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 PDFInfo
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Abstract
本发明公开了一种近红外发光量子点荧光光谱法测定纳米金浓度的方法。在含有近红外发光的Ag2S、Ag2Se或Ag2Te量子点的体系中，加入不同体积的待测纳米金，由于待测纳米金使得近红外发光的Ag2S、Ag2Se或Ag2Te量子点的荧光强度产生有规律的变化，通过分析近红外发光的Ag2S、Ag2Se或Ag2Te量子点点荧光强度变化的量来实现对待纳米金浓度的定量检测；近红外发光的Ag2S、Ag2Se或Ag2Te量子点对纳米金的检测范围分别为5.93-27.09×10-6mol/l、3.39-28.79×10-6mol/l或3.39-16.93×10-6mol/l；其相关系数（r2）分别为0.9956、0.9954或0.9865。本发明的检测方法操作简单、检测快速、成本低。
The invention discloses a method for measuring the concentration of nano-gold by near-infrared luminescent quantum dot fluorescence spectrometry. In a system containing near-infrared luminescent Ag 2 S, Ag 2 Se or Ag 2 Te quantum dots, adding different volumes of gold nanoparticles to be tested, the near-infrared luminescent Ag 2 S, Ag 2 Se or The fluorescence intensity of Ag 2 Te quantum dots changes regularly, and the quantitative detection of the concentration of gold nanoparticles is realized by analyzing the amount of fluorescence intensity changes of Ag 2 S, Ag 2 Se or Ag 2 Te quantum dots that emit near-infrared light; near-infrared The detection ranges of luminescent Ag 2 S, Ag 2 Se or Ag 2 Te quantum dots to nano gold are 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; their correlation coefficients (r 2 ) are 0.9956, 0.9954 or 0.9865, respectively. The detection method of the invention is simple in operation, fast in detection and low in cost.
Description
技术领域 technical field
本发明涉及一种近红外发光量子点荧光光谱法测定纳米金浓度的方法。 The invention relates to a method for measuring the concentration of nano-gold by near-infrared luminescence quantum dot fluorescence spectrometry.
背景技术 Background technique
在快速分析检测手段中，光学检测是常用的方法之一，它具有信息容量大、 响应速度快、灵敏度高、操作简便、成本低廉等优点。光学检测中一个重要的方法是荧光光谱法。目前有机染料是应用最为普遍的荧光物质，但由于它们的激发光谱较窄、而其荧光特征谱又较宽，且分布不对称，因此要同时检测多种组分比较困难。另外，有机染料的最大缺陷是光化学稳定性差。近年来，量子点由于其特殊的光学和电学性质， 已成为生化分析检测领域的研究热点之一。与有机荧光染料相比，近红外荧光量子点有以下优点：（1)荧光发射比较稳定，不易被光漂白，且其发光寿命较长，可达ms级；(2)荧光发射强度高，谱峰窄，峰形对称；(3)发射波长随粒径可调，因此改变粒径就可获得多色发光；(4)其激发谱在吸收阈值以上几乎是连续的，有利于多波长激发。因而量子点有望取代有机染料应用于生物方面的检测。目前量子点已被应用于重金属离子含量测定、疾病标志物（如核酸、半乳糖等）测定及药物测定等方面，但近红外荧光量子点用于检测纳米粒子含量的研究还未见报道。 Among the rapid analysis and detection methods, optical detection is one of the commonly used methods, which has the advantages of large information capacity, fast response speed, high sensitivity, easy operation, and low cost. An important method in optical detection is fluorescence spectroscopy. At present, organic dyes are the most commonly used fluorescent substances. However, due to their narrow excitation spectrum, broad fluorescence characteristic spectrum and asymmetric distribution, it is difficult to detect multiple components at the same time. In addition, the biggest defect of organic dyes is poor photochemical stability. In recent years, due to their special optical and electrical properties, quantum dots have become one of the research hotspots in the field of biochemical analysis and detection. Compared with organic fluorescent dyes, near-infrared fluorescent quantum dots have the following advantages: (1) the fluorescence emission is relatively stable, not easy to be photobleached, and its luminescence life is longer, which can reach ms level; (2) the fluorescence emission intensity is high, and the spectrum The peak is narrow and the peak shape is symmetrical; (3) the emission wavelength is adjustable with the particle size, so polychromatic emission can be obtained by changing the particle size; (4) the excitation spectrum is almost continuous above the absorption threshold, which is conducive to multi-wavelength excitation. Therefore, quantum dots are expected to replace organic dyes in biological detection. At present, quantum dots have been used in the determination of heavy metal ion content, disease markers (such as nucleic acid, galactose, etc.) and drug determination, but there is no report on the use of near-infrared fluorescent quantum dots to detect the content of nanoparticles.
发明内容 Contents of the invention
本发明的目的是提供一种近红外发光量子点荧光光谱法定量测定纳米金浓度的方法。 The object of the present invention is to provide a method for quantitatively measuring the concentration of nano-gold by near-infrared luminescent quantum dot fluorescence spectrometry.
本发明的方法是在含有水溶性近红外荧光量子点的体系中，加入一定量的待测纳米金，由于待测纳米金可使水溶性量子点的荧光强度产生有规律的减弱变化，通过分析水溶性量子点荧光强度变化的量来实现对待纳米金浓度的定量检测。 The method of the present invention is to add a certain amount of nano-gold to be tested in the system containing water-soluble near-infrared fluorescent quantum dots, because the nano-gold to be tested can make the fluorescence intensity of the water-soluble quantum dots weaken regularly, and through analysis Quantitative detection of the concentration of gold nanoparticles to be realized by changing the amount of fluorescence intensity of the water-soluble quantum dots.
具体步骤为： The specific steps are:
（1）在合成过程保持搅拌状态的体系中，将0.1mol/L的AgNO3溶液2-8ml注入到100ml去离子水中，加入0.2-2.0mmol白色固体的L-半胱氨酸作为修饰剂，待溶解后用1mol/L的氢氧化钠溶液调节体系pH值至11，溶液体系呈无色透明，随后加入0.5-4ml浓度为0.1mol/L的S源溶液、10-30ml浓度为5.0 × 10-3mol/L的Se源或10-30ml浓度为5.0 × 10-3mol/L的Te源溶液，即得到近红外发光的Ag2S、Ag2Se或Ag2Te量子点。 (1) In the system kept stirring during the synthesis process, inject 2-8ml of 0.1mol/L AgNO 3 solution into 100ml of deionized water, add 0.2-2.0mmol of white solid L-cysteine as a modifier, After dissolving, use 1mol/L sodium hydroxide solution to adjust the pH value of the system to 11, the solution system is colorless and transparent, then add 0.5-4ml of S source solution with a concentration of 0.1mol/L, 10-30ml with a concentration of 5.0 × 10 -3 mol/L Se source or 10-30ml Te source solution with a concentration of 5.0 × 10 -3 mol/L to obtain near-infrared luminescent Ag 2 S, Ag 2 Se or Ag 2 Te quantum dots.
（2）在8-10个容量管中分别加入1.8-2.4 ml浓度为0.75-1.0×10-3mol/L的步骤（1）所得的近红外发光的Ag2S、Ag2Se或Ag2Te量子点，分别用pH=8.04、浓度为0.05mol/L的磷酸（PBS）缓冲溶液进行稀释，分别加入0-200 ul浓度为5.08×10-4mol/L的纳米金溶胶后，再分别用pH=8.04、浓度为0.05mol/L的磷酸（PBS）缓冲溶液定容到3ml，采用荧光分光光度计检测混合溶液体系，得到体系的荧光光谱，通过分析近红外发光Ag2S、Ag2Se或Ag2Te量子点的荧光特征峰的强度变化与纳米金浓度的关系获得待检测纳米金的数据；近红外发光Ag2S、Ag2Se或Ag2Te量子点对纳米金浓度的检测范围分别为5.93-27.09×10-6mol/l、3.39-28.79×10-6mol/l或3.39 - 16.93 ×10-6mol/l；其相关系数（r2）分别为0.9956、0.9954或0.9865。 (2) Add 1.8-2.4 ml of Ag 2 S, Ag 2 Se or Ag 2 with a concentration of 0.75-1.0×10 -3 mol/L obtained in step (1) to 8-10 volumetric tubes respectively Te quantum dots were diluted with phosphoric acid (PBS) buffer solution with a pH=8.04 and a concentration of 0.05 mol/L, respectively, and 0-200 ul of nano-gold sol with a concentration of 5.08×10 -4 mol/L were added, and then respectively Use a phosphoric acid (PBS) buffer solution with a pH=8.04 and a concentration of 0.05mol/L to adjust the volume to 3ml, use a fluorescence spectrophotometer to detect the mixed solution system, obtain the fluorescence spectrum of the system, and analyze the near-infrared luminescent Ag 2 S, Ag 2 The relationship between the intensity change of the fluorescence characteristic peak of Se or Ag 2 Te quantum dots and the concentration of nano-gold to obtain the data of the nano-gold to be detected; the detection of the concentration of nano-gold by near-infrared luminescent Ag 2 S, Ag 2 Se or Ag 2 Te quantum dots The ranges are 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; their correlation coefficients (r 2 ) are 0.9956, 0.9954 or 0.9865, respectively .
所述S源为Na2S·5H2O。 The S source is Na 2 S·5H 2 O.
所述Se源为Na2SeO3在NaBH4的还原下制备的NaHSe。 The Se source is NaHSe prepared by reducing Na 2 SeO 3 with NaBH 4 .
所述Te源为Na2TeO3在NaBH4的还原下制备的NaHTe。 The Te source is NaHTe prepared by reducing Na 2 TeO 3 with NaBH 4 .
Se源制备过程为：量取100ml去离子水，加入0.0866g (0.5mmol) Na2SeO3，待溶解后加入0.2598g NaBH4，密封系统且温度为90℃下反应而得到的浓度为5.0×10-3mol/L的Se源。 The preparation process of Se source is: measure 100ml of deionized water, add 0.0866g (0.5mmol) Na 2 SeO 3 , add 0.2598g NaBH 4 after dissolving, seal the system and react at 90°C to obtain a concentration of 5.0× 10 -3 mol/L Se source.
Te源制备过程为：量取100ml去离子水，加入0.1108g (0.5mmol) Na2TeO3，待溶解后加入0.3324g NaBH4，密封系统且温度为90℃下反应而得到的浓度为5.0×10-3mol/L的Te源。 The preparation process of Te source is: measure 100ml deionized water, add 0.1108g (0.5mmol) Na 2 TeO 3 , add 0.3324g NaBH 4 after dissolving, seal the system and react at 90°C to obtain a concentration of 5.0× 10 -3 mol/L Te source.
本发明的检测方法操作简单、检测快速、成本低，可用于纳米金的分析检测。 The detection method of the invention is simple in operation, fast in detection and low in cost, and can be used for the analysis and detection of nano gold.
附图说明 Description of drawings
图1为本发明实施例1所制得的近红外发光的Ag2S 量子点的XRD衍射图。 FIG. 1 is an XRD diffraction pattern of near-infrared luminescent Ag 2 S quantum dots prepared in Example 1 of the present invention.
图2为本发明实施例1所制得的近红外发光的Ag2S 量子点的TEM图。 FIG. 2 is a TEM image of the near-infrared emitting Ag 2 S quantum dots prepared in Example 1 of the present invention.
图3为本发明实施例1所制得的近红外发光的Ag2S 量子点和加入纳米金的量子点的紫外-可见、荧光光谱图。 Fig. 3 is the ultraviolet-visible and fluorescence spectrum diagrams of the near-infrared luminescent Ag 2 S quantum dots and the quantum dots added with gold nanoparticles prepared in Example 1 of the present invention.
图4为本发明实施例1所制得的近红外发光的Ag2S量子点的荧光特征峰强度变化与不同浓度纳米Au的线性关系图。 FIG. 4 is a graph showing the linear relationship between the intensity change of the fluorescence characteristic peak of the near-infrared luminescent Ag 2 S quantum dots prepared in Example 1 of the present invention and different concentrations of nano-Au.
图5为本发明实施例2所制得的近红外发光的Ag2Se 量子点和加入纳米金后的量子点的紫外-可见、荧光光谱图。 Fig. 5 is the ultraviolet-visible and fluorescence spectrum diagrams of the near-infrared luminescent Ag 2 Se quantum dots prepared in Example 2 of the present invention and the quantum dots added with gold nanoparticles.
图6为本发明实施例2所制得的近红外发光的Ag2Se量子点的荧光特征峰强度变化与不同浓度纳米Au的线性关系图。 Fig. 6 is a graph showing the linear relationship between the intensity change of the fluorescence characteristic peak of the near-infrared luminescent Ag 2 Se quantum dots prepared in Example 2 of the present invention and different concentrations of nano-Au.
图7为本发明实施例3所制得的近红外发光的Ag2Te 量子点和加入纳米金后的量子点的紫外-可见、荧光光谱图。 Fig. 7 is the ultraviolet-visible and fluorescence spectrum diagrams of the near-infrared luminescent Ag 2 Te quantum dots prepared in Example 3 of the present invention and the quantum dots added with gold nanoparticles.
图8为本发明实施例3所制得的近红外发光的Ag2Te量子点的荧光特征峰强度变化与不同浓度纳米金的线性关系图。 Fig. 8 is a graph showing the linear relationship between the intensity change of the fluorescence characteristic peak of the near-infrared luminescent Ag 2 Te quantum dots prepared in Example 3 of the present invention and different concentrations of gold nanoparticles.
具体实施方式 Detailed ways
实施例1：Example 1:
（1）在合成过程保持搅拌状态的体系中，将4ml浓度为0.1mol/L的AgNO3溶液注入到100ml去离子水中，加入1.2mmol白色固体的L-半胱氨酸作为修饰剂，待溶解后用1mol/L的氢氧化钠溶液调节体系pH值至11，溶液体系呈无色透明，加入1ml浓度为0.1mol/L的Na2S·5H2O，得到棕红色的溶胶即近红外发光的Ag2S量子点，XRD测试表明所得近红外发光的Ag2S量子点为单斜结构晶系的Ag2S（如图1所示），形貌为球形颗粒，且颗粒之间呈链状，颗粒直径大小为5 nm（见图2）。 (1) In the system kept stirring during the synthesis process, inject 4ml of AgNO 3 solution with a concentration of 0.1mol/L into 100ml of deionized water, add 1.2mmol of white solid L-cysteine as a modifier, and wait to dissolve Finally, use 1mol/L sodium hydroxide solution to adjust the pH value of the system to 11. The solution system is colorless and transparent. Add 1ml of Na 2 S 5H 2 O with a concentration of 0.1mol/L to obtain a brownish-red sol that emits near-infrared light. XRD test shows that the obtained near-infrared luminescent Ag 2 S quantum dots are Ag 2 S in the monoclinic crystal system (as shown in Figure 1), and the morphology is spherical particles with chains between particles. shape with a particle diameter of 5 nm (see Figure 2).
（2）在10个容量管中分别加入1.8 ml浓度为1.0×10-3mol/L的步骤（1）所得近红外发光的Ag2S量子点，分别用pH=8.04、浓度为0.05mol/L的磷酸（PBS）缓冲溶液进行稀释，分别加入0、35、40、50、60、80、100、120、140和160ul浓度为5.08×10-4mol/L的纳米金溶胶后，再分别用pH=8.04、浓度为0.05mol/L的磷酸（PBS）缓冲溶液定容到3ml，利用荧光分光光度计测定所得含有浓度为0、5.93、6.77、8.47、10.16、13.55、16.93、20.32、23.71、27.09×10-6 mol/L纳米金的近红外发光的Ag2S量子点的荧光光谱，其中近红外发光的Ag2S量子点的浓度为0.6×10-3mol/L。 (2) Add 1.8 ml of Ag 2 S quantum dots with a concentration of 1.0×10 -3 mol/L to 10 volumetric tubes respectively, and use pH=8.04 and a concentration of 0.05 mol/L L of phosphoric acid (PBS) buffer solution was diluted, and 0, 35, 40, 50, 60, 80, 100, 120, 140 and 160ul of nano-gold sol with a concentration of 5.08×10 -4 mol/L were added respectively, and then respectively Use a phosphoric acid (PBS) buffer solution with a pH=8.04 and a concentration of 0.05mol/L to make up to 3ml, and use a fluorescence spectrophotometer to measure the concentration of 0, 5.93, 6.77, 8.47, 10.16, 13.55, 16.93, 20.32, 23.71 , 27.09×10 -6 mol/L fluorescence spectrum of near-infrared luminescent Ag 2 S quantum dots of gold nanoparticles, wherein the concentration of near-infrared luminescent Ag 2 S quantum dots is 0.6×10 -3 mol/L.
（3）在步骤（2）中分别加入不同体积纳米金后的近红外发光的Ag2S量子点的荧光特征峰（750nm处的发射峰）的强度变化值△F750nm对加入纳米金的浓度作图（见图3、图4），纳米金检测的线性范围为5.93-27.09×10-6mol/L，检测限为5.08×10-6 mol/L，相关系数R=-0.9978 (r2=0.9956)；线性回归方程为△F750nm =42.88-3.81C。 (3) The intensity change value of the fluorescence characteristic peak (emission peak at 750nm) of the near-infrared luminescent Ag 2 S quantum dots after adding different volumes of gold nanoparticles in step (2) △F 750nm versus the concentration of gold nanoparticles added Drawing (see Figure 3 and Figure 4), the linear range of gold nanometer detection is 5.93-27.09×10 -6 mol/L, the detection limit is 5.08×10 -6 mol/L, and the correlation coefficient R=-0.9978 (r 2 =0.9956); the linear regression equation is △F 750nm =42.88-3.81C.
the
实施例2：Example 2:
（1）在合成过程保持搅拌状态的体系中，将6ml 浓度为0.1mol/L的AgNO3溶液注入到85ml去离子水中，加入1.8mmol白色固体的L-半胱氨酸作为修饰剂，待溶解后用1mol/L的氢氧化钠溶液调节体系pH值至11，溶液体系呈无色透明，加入15ml浓度为5.0×10-3mol/L的Se源即得到近红外发光的Ag2Se量子点溶胶。 (1) In the system that was kept stirring during the synthesis process, inject 6ml of AgNO 3 solution with a concentration of 0.1mol/L into 85ml of deionized water, add 1.8mmol of white solid L-cysteine as a modifier, and wait to dissolve Finally, adjust the pH value of the system to 11 with 1mol/L sodium hydroxide solution, the solution system is colorless and transparent, add 15ml of Se source with a concentration of 5.0× 10-3 mol/L to obtain near-infrared luminescent Ag 2 Se quantum dots Sol.
（2）在9个容量管中分别加入2.4ml浓度0.75×10-3mol/L的步骤（1）所得近红外发光的Ag2Se量子点，分别用pH=8.04、浓度为0.05mol/L的磷酸（PBS）缓冲溶液进行稀释，分别加入0、20、40、80、100、120、140、160和170ul浓度为5.08×10-4mol/L的纳米金溶胶后，再分别用pH=8.04、浓度为0.05mol/L的磷酸（PBS）缓冲溶液定容到3ml，利用荧光分光光度计测定所得含有浓度为0、3.39、6.77、13.55、16.93、20.32、23.71、27.09和28.79×10-6 mol/L纳米金的近红外发光的Ag2Se量子点的荧光光谱，其中近红外发光的Ag2Se量子点的浓度0.6×10-3mol/L。 (2) Add 2.4ml of Ag 2 Se quantum dots with a concentration of 0.75×10 -3 mol/L to 9 volumetric tubes respectively. Phosphoric acid (PBS) buffer solution was diluted, and 0, 20, 40, 80, 100, 120, 140, 160 and 170ul of nano-gold sol with a concentration of 5.08×10 -4 mol/L were added respectively, and then pH = 8.04. Dilute the phosphoric acid (PBS) buffer solution with a concentration of 0.05mol/L to 3ml, and use a fluorescence spectrophotometer to measure the concentration of 0, 3.39, 6.77, 13.55, 16.93, 20.32, 23.71, 27.09 and 28.79×10 - Fluorescence spectrum of near-infrared-emitting Ag 2 Se quantum dots of 6 mol/L nano-gold, wherein the concentration of near-infrared-emitting Ag 2 Se quantum dots is 0.6×10 -3 mol/L.
（3）将步骤（2）中分别加入不同体积纳米金的近红外发光的Ag2Se量子点的荧光特征峰（784nm）强度变化值△F784nm对加入纳米金的浓度作图（见图5、图6）， 纳米金检测的线性范围为3.39-28.79×10-6mol/L，检测限为2.54×10-6mol/L，相关系数R=-0.9977 (r2=0.9954)；线性回归方程为△F784nm =23.03-16.16C。 (3) In step (2), the intensity change value of the characteristic peak (784nm) of the fluorescence characteristic peak ( 784nm ) of Ag 2 Se quantum dots with different volumes of gold nanoparticles added in the step (2) is plotted against the concentration of gold nanoparticles added (see Figure 5 , Figure 6), the linear range of nano-gold detection is 3.39-28.79×10 -6 mol/L, the detection limit is 2.54×10 -6 mol/L, the correlation coefficient R=-0.9977 (r 2 =0.9954); linear regression The equation is ΔF 784nm =23.03-16.16C.
所述Se源为Na2SeO3在NaBH4的还原下制备的NaHSe。 The Se source is NaHSe prepared by reducing Na 2 SeO 3 with NaBH 4 .
所述Se源制备过程为：量取100ml去离子水，加入0.0866g (0.5mmol) Na2SeO3，待溶解后加入0.2598g NaBH4，密封系统且温度为90℃下反应而得到的浓度为5.0×10-3mol/L的Se源。 The preparation process of the Se source is as follows: measure 100ml of deionized water, add 0.0866g (0.5mmol) Na 2 SeO 3 , add 0.2598g NaBH 4 after dissolving, seal the system and react at a temperature of 90°C to obtain a concentration of 5.0×10 -3 mol/L Se source.
实施例3：Example 3:
（1）在合成过程保持搅拌状态的体系中，将0.1mol/L的AgNO3溶液4.5ml（0.45mmol）注入到85ml去离子水中，加入0.90mmol白色固体的L-半胱氨酸作为修饰剂，待溶解后用1mol/L的氢氧化钠溶液调节体系pH值至11，溶液体系呈无色透明，加入浓度为5.0×10-3mol/L的Te源15mL（0.075mmol）即得到近红外发光的Ag2Te量子点溶胶。 (1) In the system kept stirring during the synthesis process, inject 4.5ml (0.45mmol) of 0.1mol/L AgNO 3 solution into 85ml of deionized water, and add 0.90mmol of white solid L-cysteine as a modifier , after being dissolved, use 1mol/L sodium hydroxide solution to adjust the pH value of the system to 11. The solution system is colorless and transparent. Add 15mL (0.075mmol) of Te source with a concentration of 5.0×10 -3 mol/L to obtain near-infrared Luminescent Ag 2 Te quantum dot sol.
（2）在8个容量管中分别加入2.4ml浓度为0.75×10-3mol/L的步骤（1）所得的近红外发光的Ag2Te量子点，分别用pH=8.04、浓度为0.05mol/L的磷酸（PBS）缓冲溶液进行稀释，分别加入0、20、40、50、60、70、80和100ul浓度为5.08×10-4mol/L的纳米金溶胶后，再分别用pH=8.04、浓度为0.05mol/L的磷酸（PBS）缓冲溶液定容到3ml，利用荧光分光光度计测定所得含有浓度为0、3.39、6.77、8.47、10.16、11.85、13.55和16.93×10-6 mol/L纳米金的近红外发光的Ag2Te量子点的荧光光谱，其中近红外发光的Ag2Te量子点的浓度0.6×10-3mol/L。 (2) Add 2.4ml of the near-infrared luminescent Ag 2 Te quantum dots obtained in the step (1) with a concentration of 0.75×10 -3 mol/L to 8 volumetric tubes, respectively, with pH=8.04 and a concentration of 0.05mol /L phosphoric acid (PBS) buffer solution to dilute, add 0, 20, 40, 50, 60, 70, 80 and 100ul nano-gold sol with a concentration of 5.08×10 -4 mol/L respectively, and then use pH= 8.04. Dilute the phosphoric acid (PBS) buffer solution with a concentration of 0.05mol/L to 3ml, and use a fluorescence spectrophotometer to measure the concentration of 0, 3.39, 6.77, 8.47, 10.16, 11.85, 13.55 and 16.93×10 -6 mol Fluorescence spectrum of near-infrared luminescent Ag 2 Te quantum dots of /L nano-gold, wherein the concentration of near-infrared luminescent Ag 2 Te quantum dots is 0.6×10 -3 mol/L.
（3）将步骤（2）中分别加入不同体积纳米金后的近红外发光的Ag2Te量子点的荧光特征峰（820nm）强度变化值△F820nm对加入纳米金的浓度作图（见图7、图8），纳米金检测的线性范围为3.39-16.93×10-6 mol/L，检测限为2.54×10-6mol/L，相关系数R = -0.9932 (r2=0.9865)，线性回归方程为△F820nm =19.86-3.19C。 (3) After adding different volumes of gold nanoparticles in step (2), the intensity change value of the fluorescence characteristic peak (820nm) of the Ag 2 Te quantum dots emitting near-infrared light ( 820nm ) is plotted against the concentration of gold nanoparticles added (see Fig. 7. Figure 8), the linear range of nano-gold detection is 3.39-16.93×10 -6 mol/L, the detection limit is 2.54×10 -6 mol/L, the correlation coefficient R = -0.9932 (r 2 =0.9865), linear The regression equation is △F 820nm =19.86-3.19C.
所述Te源为Na2TeO3在NaBH4的还原下制备的NaHTe。 The Te source is NaHTe prepared by reducing Na 2 TeO 3 with NaBH 4 .
所述Te源制备过程为：量取100ml去离子水，加入0.1108g (0.5mmol) Na2TeO3，待溶解后加入0.3324g NaBH4，密封系统且温度为90℃下反应而得到的浓度为5.0×10-3mol/L的Te源。 The preparation process of the Te source is as follows: measure 100ml of deionized water, add 0.1108g (0.5mmol) Na 2 TeO 3 , add 0.3324g NaBH 4 after dissolving, seal the system and react at a temperature of 90°C to obtain a concentration of 5.0×10 -3 mol/L Te source.
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