CN107607508B - Method for detecting trivalent gold ions by using water-soluble fluorescent compound - Google Patents
Method for detecting trivalent gold ions by using water-soluble fluorescent compound Download PDFInfo
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- CN107607508B CN107607508B CN201710814257.4A CN201710814257A CN107607508B CN 107607508 B CN107607508 B CN 107607508B CN 201710814257 A CN201710814257 A CN 201710814257A CN 107607508 B CN107607508 B CN 107607508B
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Abstract
A method for detecting trivalent gold ions by using a water-soluble fluorescent compound comprises the steps of detecting trivalent gold ions with different concentrations by using TPCANa aqueous solution to obtain corresponding fluorescence curves; relative fluorescence intensity (F) with trivalent gold ion concentration as abscissa0‑F)/F0Obtaining a standard curve of the concentration of the TPCANa detected trivalent gold ions as a vertical coordinate; according to the standard curve, the linear regression equation is as follows within the range of 40-175 mu mol/L: (F)0‑F)/F00.00688C-0.28209, when a sample containing trivalent gold ions is detected, different fluorescence intensities of TPCANa aqueous solution for the trivalent gold ions with different concentrations are detected, and the linear regression equation is substituted to obtain the concentration of the trivalent gold ions. The salt synthesized by the invention has the advantages of good selectivity, wide linear range, high sensitivity, simple synthesis method, excellent water solubility and the like for identifying the trivalent gold ions.
Description
Technical Field
The invention relates to Au3+A detection and analysis technology, in particular to a method for detecting trivalent gold ions by using a water-soluble fluorescent compound.
Background
Gold is a noble metal, has wide application in various fields such as catalysis, selective oxidation, nano diagnosis and detection, and mainly exists in the form of Au (III) in water. Although simple gold substance is inert, gold ions in gold salt can interact with enzyme and DNA, so that the gold salt has potential toxicity to human bodies and can damage liver, kidney and peripheral nervous systems, and therefore, the construction of a high-selectivity and high-sensitivity detection method for trivalent gold ions is very important. However, the existing trivalent gold ion detection method is mainly based on organic molecular fluorescent probes, the synthesis process of the probes is complicated and difficult to produce in large quantities, and most of the probes need to be carried out in an organic phase or a semi-aqueous phase, so that the application of the probes in trivalent gold ion detection is limited.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a method for detecting trivalent gold ions by using a water-soluble fluorescent compound.
In order to achieve the purpose, the invention adopts the technical scheme that:
a method for detecting trivalent gold ions by using water-soluble fluorescent compounds comprises detecting trivalent gold ions with different concentrations by using TPCANa aqueous solution to obtain corresponding fluorescence curve,then, the fluorescence intensity (F) was measured with the concentration of trivalent gold ion as the abscissa0-F)/F0Obtaining a standard curve of the concentration of the TPCANa detected trivalent gold ions as a vertical coordinate; according to the standard curve, the linear regression equation is as follows within the range of 40-175 mu mol/L: (F)0-F)/F00.00688C-0.28209, wherein C is the concentration of trivalent gold ion, F0Fluorescence intensity of a blank control group of TPCANa in 50 mu mol/L aqueous solution, and detection of Au with different concentrations by F in 50 mu mol/L TPCANa aqueous solution3+The fluorescence intensity of (a);
when a sample containing the trivalent gold ions is detected, the TPCANa aqueous solution detects different fluorescence intensities of the trivalent gold ions with different concentrations, and the different fluorescence intensities are substituted into a linear regression equation to obtain the concentration of the trivalent gold ions.
In a further development of the invention, TPCANa is prepared by the following method: adding TPCA into NaOH solution to obtain TPCANa aqueous solution, adding the aqueous solution into absolute ethyl alcohol, separating out precipitate, filtering, and drying to obtain TPCANa.
The further improvement of the invention is that the concentration of the sodium hydroxide solution is 0.5 mol/L-1.0 mol/L.
A further improvement of the invention is that the volume ratio of the aqueous solution to the absolute ethanol is 1: 10.
The invention is further improved in that the molar ratio of TPCA to NaOH is 1: 1-5.
A further improvement of the invention is that the molar ratio of TPCA to NaOH is 1: 3.
Compared with the prior art, the invention has the beneficial effects that: the invention adopts TPCANa aqueous solution to detect the trivalent gold ions with different concentrations to obtain corresponding fluorescence curves, and then takes the concentration of the trivalent gold ions as the abscissa and the relative fluorescence intensity (F)0-F)/F0Obtaining a standard curve of the concentration of the TPCANa detected trivalent gold ions as a vertical coordinate; the linear regression equation is obtained according to the standard curve in the range of 40-175 mu mol/L: (F)0-F)/F00.00688C-0.28209, wherein C is the concentration of trivalent gold ion, F0Fluorescence intensity of 50. mu. mol/L TPCANa blank control group, F of 50. mu. mol/L TPCANa aqueous solutionMeasuring Au of different concentrations3+The fluorescence intensity of (a); when a sample containing trivalent gold ions is detected, the TPCANa fluorescent probe (TPCANa aqueous solution) detects the trivalent gold ions with different concentrations to obtain different fluorescence intensities, and the different fluorescence intensities are substituted into a linear regression equation to obtain the concentration of the trivalent gold ions. The salt compound is used as a probe, and the method has good selectivity for identifying trivalent gold ions and wide linear range. The fluorescent probe can be used for directly detecting Au in a water phase3+And need not be carried out in the organic phase.
Furthermore, the synthesis method of TPCANa is simple, TPCA and NaOH react in water and then precipitate out a product in ethanol, the obtained product has excellent water solubility, the synthesis method is non-toxic, the cost is low, the fluorescence yield is high, and the product is easy to store and transport.
Drawings
FIG. 1 is a diagram of the excitation/emission spectrum of TPCANa, a synthetic material of the present invention.
FIG. 2 is a photoluminescence map of the synthetic material TPCANa of the present invention.
FIG. 3 is a fluorescence emission diagram of the interaction of TPCANa and trivalent gold ions as a synthetic material of the present invention.
FIG. 4 is a fluorescent histogram of the interaction of synthetic material TPCANa of the present invention with various cations.
FIG. 5 shows the fluorescence intensity of TPCANa, a synthetic material of the invention, at different pH values.
FIG. 6 is a linear curve obtained by the present invention.
Detailed Description
The present invention will be described in detail with reference to the accompanying drawings.
The invention prepares TPCANa: adding TPCA into an aqueous solution of sodium hydroxide for reaction to obtain a salt solution, transferring the salt solution into an organic solvent in an ice-water bath to precipitate, filtering and drying at 95-105 ℃ to obtain a final salt product, namely TPCANa, wherein the molar ratio of TPCA to NaOH is 1: 1-5, preferably 1:3, the concentration of the aqueous solution of sodium hydroxide is 0.5-1.0 mol/L, and the organic solvent is absolute ethyl alcohol. The volume ratio of the aqueous solution of the salt compound to the organic solvent is 1: 10. The structural formula of the salt product is as follows:
the method for detecting the trivalent gold ions by adopting TPCANa comprises the following steps:
a. detecting trivalent gold ions: 250mL of a 0.5mmol/L aqueous TPCANa solution was prepared, and the solution was diluted to 0 to 200. mu. mol/L for fluorometry. The specific diluted concentrations were: (10. mu. mol/L, 20. mu. mol/L, 30. mu. mol/L, 40. mu. mol/L, 50. mu. mol/L, 60. mu. mol/L, 70. mu. mol/L, 80. mu. mol/L, 90. mu. mol/L, 100. mu. mol/L), which is the optimal concentration for determining the working of the fluorescent probe; the fluorescence intensity gradually increases with the concentration of the salt compound solution, but does not increase linearly, and the fluorescence quenching phenomenon exists.
Therefore, TPCANa aqueous solution with concentration of 0.5mmol/L is selected for determination: mixing 100 mu L of TPCANa aqueous solution (0.5mmol/L) with trivalent gold ions with different concentrations, metering the volume to 10mL, incubating for 1h at 60 ℃, performing fluorescence measurement, and gradually weakening the fluorescence intensity at 420nm along with the increase of the concentration of the trivalent gold ions; relative fluorescence intensity (F) with trivalent gold ion concentration as abscissa0–F)/F0Obtaining a working curve of the concentration of the trivalent gold ions as a vertical coordinate, wherein within the range of 40-175 mu mol/L, a linear regression equation is as follows: (F)0-F)/F00.00688C-0.28209, C is the concentration of trivalent gold ions in μmol/L.
b. And (3) environment screening: the aqueous solution of the salt compound is added with trivalent gold ions under different conditions for condition screening. The different conditions are as follows: different pH, interference of other metal cations. The specific operation is as follows: diluting 100 mu L of TPCANa (0.5mmol/L) to 10mL, adjusting the pH value to 2-13, and measuring the fluorescence emission intensity at 420 nm; fluorescence intensity at 420nm was measured by mixing and diluting 100. mu.L of TPCANa (0.5mmol/L) with different metal cations to 10 mL.
Example 1
Preparation of TPCANa
Dissolving 1.5g of TPCA into 20mL of NaOH aqueous solution (1mol/L), after complete dissolution, dropwise adding the solution into 200mL of anhydrous ethanol in ice bath, separating out white precipitate, wherein the white precipitate is TPCANa, cleaning the precipitate by using saturated sodium carbonate solution, removing residual TPCA, carrying out suction filtration on the obtained powder, and drying to obtain TPCANa.
The TPCANa obtained in the example is tested to obtain an excitation/emission spectrogram (figure 1) and a photoluminescence spectrogram (figure 2), and as can be seen from figures 1 and 2, the TPCANa prepared successfully by the method has fluorescence and can be used as a fluorescent probe.
TPCANa reacts with gold ion
mu.L of TPCANa (0.5mmol/L) aqueous solution is added into trivalent gold ion solution (0.25mmol/L) with different volumes, diluted to 10mL, and fluorescence measurement is carried out, wherein the fluorescence emission intensity at 420nm gradually decreases with the increase of the trivalent gold ion concentration (from 0. mu. mol/L to 200. mu. mol/L, specifically 0. mu. mol/L, 1. mu. mol/L, 2. mu. mol/L, 4. mu. mol/L, 6. mu. mol/L, 8. mu. mol/L, 10. mu. mol/L, 20. mu. mol/L, 40. mu. mol/L, 60. mu. mol/L, 80. mu. mol/L, 100. mu. mol/L, 125. mol/L, 150. mu. mol/L, 175. mu. mol/L and 200. mu. mol/L), and the fluorescence emission is shown in FIG. 3.
pH response Range of TPCANa
Diluting 100 mu L of TPCANa (0.5mmol/L) aqueous solution to 10mL, adjusting the pH value to 2-13, and measuring the fluorescence emission intensity at 420 nm; mu.L of TPCANa (0.5mmol/L) was diluted to 10mL and adjusted to pH 2 to 13, specifically, pH: 2. the fluorescence intensity at 420nm was measured at 3, 4, 5, 6, 7, 8, 9, 11, 12, 13, see FIG. 4.
Sensitive detection of TPCANa
100 μ L of TPCANa (0.5mmol/L) in water was mixed with different metal cations (Ag)+、Fe2+(500μmol/L)、Ca2+、Cu2+、Zn2+、Mg2+、Al3+、Na+、Ba2+、K+、Cd2+、In3+、Sn4+(500μM)、Ce3+(500μM)、Fe3+(500μmol/L)、Au3+(100 mu mol/L) and the concentration of the rest metal cations are all 1mmol/L), mixing and diluting to 10mL, and measuring the corresponding 420nm of different metal ionsThe fluorescence intensity histogram of (A) and (B) in FIG. 5 shows that other metal ions do not interfere with the determination of trivalent gold ions by TPCANa.
Obtaining a Linear Curve
Mixing 100 μ L of TPCANa (0.5mmol/L) water solution with different volumes of trivalent gold ions (0.25mM) and making the volume to 10mL to obtain 50 μ M TPCANa and a series of Au3+After incubation for 1h at 60 ℃ at a concentration (from 0 to 200. mu.M), performing fluorescence measurement, wherein the fluorescence intensity at 420nm gradually decreases with the increase of the concentration of the trivalent gold ions; relative fluorescence intensity (F) with trivalent gold ion concentration as abscissa0–F)/F0Is ordinate, F0Fluorescence intensity of 50 μ M TPCANa blank control group, and detection of Au with different concentrations for 50 μ M TPCANa aqueous solution3+Obtaining a working curve of the concentration of the trivalent gold ions according to the fluorescence intensity, wherein within the range of 40-175 mu mol/L, a linear regression equation is as follows: (F)0–F)/F0C is the concentration of trivalent gold ions in μmol/L, 0.00688C-0.28209, the linear curve is shown in fig. 6.
When the trivalent gold ion is detected to contain the trivalent gold ion, TPCANa aqueous solution (50 mu mol/L) is used for detecting the trivalent gold ion with different concentrations, and the detected fluorescence intensity (which can be within the linear range of detection) is substituted into a linear regression equation to obtain the concentration of the trivalent gold ion.
The salt synthesized by the invention has the advantages of good selectivity, wide linear range, high sensitivity, simple synthesis method, excellent water solubility and the like for identifying the trivalent gold ions.
Claims (3)
1. A method for detecting trivalent gold ions by using a water-soluble fluorescent compound is characterized in that TPCANa aqueous solution is adopted to detect trivalent gold ions with different concentrations to obtain corresponding fluorescence curves, and then the concentration of the trivalent gold ions is taken as a horizontal coordinate and the relative fluorescence intensity (F) is obtained0-F)/F0Obtaining a standard curve of the concentration of the TPCANa detected trivalent gold ions as a vertical coordinate; according to the standard curve, the linear regression equation is as follows within the range of 40-175 mu mol/L: (F)0-F)/F00.00688C-0.28209, whereinC is the concentration of trivalent gold ion, F0Fluorescence intensity of blank control group with 50 mu mol/L TPCANa aqueous solution, and detection of Au with different concentrations with F50 mu mol/L TPCANa aqueous solution3+The fluorescence intensity of (a);
when a sample containing trivalent gold ions is detected, the TPCANa aqueous solution detects the trivalent gold ions with different concentrations to obtain different fluorescence intensities, and the fluorescence intensities are substituted into a linear regression equation to obtain the concentration of the trivalent gold ions;
wherein TPCANa is prepared by the following method: adding TPCA into NaOH solution to obtain TPCANa aqueous solution, adding the aqueous solution into absolute ethyl alcohol, separating out precipitate, carrying out suction filtration, and drying to obtain TPCANa;
the concentration of the sodium hydroxide solution is 0.5 mol/L-1.0 mol/L;
the volume ratio of the aqueous solution to the absolute ethyl alcohol is 1: 10.
2. The method for detecting trivalent gold ions by using the water-soluble fluorescent compound as claimed in claim 1, wherein the molar ratio of TPCA to NaOH is 1: 1-5.
3. The method for detecting trivalent gold ions by using water-soluble fluorescent compound as claimed in claim 1, wherein the molar ratio of TPCA to NaOH is 1: 3.
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| Carbon dots with high fluorescent quantum yield: the fluorescence originates from organic fluorophores;Lei Shi et al;《Nanoscale》;20160708;第8卷(第30期);第14374-14378页 * |
| 功能化石墨烯量子点的分析应用研究;蔡菲;《中国优秀硕士学位论文全文数据库 工程科技I辑》;20151215;第2章2.2.2节小结部分 * |
| 金(III)离子荧光探针的研究进展;刘通秀等;《中国科学》;20170420;第47卷(第5期);第524-529页 * |
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