is low.
Description
Technical field
A kind of method that the present invention relates to near-infrared luminous quantum dot fluorescence spectrographic determination nanometer gold concentration.
Background technology
Quickly analyzing in detection means, optical detection is one of conventional method, and it has, and information capacity is big, fast response time, the advantage such as highly sensitive, easy and simple to handle, with low cost.In optical detection, an important method is fluorescent spectrometry.Current organic dyestuff is to apply fluorescent material the most general, but its fluorescent characteristics spectrum is wider owing to their excitation spectrum is narrower, and is distributed asymmetric, therefore to detect various ingredients relatively difficult simultaneously.It addition, the greatest drawback of organic dyestuff to be photochemical stability poor.In recent years, quantum dot is due to its special electrical and optical properties, it has also become one of study hotspot of biochemical analysis detection field.Compared with organic fluorescent dye, near infrared fluorescence quantum point has the advantage that (1) fluorescent emission is more stable, and not easily by photobleaching, and its luminescent lifetime is longer, up to ms level；(2) fluorescent emission intensity is high, and spectral peak is narrow, and peak shape is symmetrical；(3) transmitted wave personal attendant particle diameter is adjustable, therefore changes particle diameter and is achieved with multicolor luminous；(4) its excitation spectrum is almost continuous print absorbing more than threshold value, is conducive to multi-wavelength excitation.Thus quantum dot is expected to replace organic dyestuff and is applied to the detection of biological aspect.In current quantum dot has been applied to heavy metal ion content mensuration, disease marker (nucleic acid, galactose etc.) mensuration and drug monitoring etc., but near infrared fluorescence quantum point have not been reported for the research detecting nanoparticle content.
Summary of the invention
It is an object of the invention to provide a kind of method that near-infrared luminous quantum dot fluorescence spectrometry method measures nanometer gold concentration.
The method of the present invention is in the system containing water solublity near infrared fluorescence quantum point, add a certain amount of nanometer gold to be measured, owing to nanometer gold to be measured can make the fluorescence intensity of water-soluble quantum dot produce regular to weaken change, realize treating the detection by quantitative of nanometer gold concentration by analyzing the amount of water-soluble quantum dot fluorescence intensity change.
Concretely comprise the following steps:
(1) it is kept stirring in the system of state in building-up process, by the AgNO of 0.1mol/L3Solution 2-8ml is injected in 100ml deionized water, add the Cys of 0.2-2.0mmol white solid as dressing agent, the sodium hydroxide solution regulation system pH value of rear 1mol/L to be dissolved is to 11, solution system is water white transparency, is subsequently added S source solution that 0.5-4ml concentration is 0.1mol/L, 10-30ml concentration is 5.0 × 10-3The Se source of mol/L or 10-30ml concentration are 5.0 × 10-3The Te source solution of mol/L, namely obtains near-infrared luminous Ag2S、Ag2Se or Ag2Te quantum dot.
(2) being separately added into 1.8-2.4ml concentration in 8-10 volume weight tube is 0.75-1.0 × 10-3The near-infrared luminous Ag of step (1) gained of mol/L2S、Ag2Se or Ag2Te quantum dot, is diluted with phosphoric acid (PBS) buffer solution that pH=8.04, concentration are 0.05mol/L respectively, and being separately added into 0-200ul concentration is 5.08 × 10-4After the nano gold sol of mol/L, more respectively with phosphoric acid (PBS) the buffer solution constant volume that pH=8.04, concentration are 0.05mol/L to 3ml, adopt spectrofluorophotometer detection mixed solution system, obtain the fluorescence spectrum of system, by analyzing near-infrared luminous Ag2S、Ag2Se or Ag2The relation of the Strength Changes at the fluorescent characteristics peak of Te quantum dot and nanometer gold concentration obtains the data of nanometer gold to be detected；Near-infrared luminous Ag2S、Ag2Se or Ag2Te quantum dot detection range respectively 5.93-27.09 × 10 to nanometer gold concentration-6mol/l、3.39-28.79×10-6Mol/l or 3.39-16.93 × 10-6Mol/l；Its correlation coefficient (r2) respectively 0.9956,0.9954 or 0.9865.
Described S source is Na2S·5H2O。
Described Se source is Na2SeO3At NaBH4The NaHSe of the lower preparation of reduction.
Described Te source is Na2TeO3At NaBH4The NaHTe of the lower preparation of reduction.
Se source preparation process is: measure 100ml deionized water, adds 0.0866g (0.5mmol) Na2SeO3, after to be dissolved, add 0.2598gNaBH4, sealing system and temperature are the concentration that at 90 DEG C, reaction obtains is 5.0 × 10-3The Se source of mol/L.
Te source preparation process is: measure 100ml deionized water, adds 0.1108g (0.5mmol) Na2TeO3, after to be dissolved, add 0.3324gNaBH4, sealing system and temperature are the concentration that at 90 DEG C, reaction obtains is 5.0 × 10-3The Te source of mol/L.
The detection method of the present invention is simple to operate, detection is quick, cost is low, can be used for the analysis of nanometer gold detection.
Accompanying drawing explanation
Fig. 1 is the near-infrared luminous Ag obtained by the embodiment of the present invention 12The XRD diffraction pattern of S quantum dot.
Fig. 2 is the near-infrared luminous Ag obtained by the embodiment of the present invention 12The TEM figure of S quantum dot.
Fig. 3 is the near-infrared luminous Ag obtained by the embodiment of the present invention 12S quantum dot and the addition ultraviolet-visible of quantum dot of nanometer gold, fluorescence spectrum figure.
Fig. 4 is the near-infrared luminous Ag obtained by the embodiment of the present invention 12The fluorescent characteristics peak intensity change of S quantum dot and the linear relationship chart of variable concentrations nanometer Au.
Fig. 5 is the near-infrared luminous Ag obtained by the embodiment of the present invention 22The ultraviolet-visible of quantum dot after Se quantum dot and addition nanometer gold, fluorescence spectrum figure.
Fig. 6 is the near-infrared luminous Ag obtained by the embodiment of the present invention 22The fluorescent characteristics peak intensity change of Se quantum dot and the linear relationship chart of variable concentrations nanometer Au.
Fig. 7 is the near-infrared luminous Ag obtained by the embodiment of the present invention 32The ultraviolet-visible of quantum dot after Te quantum dot and addition nanometer gold, fluorescence spectrum figure.
Fig. 8 is the near-infrared luminous Ag obtained by the embodiment of the present invention 32The fluorescent characteristics peak intensity change of Te quantum dot and the linear relationship chart of variable concentrations nanometer gold.
Detailed description of the invention
Embodiment 1:
(1) it is kept stirring in the system of state in building-up process, is the AgNO of 0.1mol/L by 4ml concentration3Solution is injected in 100ml deionized water, adds the Cys of 1.2mmol white solid as dressing agent, and the sodium hydroxide solution regulation system pH value of rear 1mol/L to be dissolved is to 11, and solution system is water white transparency, and adding 1ml concentration is the Na of 0.1mol/L2S·5H2O, obtains henna colloidal sol and near-infrared luminous Ag2S quantum dot, XRD test shows the Ag that gained is near-infrared luminous2S quantum dot is the Ag of monocline crystallographic system2S(is as shown in Figure 1), pattern is spheroidal particle, and in chain between granule, particle diameter is sized to 5nm(and sees Fig. 2).
(2) being separately added into 1.8ml concentration in 10 volume weight tubes is 1.0 × 10-3The Ag that step (1) gained of mol/L is near-infrared luminous2S quantum dot, is diluted with phosphoric acid (PBS) buffer solution that pH=8.04, concentration are 0.05mol/L respectively, be separately added into 0,35,40,50,60,80,100,120,140 and 160ul concentration be 5.08 × 10-4After the nano gold sol of mol/L, again respectively with phosphoric acid (PBS) the buffer solution constant volume that pH=8.04, concentration are 0.05mol/L to 3ml, utilizing fluorescent spectrophotometer assay gained to contain concentration is 0,5.93,6.77,8.47,10.16,13.55,16.93,20.32,23.71,27.09 × 10-6The near-infrared luminous Ag of mol/L nanometer gold2The fluorescence spectrum of S quantum dot, wherein near-infrared luminous Ag2The concentration of S quantum dot is 0.6 × 10-3mol/L。
(3) the near-infrared luminous Ag after being separately added into different volumes nanometer gold in step (2)2The Strength Changes value △ F at the fluorescent characteristics peak (emission peak at 750nm place) of S quantum dot750nmTo concentration mapping (see Fig. 3, Fig. 4) adding nanometer gold, the range of linearity of nanometer gold detection is 5.93-27.09 × 10-6Mol/L, detection is limited to 5.08 × 10-6Mol/L, coefficient R=-0.9978 (r2=0.9956)；Equation of linear regression is △ F750nm=42.88-3.81C。
Embodiment 2:
(1) it is kept stirring in the system of state in building-up process, is the AgNO of 0.1mol/L by 6ml concentration3Solution is injected in 85ml deionized water, adds the Cys of 1.8mmol white solid as dressing agent, and the sodium hydroxide solution regulation system pH value of rear 1mol/L to be dissolved is to 11, and solution system is water white transparency, and adding 15ml concentration is 5.0 × 10-3Namely the Se source of mol/L obtains near-infrared luminous Ag2Se quantum dot colloidal sol.
(2) in 9 volume weight tubes, 2.4ml concentration 0.75 × 10 it is separately added into-3The Ag that step (1) gained of mol/L is near-infrared luminous2Se quantum dot, is diluted with phosphoric acid (PBS) buffer solution that pH=8.04, concentration are 0.05mol/L respectively, be separately added into 0,20,40,80,100,120,140,160 and 170ul concentration be 5.08 × 10-4After the nano gold sol of mol/L, again respectively with phosphoric acid (PBS) the buffer solution constant volume that pH=8.04, concentration are 0.05mol/L to 3ml, utilizing fluorescent spectrophotometer assay gained to contain concentration is 0,3.39,6.77,13.55,16.93,20.32,23.71,27.09 and 28.79 × 10-6The near-infrared luminous Ag of mol/L nanometer gold2The fluorescence spectrum of Se quantum dot, wherein near-infrared luminous Ag2The concentration 0.6 × 10 of Se quantum dot-3mol/L。
(3) step (2) will be separately added into the near-infrared luminous Ag of different volumes nanometer gold2Fluorescent characteristics peak (784nm) the Strength Changes value △ F of Se quantum dot784nmTo concentration mapping (see Fig. 5, Fig. 6) adding nanometer gold, the range of linearity of nanometer gold detection is 3.39-28.79 × 10-6Mol/L, detection is limited to 2.54 × 10-6Mol/L, coefficient R=-0.9977 (r2=0.9954)；Equation of linear regression is △ F784nm=23.03-16.16C。
Described Se source is Na2SeO3At NaBH4The NaHSe of the lower preparation of reduction.
Described Se source preparation process is: measure 100ml deionized water, adds 0.0866g (0.5mmol) Na2SeO3, after to be dissolved, add 0.2598gNaBH4, sealing system and temperature are the concentration that at 90 DEG C, reaction obtains is 5.0 × 10-3The Se source of mol/L.
Embodiment 3:
(1) it is kept stirring in the system of state in building-up process, by the AgNO of 0.1mol/L3Solution 4.5ml(0.45mmol) it is injected in 85ml deionized water, add the Cys of 0.90mmol white solid as dressing agent, the sodium hydroxide solution regulation system pH value of rear 1mol/L to be dissolved is to 11, and solution system is water white transparency, and adding concentration is 5.0 × 10-3The Te source 15mL(0.075mmol of mol/L) namely obtain near-infrared luminous Ag2Te quantum dot colloidal sol.
(2) being separately added into 2.4ml concentration in 8 volume weight tubes is 0.75 × 10-3The near-infrared luminous Ag of step (1) gained of mol/L2Te quantum dot, is diluted with phosphoric acid (PBS) buffer solution that pH=8.04, concentration are 0.05mol/L respectively, be separately added into 0,20,40,50,60,70,80 and 100ul concentration be 5.08 × 10-4After the nano gold sol of mol/L, again respectively with phosphoric acid (PBS) the buffer solution constant volume that pH=8.04, concentration are 0.05mol/L to 3ml, utilizing fluorescent spectrophotometer assay gained to contain concentration is 0,3.39,6.77,8.47,10.16,11.85,13.55 and 16.93 × 10-6The near-infrared luminous Ag of mol/L nanometer gold2The fluorescence spectrum of Te quantum dot, wherein near-infrared luminous Ag2The concentration 0.6 × 10 of Te quantum dot-3mol/L。
(3) step (2) will be separately added into the near-infrared luminous Ag after different volumes nanometer gold2Fluorescent characteristics peak (820nm) the Strength Changes value △ F of Te quantum dot820nmTo concentration mapping (see Fig. 7, Fig. 8) adding nanometer gold, the range of linearity of nanometer gold detection is 3.39-16.93 × 10-6Mol/L, detection is limited to 2.54 × 10-6Mol/L, coefficient R=-0.9932 (r2=0.9865), equation of linear regression is △ F820nm=19.86-3.19C。
Described Te source is Na2TeO3At NaBH4The NaHTe of the lower preparation of reduction.
Described Te source preparation process is: measure 100ml deionized water, adds 0.1108g (0.5mmol) Na2TeO3, after to be dissolved, add 0.3324gNaBH4, sealing system and temperature are the concentration that at 90 DEG C, reaction obtains is 5.0 × 10-3The Te source of mol/L.
Claims (1)
1. the method for a near-infrared luminous quantum dot fluorescence spectrographic determination nanometer gold concentration, it is characterised in that concretely comprise the following steps:
(1) it is kept stirring in the system of state in building-up process, by the AgNO of 0.1mol/L3Solution 2-8ml is injected in 100ml deionized water, add the Cys of 0.2-2.0mmol white solid as dressing agent, the sodium hydroxide solution regulation system pH value of rear 1mol/L to be dissolved is to 11, solution system is water white transparency, is subsequently added S source solution that 0.5-4ml concentration is 0.1mol/L, 10-30ml concentration is 5.0 × 10-3The Se source of mol/L or 10-30ml concentration are 5.0 × 10-3The Te source solution of mol/L, namely obtains near-infrared luminous Ag2S、Ag2Se or Ag2Te quantum dot；
(2) being separately added into 1.8-2.4ml concentration in 8-10 volume weight tube is 0.75-1.0 × 10-3The Ag that step (1) gained of mol/L is near-infrared luminous2S、Ag2Se or Ag2Te quantum dot, is diluted with the phosphate buffer solution that pH=8.04, concentration are 0.05mol/L respectively, and being separately added into 0-200ul concentration is 5.08 × 10-4After the nano gold sol of mol/L different volumes, again respectively with the phosphate buffer solution constant volume that pH=8.04, concentration are 0.05mol/L to 3ml, adopt spectrofluorophotometer detection mixed solution system, obtain the fluorescence spectrum of system, by analyzing near-infrared luminous Ag2S、Ag2Se or Ag2The relation of the Strength Changes at the fluorescent characteristics peak of Te quantum dot and nanometer gold concentration obtains the data of nanometer gold to be detected；Near-infrared luminous Ag2S、Ag2Se or Ag2Te quantum dot detection range respectively 5.93-27.09 × 10 to nanometer gold concentration-6mol/l、3.39-28.79×10-6Mol/l or 3.39-16.93 × 10-6Mol/l；Its linearly dependent coefficient r2Respectively 0.9956,0.9954 or 0.9865；
Described S source is Na2S·5H2O；
Described Se source is Na2SeO3At NaBH4The NaHSe of the lower preparation of reduction；
Described Te source is Na2TeO3At NaBH4The NaHTe of the lower preparation of reduction；
Se source preparation process is: measure 100ml deionized water, adds 0.0866g (0.5mmol) Na2SeO3, after to be dissolved, add 0.2598gNaBH4, sealing system and temperature are the concentration that at 90 DEG C, reaction obtains is 5.0 × 10-3The Se source of mol/L；
Te source preparation process is: measure 100ml deionized water, adds 0.1108g (0.5mmol) Na2TeO3, after to be dissolved, add 0.3324gNaBH4, sealing system and temperature are the concentration that at 90 DEG C, reaction obtains is 5.0 × 10-3The Te source of mol/L.
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| CN106190126B (en) * | 2015-05-04 | 2018-11-06 | 中国科学院苏州纳米技术与纳米仿生研究所 | Monodisperse near-infrared silver telluride quantum dot and preparation method thereof |
| CN106867506B (en) * | 2017-03-07 | 2020-01-07 | 重庆高圣生物医药有限责任公司 | Near-infrared nano fluorescent probe and preparation method thereof |
| CN108441212B (en) * | 2018-03-28 | 2021-04-30 | 苏州星烁纳米科技有限公司 | Preparation method of silver sulfide nanocrystalline |
| CN114854416B (en) * | 2021-01-20 | 2023-06-02 | 中国科学院苏州纳米技术与纳米仿生研究所 | Near-infrared silver-gold-selenium fluorescent quantum dot and preparation method and application thereof |
| CN113620259B (en) * | 2021-07-22 | 2023-05-30 | 先导薄膜材料有限公司 | Ag (silver) alloy 2 Se nano material and preparation method and application thereof |
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Application publication date: 20140827 Assignee: Guangxi shimaoda Technology Co.,Ltd. Assignor: GUILIN University OF TECHNOLOGY Contract record no.: X2022450000494 Denomination of invention: Determination of Gold Nanoparticles by Near Infrared Luminescent Quantum Dot Fluorescence Spectrometry Granted publication date: 20160629 License type: Common License Record date: 20221229 |
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