CN104007095A - Method for measuring concentration of nanogold by adopting near infrared luminescent quantum dot fluorescent spectrometry - Google Patents

Method for measuring concentration of nanogold by adopting near infrared luminescent quantum dot fluorescent spectrometry Download PDF

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CN104007095A
CN104007095A CN201410237382.XA CN201410237382A CN104007095A CN 104007095 A CN104007095 A CN 104007095A CN 201410237382 A CN201410237382 A CN 201410237382A CN 104007095 A CN104007095 A CN 104007095A
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CN104007095B (en
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覃爱苗
吴秀兰
杜为林
廖雷
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Guilin University of Technology
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Abstract

The invention discloses a method for measuring the concentration of nanogold by adopting near infrared luminescent quantum dot fluorescent spectrometry. Different volumes of nanogolds to be measured are added into a system containing near infrared luminescent Ag2S, Ag2Se or Ag2Te quantum dots, the fluorescence intensity of the near infrared luminescent Ag2S, Ag2Se or Ag2Te quantum dots is regularly changed by the nanogolds to be measured, and the changing strength in the fluorescent intensity of the near infrared luminescent Ag2S, Ag2Se or Ag2Te quantum dots are analyzed to quantitatively detect the concentration of the nanogolds to be measured, wherein the range of detection of the near infrared luminescent Ag2S, Ag2Se or Ag2Te quantum dots over the nanogolds is (5.93-27.09)*10<-6>mol/l, (3.39-28.79)*10<-6>mol/l or (3.39-16.93)*10<-6>mol/l; a related coefficient (r<2>) is 0.9956, 0.9954 or 0.9865. According to the detection method, the operation is easy, the detection is quick and the cost is low.

Description

The method of near-infrared luminous quantum dot fluorescence spectrographic determination nm of gold concentration
Technical field
The present invention relates to a kind of method of near-infrared luminous quantum dot fluorescence spectrographic determination nm of gold concentration.
Background technology
In express-analysis detection means, optical detection is one of conventional method, and it has, and information capacity is large, 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.At present organic dyestuff is to apply the most general fluorescent material, but because their excitation spectrum is compared with narrow and its fluorescent characteristics spectrum is wider, and it is asymmetric to distribute, and therefore will detect various ingredients more difficult simultaneously.In addition, the greatest drawback of organic dyestuff is that photochemical stability is poor.In recent years, quantum dot, due to its special electrical and optical properties, has become one of study hotspot of biochemical analysis detection field.Compared with organic fluorescent dye, near infrared fluorescence quantum point has following advantage: (1) fluorescent emission is more stable, be difficult for by photobleaching, and its luminescent lifetime is longer, can reach ms level; (2) fluorescent emission intensity is high, and spectrum peak is narrow, peak shape symmetry; (3) emission wavelength is adjustable with particle diameter, therefore changes particle diameter and just can obtain multicolor luminous; (4) its excitation spectrum is almost continuous absorbing more than threshold value, is conducive to multi-wavelength excitation.Thereby quantum dot is expected to replace organic dyestuff and is applied to the detection of biological aspect.Quantum dot has been applied to the aspects such as heavy metal ion content mensuration, disease marker (as nucleic acid, galactose etc.) mensuration and drug monitoring at present, but near infrared fluorescence quantum point have not been reported for detection of the research of nanoparticle content.
Summary of the invention
The object of this invention is to provide a kind of method of near-infrared luminous quantum dot fluorescence spectroscopic methodology quantitative measurement nm of gold concentration.
Method of the present invention is in the system that contains water-soluble near infrared fluorescence quantum point, add a certain amount of nm of gold to be measured, produce the regular variation that weakens because nm of gold to be measured can make the fluorescence intensity of water-soluble quantum dot, realize by the amount of analyzing water-soluble quantum dot fluorescence intensity change the quantitative detection for the treatment of nm of gold concentration.
Concrete steps are:
(1) keep in the system of stirring, by the AgNO of 0.1mol/L in building-up process 3solution 2-8ml is injected in 100ml deionized water, add the Cys of 0.2-2.0mmol white solid as dressing agent, the rear sodium hydroxide solution regulation system pH value to 11 with 1mol/L to be dissolved, solution system is water white transparency, and adding subsequently 0.5-4ml concentration is that S source solution, the 10-30ml concentration of 0.1mol/L 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, obtains near-infrared luminous Ag 2s, Ag 2se or Ag 2te quantum dot.
(2) in 8-10 volume weight tube, adding respectively 1.8-2.4 ml concentration is 0.75-1.0 × 10 -3the near-infrared luminous Ag of step (1) gained of mol/L 2s, Ag 2se or Ag 2phosphoric acid (PBS) buffer solution that Te quantum dot is 0.05mol/L by pH=8.04, concentration respectively dilutes, and adding respectively 0-200 ul concentration is 5.08 × 10 -4after the nano gold sol of mol/L, then phosphoric acid (PBS) the buffer solution constant volume that is 0.05mol/L by pH=8.04, concentration is respectively to 3ml, adopts fluorospectrophotometer to detect mixed solution system, obtains the fluorescence spectrum of system, by analyzing near-infrared luminous Ag 2s, Ag 2se or Ag 2the Strength Changes at the fluorescent characteristics peak of Te quantum dot and the relation of nm of gold concentration obtain the data of nm of gold to be detected; Near-infrared luminous Ag 2s, Ag 2se or Ag 2te quantum dot is respectively 5.93-27.09 × 10 to the sensing range of nm of gold concentration -6mol/l, 3.39-28.79 × 10 -6mol/l or 3.39-16.93 × 10 -6mol/l; Its related coefficient (r 2) be respectively 0.9956,0.9954 or 0.9865.
Described S source is Na 2s5H 2o.
Described Se source is Na 2seO 3at NaBH 4reduction under the NaHSe for preparing.
Described Te source is Na 2teO 3at NaBH 4reduction under the NaHTe for preparing.
Se source preparation process is: measure 100ml deionized water, add 0.0866g (0.5mmol) Na 2seO 3, add 0.2598g NaBH after to be dissolved 4, sealing system and temperature are that 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, add 0.1108g (0.5mmol) Na 2teO 3, add 0.3324g NaBH after to be dissolved 4, sealing system and temperature are that the concentration that at 90 DEG C, reaction obtains is 5.0 × 10 -3the Te source of mol/L.
Detection method of the present invention is simple to operate, detection is quick, cost is low, can be used for the analyzing and testing of nm of gold.
Brief description of the drawings
Fig. 1 is the prepared near-infrared luminous Ag of the embodiment of the present invention 1 2the XRD diffractogram of S quantum dot.
Fig. 2 is the prepared near-infrared luminous Ag of the embodiment of the present invention 1 2the TEM figure of S quantum dot.
Fig. 3 is the prepared near-infrared luminous Ag of the embodiment of the present invention 1 2s quantum dot and add ultraviolet-visible, the fluorescence spectrum figure of quantum dot of nm of gold.
Fig. 4 is the prepared near-infrared luminous Ag of the embodiment of the present invention 1 2the fluorescent characteristics peak intensity of S quantum dot changes the linear relationship chart with variable concentrations nanometer Au.
Fig. 5 is the prepared near-infrared luminous Ag of the embodiment of the present invention 2 2se quantum dot and the ultraviolet-visible, the fluorescence spectrum figure that add the quantum dot after nm of gold.
Fig. 6 is the prepared near-infrared luminous Ag of the embodiment of the present invention 2 2the fluorescent characteristics peak intensity of Se quantum dot changes the linear relationship chart with variable concentrations nanometer Au.
Fig. 7 is the prepared near-infrared luminous Ag of the embodiment of the present invention 3 2te quantum dot and the ultraviolet-visible, the fluorescence spectrum figure that add the quantum dot after nm of gold.
Fig. 8 is the prepared near-infrared luminous Ag of the embodiment of the present invention 3 2the fluorescent characteristics peak intensity of Te quantum dot changes the linear relationship chart with variable concentrations nm of gold.
Embodiment
embodiment 1:
(1) keep in the system of stirring the AgNO that is 0.1mol/L by 4ml concentration in building-up process 3solution is injected in 100ml deionized water, adds the Cys of 1.2mmol white solid as dressing agent, the rear sodium hydroxide solution regulation system pH value to 11 with 1mol/L to be dissolved, and solution system is water white transparency, and adding 1ml concentration is the Na of 0.1mol/L 2s5H 2o, obtaining henna colloidal sol is near-infrared luminous Ag 2s quantum dot, XRD test shows the Ag that gained is near-infrared luminous 2s quantum dot is the Ag of monocline crystallographic system 2s(is as shown in Figure 1), pattern is spheric grain, and between particle, is chain, particle diameter size is that 5 nm(are shown in Fig. 2).
(2) in 10 volume weight tubes, adding respectively 1.8 ml concentration is 1.0 × 10 -3the near-infrared luminous Ag of step (1) gained of mol/L 2phosphoric acid (PBS) buffer solution that S quantum dot is 0.05mol/L by pH=8.04, concentration respectively dilutes, add respectively 0,35,40,50,60,80,100,120,140 and 160ul concentration be 5.08 × 10 -4after the nano gold sol of mol/L, phosphoric acid (PBS) the buffer solution constant volume that is 0.05mol/L by pH=8.04, concentration respectively is again to 3ml, and 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 nm of gold 2the fluorescence spectrum of S quantum dot, wherein near-infrared luminous Ag 2the concentration of S quantum dot is 0.6 × 10 -3mol/L.
(3) in step (2), add respectively the near-infrared luminous Ag after different volumes nm of gold 2the Strength Changes value △ F at the fluorescent characteristics peak (emission peak at 750nm place) of S quantum dot 750nmto adding the concentration mapping (seeing Fig. 3, Fig. 4) of nm of gold, the range of linearity that nm of gold detects is 5.93-27.09 × 10 -6mol/L, detects and is limited to 5.08 × 10 -6mol/L, coefficient R=-0.9978 (r 2=0.9956); Equation of linear regression is △ F 750nm=42.88-3.81C.
 
embodiment 2:
(1) keep in the system of stirring the AgNO that is 0.1mol/L by 6ml concentration in building-up process 3solution is injected in 85ml deionized water, adds the Cys of 1.8mmol white solid as dressing agent, the rear sodium hydroxide solution regulation system pH value to 11 with 1mol/L to be dissolved, and solution system is water white transparency, and adding 15ml concentration is 5.0 × 10 -3the Se source of mol/L obtains near-infrared luminous Ag 2se quantum dot colloidal sol.
(2) in 9 volume weight tubes, add respectively 2.4ml concentration 0.75 × 10 -3the near-infrared luminous Ag of step (1) gained of mol/L 2phosphoric acid (PBS) buffer solution that Se quantum dot is 0.05mol/L by pH=8.04, concentration respectively dilutes, add respectively 0,20,40,80,100,120,140,160 and 170ul concentration be 5.08 × 10 -4after the nano gold sol of mol/L, phosphoric acid (PBS) the buffer solution constant volume that is 0.05mol/L by pH=8.04, concentration respectively is again to 3ml, and 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 nm of gold 2the fluorescence spectrum of Se quantum dot, wherein near-infrared luminous Ag 2the concentration 0.6 × 10 of Se quantum dot -3mol/L.
(3) the near-infrared luminous Ag of different volumes nm of gold will be added respectively in step (2) 2fluorescent characteristics peak (784nm) the Strength Changes value △ F of Se quantum dot 784nmto adding the concentration mapping (seeing Fig. 5, Fig. 6) of nm of gold, the range of linearity that nm of gold detects is 3.39-28.79 × 10 -6mol/L, detects and is limited to 2.54 × 10 -6mol/L, coefficient R=-0.9977 (r 2=0.9954); Equation of linear regression is △ F 784nm=23.03-16.16C.
Described Se source is Na 2seO 3at NaBH 4reduction under the NaHSe for preparing.
Described Se source preparation process is: measure 100ml deionized water, add 0.0866g (0.5mmol) Na 2seO 3, add 0.2598g NaBH after to be dissolved 4, sealing system and temperature are that the concentration that at 90 DEG C, reaction obtains is 5.0 × 10 -3the Se source of mol/L.
embodiment 3:
(1) keep in the system of stirring, by the AgNO of 0.1mol/L in building-up process 3solution 4.5ml(0.45mmol) be injected in 85ml deionized water, add the Cys of 0.90mmol white solid as dressing agent, the rear sodium hydroxide solution regulation system pH value to 11 with 1mol/L to be dissolved, solution system is water white transparency, and adding concentration is 5.0 × 10 -3the Te source 15mL(0.075mmol of mol/L) obtain near-infrared luminous Ag 2te quantum dot colloidal sol.
(2) in 8 volume weight tubes, adding respectively 2.4ml concentration is 0.75 × 10 -3the near-infrared luminous Ag of step (1) gained of mol/L 2phosphoric acid (PBS) buffer solution that Te quantum dot is 0.05mol/L by pH=8.04, concentration respectively dilutes, add respectively 0,20,40,50,60,70,80 and 100ul concentration be 5.08 × 10 -4after the nano gold sol of mol/L, phosphoric acid (PBS) the buffer solution constant volume that is 0.05mol/L by pH=8.04, concentration respectively is again to 3ml, and 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 nm of gold 2the fluorescence spectrum of Te quantum dot, wherein near-infrared luminous Ag 2the concentration 0.6 × 10 of Te quantum dot -3mol/L.
(3) the near-infrared luminous Ag after different volumes nm of gold will be added respectively in step (2) 2fluorescent characteristics peak (820nm) the Strength Changes value △ F of Te quantum dot 820nmto adding the concentration mapping (seeing Fig. 7, Fig. 8) of nm of gold, the range of linearity that nm of gold detects is 3.39-16.93 × 10 -6mol/L, detects and is limited to 2.54 × 10 -6mol/L, coefficient R=-0.9932 (r 2=0.9865), equation of linear regression is △ F 820nm=19.86-3.19C.
Described Te source is Na 2teO 3at NaBH 4reduction under the NaHTe for preparing.
Described Te source preparation process is: measure 100ml deionized water, add 0.1108g (0.5mmol) Na 2teO 3, add 0.3324g NaBH after to be dissolved 4, sealing system and temperature are that the concentration that at 90 DEG C, reaction obtains is 5.0 × 10 -3the Te source of mol/L.

Claims (1)

1. a method for near-infrared luminous quantum dot fluorescence spectrographic determination nm of gold concentration, is characterized in that concrete steps are:
(1) keep in the system of stirring, by the AgNO of 0.1mol/L in building-up process 3solution 2-8ml is injected in 100ml deionized water, add the Cys of 0.2-2.0mmol white solid as dressing agent, the rear sodium hydroxide solution regulation system pH value to 11 with 1mol/L to be dissolved, solution system is water white transparency, and adding subsequently 0.5-4ml concentration is that S source solution, the 10-30ml concentration of 0.1mol/L 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, obtains near-infrared luminous Ag 2s, Ag 2se or Ag 2te quantum dot;
(2) in 8-10 volume weight tube, adding respectively 1.8-2.4 ml concentration is 0.75-1.0 × 10 -3the near-infrared luminous Ag of step (1) gained of mol/L 2s, Ag 2se or Ag 2te quantum dot, dilutes with the phosphate buffer solution that pH=8.04, concentration are 0.05mol/L respectively, and adding respectively 0-200 ul concentration is 5.08 × 10 -4after the nano gold sol of mol/L, then the phosphate buffer solution constant volume that is 0.05mol/L by pH=8.04, concentration is respectively to 3ml, adopts fluorospectrophotometer to detect mixed solution system, obtains the fluorescence spectrum of system, by analyzing near-infrared luminous Ag 2s, Ag 2se or Ag 2the Strength Changes at the fluorescent characteristics peak of Te quantum dot and the relation of nm of gold concentration obtain the data of nm of gold to be detected; Near-infrared luminous Ag 2s, Ag 2se or Ag 2te quantum dot is respectively 5.93-27.09 × 10 to the sensing range of nm of gold concentration -6mol/l, 3.39-28.79 × 10 -6mol/l or 3.39-16.93 × 10 -6mol/l; Its correlation coefficient r 2be respectively 0.9956,0.9954 or 0.9865;
Described S source is Na 2s5H 2o;
Described Se source is Na 2seO 3at NaBH 4reduction under the NaHSe for preparing;
Described Te source is Na 2teO 3at NaBH 4reduction under the NaHTe for preparing;
Se source preparation process is: measure 100ml deionized water, add 0.0866g (0.5mmol) Na 2seO 3, add 0.2598g NaBH after to be dissolved 4, sealing system and temperature are that 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, add 0.1108g (0.5mmol) Na 2teO 3, add 0.3324g NaBH after to be dissolved 4, sealing system and temperature are that the concentration that at 90 DEG C, reaction obtains is 5.0 × 10 -3the Te source of mol/L.
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CN106190126A (en) * 2015-05-04 2016-12-07 中国科学院苏州纳米技术与纳米仿生研究所 Single dispersing near-infrared silver telluride quantum dot and preparation method thereof
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CN114854416A (en) * 2021-01-20 2022-08-05 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
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
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