CN107589098B - Method for fluorescence detection of trace uranyl ions - Google Patents
Method for fluorescence detection of trace uranyl ions Download PDFInfo
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- CN107589098B CN107589098B CN201710764481.7A CN201710764481A CN107589098B CN 107589098 B CN107589098 B CN 107589098B CN 201710764481 A CN201710764481 A CN 201710764481A CN 107589098 B CN107589098 B CN 107589098B
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Abstract
The invention relates to a method for fluorescence detection of trace uranyl ions, which comprises the following steps: (a) adding esculin and a mesoporous molecular sieve into a water solution containing uranyl ions, and performing fluorescence detection to obtain the fluorescence intensity of the water solution; (b) preparing a solution without uranyl ions, and measuring the fluorescence intensity of the solution to be F0; (c) preparing solutions containing uranyl ions with different concentrations, and measuring the fluorescence intensity to be Fn; (d) F0/Fn-1 is used as an ordinate, and the concentration of uranyl ions is used as an abscissa to draw a curve; (e) diluting the aqueous solution in the step (a) in proportion until the measured fluorescence intensity falls in the range of 0.001-0.05 [ mu ] mol/L according to the concentration corresponding to the curve in the step (d); multiplying the corresponding concentration by the dilution factor. Therefore, the concentration of the uranyl ions in the aqueous solution can be accurately measured, and the lower detection limit can be as low as 6 nM.
Description
Technical Field
the invention relates to the field of radioactive substance detection, in particular to a method for fluorescence detection of trace uranyl ions.
background
With the gradual depletion of traditional non-renewable energy sources such as coal and petroleum, clean energy sources represented by nuclear energy are more and more favored by people and are more and more widely used in the global scope. One of the main raw materials of nuclear energy is uranium, so that the probability of human exposure to the threat of uranium is increasing. The threat of uranium comes from its own radioactive toxicity and chemical toxicity, which can cause serious injury to human organs and bodies upon contact or entry into the human body. High doses of uranium also have a significant environmental hazard. The most stable form of uranium in aqueous solution under aerobic or hypoxymic conditions is the uranyl ion UO22+, which has some solubility in water and is therefore free to migrate in the environment. Therefore, the method has certain strategic significance on the detection and monitoring of the uranyl and is very necessary.
prior to this time, there have been many reports of monitoring for uranyl ions. Some of these methods are based on complex or expensive instruments. These methods are not deemed acceptable by the general public because they are generally relatively expensive and require relatively stringent sample preparation and instrument operation, which makes field monitoring difficult to achieve. On the other hand, the probe itself has been developed, and some novel nanomaterials and media have been reported. Recently, chen et al reported mesoporous silicon/carbon dot composite CDs/SBA-NH2 materials that are capable of not only adsorbing uranyl ions, but also monitoring the adsorption process (z.wang, c.xu, y.lu, f.wu, g.ye, g.wei, t.sun and j.chen, ACS appl.mater.interfaces,2017,9, 7392.). The field team at Illinois university reported a DNA enzyme with specific coordination to uranyl ions that had nearly perfect detection of uranyl ions with a detection limit of 45pM in 2007, after which their team also reported the first intracellular detection of uranyl ions (J.Liu, A.K.Brown, X.Meng, D.M.Cropek, J.D.Istok, D.B.Watson and Y.Lu, Proc.Natl.Acad.Sci.U.S.A.,2007,104,2056; P.Wu, K.Hwang, T.Lan and Y.Lu, J.Am.Chem.Soc.,2013,135,5254.). The DNA enzyme has a good application prospect in the field of metal ion detection, so that the DNA enzyme is widely concerned, and is also used for various technologies to detect trace uranyl ions. However, the screening process of such metal ion-specific dnases is complicated and time-consuming, so that the method is not convenient and economical.
among the different technical methods, the fluorescence technology is obviously a powerful tool with high cost performance and simple and convenient operation. However, there are few reports on the detection of uranyl ions by fluorescence, and there are fewer reports on the use of small fluorescent molecules, which is quite different from the case of other metal ions. The reason for this may be that it is difficult to achieve a satisfactory detection limit using fluorescent small molecule detection. The detection limit is one of the main obstacles for detecting trace uranyl ions by using a fluorescence technology, so how to improve the sensitivity of the probe is a very important link. There are few reports on improving the sensitivity of probes.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a method for fluorescence detection of trace uranyl ions.
in order to achieve the purpose, the invention adopts the technical scheme that: a method for fluorescence detection of trace uranyl ions comprises the following steps:
(a) adding esculin and a mesoporous molecular sieve into a water solution containing uranyl ions, and performing fluorescence detection to obtain the fluorescence intensity of the water solution; the ratio of esculin to the mesoporous molecular sieve is 5-15 mu mol/L: 0.05-0.2 mg/mL;
(b) Preparing a solution without uranyl ions, and measuring the fluorescence intensity of the solution to be F0; the solution which does not contain uranyl ions contains esculin and a mesoporous molecular sieve with the same concentration as that in the step (a);
(c) preparing solutions containing uranyl ions with different concentrations, and measuring the fluorescence intensity to be Fn; said solutions containing different concentrations of uranyl ions contain the same concentrations of esculin and mesoporous molecular sieve as in step (a);
(d) F0/Fn-1 is used as an ordinate, and the concentration of uranyl ions is used as an abscissa to draw a curve;
(e) Diluting the aqueous solution in the step (a) in proportion until the measured fluorescence intensity falls in the range of 0.001-0.05 [ mu ] mol/L according to the concentration corresponding to the curve in the step (d); multiplying the corresponding concentration by the dilution factor.
Optimally, the ratio of the esculin to the mesoporous molecular sieve is 10 mu mol/L: 0.1 mg/mL.
optimally, the mesoporous molecular sieve is SBA-15, SBA-1 or MCM-48.
Preferably, in the step (b) and the step (c), the solution not containing uranyl ions and the solution containing different concentrations of uranyl ions are prepared by mixing methanol and water in a volume ratio of 1: 1.
Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages: the method for the fluorescence detection of trace uranyl ions comprises the steps of measuring the fluorescence intensity of solutions with different concentrations of uranyl ions and solutions without uranyl ions, and drawing a standard curve; if necessary, the aqueous solution to be detected can be diluted until the corresponding concentration falls within the range of 0.001-0.05 mu mol/L, and the concentration is multiplied by the dilution multiple, so that the concentration of the uranyl ions in the aqueous solution can be accurately measured, and the lower detection limit can be as low as 6 nM.
Drawings
FIG. 1 is a standard curve drawn in the fluorescence detection method for trace uranyl ions according to the present invention;
FIG. 2 is a low concentration standard curve drawn in the fluorescence detection method for trace uranyl ions according to the present invention;
FIG. 3 is a schematic diagram of a fluorescence detection method for trace uranyl ions according to the present invention.
Detailed Description
The present invention will be further illustrated with reference to the following examples.
the invention discloses a method for fluorescence detection of trace uranyl ions, which comprises the following steps:
(a) adding esculin (esculin) and mesoporous molecular sieve (SBA-15 is usually selected, and other types of products such as SBA-1 or MCM-48 can also be used) into the aqueous solution containing uranyl ions, and carrying out fluorescence detection to obtain the fluorescence intensity of the aqueous solution at the wavelength of 455 nm; the ratio of esculin to the mesoporous molecular sieve is 5-15 mu mol/L: 0.05-0.2 mg/mL; when the ratio of esculin to mesoporous molecular sieve is 10 mu mol/L and 0.1mg/mL respectively, the fluorescence detection effect is best, and the lower limit of detection is as low as 6nM (namely 6 nmol/L; the same below);
(b) Preparing a solution (blank sample) without uranyl ions, and measuring the fluorescence intensity of the solution to be F0; the solution without uranyl ions contains esculin and mesoporous molecular sieve with the same concentration as that in the step (a), and the specific ratio of esculin to mesoporous molecular sieve is as follows: 5-15 mu mol/L: 0.05-0.2 mg/mL;
(c) Preparing solutions containing different concentrations of uranyl ions (specifically 0.001, 0.002, 0.005, 0.01, 0.02, 0.03, 0.04, 0.05, 0.1, 0.2, 0.5, 1, 2, 3, 4, 5, 6, 7, 8, 9 and 10 μ M), and measuring the fluorescence intensity to be Fn (specifically marked as F1, F2, F3, F4, F5, F6, F7, F8, F9, F10, F11, F12, F13, F14, F15, F16, F17, F18, F19, F20 and F21 respectively); the solutions containing uranyl ions with different concentrations contain esculin and mesoporous molecular sieve with the same concentration as in the step (a); the solvent in step (b) and step (c) is usually a mixture of methanol and water in a volume ratio of 1: 1;
(d) Drawing a curve by taking F0/Fn-1 as an ordinate and taking the concentration of the uranyl ions as an abscissa (namely drawing the 22 data points into a standard curve as shown in a figure 1); it can be found that the standard difference is substantially linear when the concentration of uranyl ions is within 0.05 μmol/L (i.e., 0.001-0.05 μmol/L); the curve at this time (as shown in fig. 2) can be expressed as F0/Fn-1 ═ KSV [ Q ], where KSV is the Stern-coefficient (KSV 8.69 × 106mol-1 · L, R2 ═ 0.994), and Q is the concentration of uranyl ions;
(e) Substituting the fluorescence intensity measured in the step (a) into the curve in the step (d) to preliminarily judge the concentration of the aqueous solution in the step (a); if the concentration of the aqueous solution is more than 0.05 mu mol/L, diluting the aqueous solution in the step (a) in proportion until the measured fluorescence intensity falls in the range of 0.001-0.05 mu mol/L according to the concentration corresponding to the curve in the step (d); and then multiplying the corresponding concentration by the dilution factor. As shown in FIG. 3, this is because SBA-15 has a certain adsorption effect on esculin, forming a local high concentration region around SBA-15; however, when the uranyl ion is added, the fluorescence intensity is reduced to a higher degree than that in the blank test, so that the corresponding F0/F-1 value is higher, and the uranyl ion and other ions can be easily distinguished; therefore, the system has very good selectivity to uranyl ions when mesoporous molecular sieves such as SBA-15 exist. The detection performance (from the aspects of sensitivity and selectivity) of the fluorescent micromolecules on the uranyl ions is greatly improved in the presence of SBA-15; when SBA-15 exists, part of the esculin and the uranyl ions are adsorbed to the surface of the SBA-15, so that the concentration of the uranyl ions around the SBA-15 is improved microscopically; so that its detection effect becomes good. More importantly, the uranyl ions and the esculin possibly have certain complexation, and the existence of the esculin has certain auxiliary effect on the adsorption of the uranyl ions.
Two samples as shown in Table 1 were selected for testing, and the results are shown in Table 1, and it can be seen that the error rate measured by the method is very small, less than 5%.
TABLE 1 test data sheet of actual samples
The above embodiments are merely illustrative of the technical concept and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the content of the present invention and implement the invention, and not to limit the scope of the invention, and all equivalent changes or modifications made according to the spirit of the present invention should be covered by the scope of the present invention.
Claims (4)
1. a method for fluorescence detection of trace uranyl ions is characterized by comprising the following steps:
(a) Adding esculin and a mesoporous molecular sieve into a water solution containing uranyl ions, and performing fluorescence detection to obtain the fluorescence intensity of the water solution; the ratio of esculin to the mesoporous molecular sieve is 5-15 mu mol/L: 0.05-0.2 mg/mL;
(b) Preparing a solution without uranyl ions, and measuring the fluorescence intensity of the solution to be F0; the solution which does not contain uranyl ions contains esculin and a mesoporous molecular sieve with the same concentration as that in the step (a);
(c) Preparing solutions containing uranyl ions with different concentrations, and measuring the fluorescence intensity to be Fn; said solutions containing different concentrations of uranyl ions contain the same concentrations of esculin and mesoporous molecular sieve as in step (a);
(d) F0/Fn-1 is used as an ordinate, and the concentration of uranyl ions is used as an abscissa to draw a curve;
(e) Diluting the aqueous solution in the step (a) in proportion until the measured fluorescence intensity falls in the range of 0.001-0.05 [ mu ] mol/L according to the concentration corresponding to the curve in the step (d); multiplying the corresponding concentration by the dilution factor.
2. The method for fluorescence detection of trace uranyl ions according to claim 1, wherein: the ratio of the esculin to the mesoporous molecular sieve is 10 mu mol/L: 0.1 mg/mL.
3. The method for fluorescence detection of trace uranyl ions according to claim 1, wherein: the mesoporous molecular sieve is SBA-15, SBA-1 or MCM-48.
4. the method for fluorescence detection of trace uranyl ions according to claim 1, wherein: in the step (b) and the step (c), the solution not containing the uranyl ions and the solution containing the uranyl ions with different concentrations are prepared by mixing methanol and water in a volume ratio of 1: 1.
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| KR102055660B1 (en) * | 2018-03-07 | 2019-12-13 | 경상대학교산학협력단 | Naphthamido-phenylazanediyl derivatives, compositions for detecting uranyl ion comprising the same and method of uranyl ion detection using the same |
| CN108680541B (en) * | 2018-03-13 | 2021-06-04 | 东华理工大学 | Method for determining trace uranium (VI) by using fluorescent molybdenum oxide quantum dots |
| CN108776113A (en) * | 2018-06-06 | 2018-11-09 | 南华大学 | A kind of application of double-core Complexes of Uranyl in ATP analyses |
| CN110596082B (en) * | 2019-10-17 | 2020-07-24 | 苏州大学 | Probe for detecting trace uranyl ions and portable EC L detector based on probe |
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| CN101921825A (en) * | 2009-09-22 | 2010-12-22 | 湖南科技大学 | Method for detecting uranium pollution by taking arabidopsis oligonucleotide fragment as probe |
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