CN114920944B - Rare earth metal organic framework material fluorescent probe and detection method of bivalent mercury ions - Google Patents
Rare earth metal organic framework material fluorescent probe and detection method of bivalent mercury ions Download PDFInfo
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Abstract
The invention discloses a rare earth metal organic framework material fluorescent probe, which is prepared by the following method: dissolving 2-amino terephthalic acid in ethanol to obtain a solution A, dissolving terbium trichloride hexahydrate in water to obtain a solution B, mixing the solution A and the solution B, uniformly stirring, transferring to an ultrasonic cleaning instrument, carrying out reaction under ultrasonic, and cleaning the product after the reaction by using water and ethanol in sequence to obtain the rare earth metal organic framework material fluorescent probe. The invention also provides a detection method of the bivalent mercury ions. The rare earth metal organic framework material fluorescent probe provided by the invention can specifically detect the content of bivalent mercury ions in a water system; the minimum detection limit can reach 1 mu M; the preparation method is simple, low in cost and suitable for large-scale production; the method for detecting the bivalent mercury ions is simple to operate, low in detection limit, high in sensitivity and good in application prospect.
Description
Technical Field
The invention relates to the field, in particular to a rare earth metal organic framework material fluorescent probe and a detection method of bivalent mercury ions.
Background
Mercury is a highly toxic heavy metal pollutant, and is widely existed in the ecological system due to various human factors and factors existing in nature, so that the health of various organisms and human beings is seriously endangered. The most common form of mercury metal is divalent mercury ion, and can be enriched in the human body through the food chain, causing serious injury to nervous, digestive, endocrine, cardiovascular and other systems. In view of the high toxicity and low lethal concentration of mercury ions, a high-sensitivity and high-selectivity rapid detection method has important practical significance. However, in practice detection of mercury ions remains a significant challenge. This is because mercury ions at low concentrations are difficult to detect and the presence of other metal ions can interfere with mercury ion detection. Currently, common detection methods include fluorescence detection, electrochemical detection, colorimetric probes and the like. Wherein, the fluorescence method is most convenient for detection and has very high application prospect. Therefore, the development of more fluorescent probes with high sensitivity, high selectivity, easy operability, short response time and low cost, which are applied to the detection of bivalent mercury ions, has practical application value. The metal organic framework nano material is a new crystal porous material, is formed by self-assembly of an organic bridging ligand serving as a support column and metal serving as a node, has the characteristics of ultrahigh surface area, porosity, adjustability and easiness in modification, is very suitable for being used as a fluorescent probe, and is expected to be applied to mercury detection, but a reliable scheme based on the technology is not disclosed at present.
Disclosure of Invention
The invention aims to solve the technical problems of the prior art and provides a rare earth metal organic framework material fluorescent probe and a detection method of bivalent mercury ions. According to the fluorescent probe provided by the invention, the principle that the energy transfer of aniline to terbium is reduced after mercury ions are coordinated with amine groups so as to influence the fluorescence intensity of terbium-containing metal organic framework materials is utilized, so that the detection of the concentration of bivalent mercury ions can be realized.
In order to solve the technical problems, the invention adopts the following technical scheme: a fluorescent probe of a rare earth metal organic framework material is prepared by the following method:
dissolving 2-amino terephthalic acid in ethanol to obtain a solution A, dissolving terbium trichloride hexahydrate in water to obtain a solution B, mixing the solution A and the solution B, uniformly stirring, transferring to an ultrasonic cleaning instrument, carrying out reaction under ultrasonic, and cleaning the product after the reaction by using water and ethanol in sequence to obtain the rare earth metal organic framework material fluorescent probe.
Preferably, the rare earth metal organic framework material fluorescent probe is prepared by the following method:
dissolving 2-amino terephthalic acid in ethanol to obtain a solution A, dissolving terbium trichloride hexahydrate in water to obtain a solution B, mixing the solution A and the solution B, uniformly stirring for 1-4 hours, transferring to an ultrasonic cleaning instrument, reacting for 0.5-3 hours under ultrasonic, and cleaning the product sequentially by using water and ethanol to obtain the rare earth metal organic framework material fluorescent probe.
Preferably, the rare earth metal organic framework material fluorescent probe is prepared by the following method:
dissolving 0.5-2g of 2-amino terephthalic acid in 15-60mL of ethanol to obtain a solution A, dissolving 1-4g of terbium trichloride hexahydrate in 15-60mL of water to obtain a solution B, mixing the solution A and the solution B, uniformly stirring for 1-4 hours at normal temperature, transferring to an ultrasonic cleaner, reacting for 0.5-3 hours under ultrasonic, and cleaning the product with water and ethanol for several times sequentially to obtain the rare earth metal organic framework material fluorescent probe.
Preferably, the rare earth metal organic framework material fluorescent probe is prepared by the following method:
1g of 2-amino terephthalic acid is dissolved in 30mL of ethanol to obtain solution A, 2g of terbium trichloride hexahydrate is dissolved in 30mL of water to obtain solution B, then the solution A and the solution B are mixed, stirred uniformly for 2 hours at normal temperature and then transferred into an ultrasonic cleaner, the reaction is carried out for 1.5 hours under ultrasonic, the product is firstly cleaned with water for three times and then is cleaned with ethanol for three times, and the rare earth metal organic framework material fluorescent probe is obtained.
The invention also discloses a method for detecting the bivalent mercury ions, which adopts the fluorescent probe of the rare earth metal organic framework material to detect the bivalent mercury ions.
Preferably, the method for detecting the divalent mercury ions comprises the following steps:
s1, constructing a standard curve for representing the relation between the concentration of bivalent mercury ions and fluorescence intensity;
s2, dispersing the rare earth metal organic framework material fluorescent probe in water to prepare a detection solution;
s3, diluting a sample of the bivalent mercury ions to be detected with water to prepare a sample solution, mixing the detection solution obtained in the step S2 with the sample solution, uniformly stirring, standing, detecting the fluorescence intensity of the product at 515nm under the excitation light of 320nm, and finally calculating according to a standard curve to obtain the concentration of the bivalent mercury ions in the sample.
Preferably, the method for detecting the divalent mercury ions comprises the following steps:
s1, constructing a standard curve for representing the relation between the concentration of bivalent mercury ions and fluorescence intensity;
s2, dispersing the rare earth metal organic framework material fluorescent probe in water to prepare a detection solution with the concentration of 0.1-0.8 mg/mL;
s3, diluting a sample of the bivalent mercury ions to be detected with water to prepare a sample solution, then taking 0.5-2mL of the detection solution obtained in the step S2, mixing with 0.5-2mL of the sample solution, uniformly stirring, standing for 5-20 minutes, detecting the fluorescence intensity of a product at 515nm under the excitation light of 320nm, and finally calculating according to a standard curve to obtain the concentration of the bivalent mercury ions in the sample.
Preferably, the method for detecting the divalent mercury ions comprises the following steps:
s1, constructing a standard curve for representing the relation between the concentration of bivalent mercury ions and fluorescence intensity;
s2, dispersing the rare earth metal organic framework material fluorescent probe in water to prepare a detection solution with the concentration of 0.2 mg/mL;
s3, diluting a sample of the bivalent mercury ions to be detected with water to prepare a sample solution, mixing 1mL of the detection solution obtained in the step S2 with 1mL of the sample solution, uniformly stirring, standing for 10 minutes, detecting the fluorescence intensity of a product at 515nm under 320nm of excitation light, and finally calculating according to a standard curve to obtain the concentration of the bivalent mercury ions in the sample.
Preferably, the step S1 specifically includes: dispersing the rare earth metal organic framework material fluorescent probe in water to prepare a standard detection solution, and uniformly dividing the standard detection solution into a plurality of parts; then adding bivalent mercury ions with different concentrations into each standard detection solution, uniformly stirring, and respectively detecting the fluorescence intensity of the product at 515nm under 320nm of excitation light; and (3) taking the concentration of the bivalent mercury ions and the fluorescence intensity as the horizontal coordinate and the vertical coordinate respectively, and performing curve fitting to obtain a standard curve for representing the relationship between the concentration of the bivalent mercury ions and the fluorescence intensity.
Preferably, the step S1 specifically includes: dispersing the rare earth metal organic framework material fluorescent probe in water to prepare a standard detection solution with the concentration of 0.2mg/mL, equally dividing the standard detection solution into 7 parts with the volume of V, and respectively adding bivalent mercury ions with the concentration of 1, 5, 10, 20, 30, 40, 50 and mu M with the volume of V into the 1 st to 7 th standard detection solutions; stirring uniformly, standing for 10 minutes, and respectively detecting the fluorescence intensity of the product at 515nm under 320nm of excitation light; and (3) taking the concentration of the bivalent mercury ions and the fluorescence intensity as the horizontal coordinate and the vertical coordinate respectively, and performing curve fitting to obtain a standard curve for representing the relationship between the concentration of the bivalent mercury ions and the fluorescence intensity.
The beneficial effects of the invention are as follows:
the rare earth metal organic framework material fluorescent probe provided by the invention is regular particles, has uniform size, length of about 500nm and width of about 200nm, is easy to disperse in water, and can conveniently detect the content of bivalent mercury ions in a water system; after the bivalent mercury ions are added into the fluorescent probe, the fluorescent signal is reduced, the fluorescent signal is linearly related to the concentration of the bivalent mercury ions within the range of 0-50 mu M, and the minimum detection limit can reach 1 mu M; the fluorescent probe has ultrahigh specific selectivity to bivalent mercury ions, and the fluorescent signal is not obviously reduced when other metal ions are added;
the rare earth metal organic framework material fluorescent probe provided by the invention has the advantages of simple preparation method and low cost, and is suitable for large-scale production;
the method for detecting the bivalent mercury ions is simple to operate, low in detection limit, high in sensitivity and good in application prospect.
Drawings
FIG. 1 is a schematic diagram of the synthetic route of a rare earth metal organic framework material fluorescent probe of the present invention;
FIG. 2 is an SEM image of a fluorescent probe of rare earth metal-organic framework material prepared in example 1 of the present invention;
FIG. 3 is an excitation and emission spectrum of a rare earth metal organic framework material fluorescent probe prepared in example 1 of the present invention;
FIG. 4 is a graph showing the change of fluorescence intensity of the rare earth metal organic framework material fluorescent probe prepared in example 1 according to the present invention with the concentration of divalent mercury ions;
FIG. 5 is a standard curve obtained in example 1 of the present invention;
FIG. 6 is a fluorescence spectrum of a rare earth metal organic framework material fluorescent probe prepared in example 1 of the present invention when 200. Mu.M of different kinds of small organic molecules are added;
fig. 7 is a schematic diagram of a mechanism analysis of detecting bivalent mercury ions by using a fluorescent probe of a rare earth metal organic framework material prepared in example 1 of the present invention.
Detailed Description
The present invention is described in further detail below with reference to examples to enable those skilled in the art to practice the same by referring to the description.
It will be understood that terms, such as "having," "including," and "comprising," as used herein, do not preclude the presence or addition of one or more other elements or groups thereof.
Example 1
A fluorescent probe of a rare earth metal organic framework material is prepared by the following method:
1g of 2-amino terephthalic acid is dissolved in 30mL of ethanol to obtain solution A, 2g of terbium trichloride hexahydrate is dissolved in 30mL of water to obtain solution B, then the solution A and the solution B are mixed, stirred uniformly for 2 hours at normal temperature and then transferred into an ultrasonic cleaner, the reaction is carried out for 1.5 hours under ultrasonic, the product is firstly cleaned with water for three times and then is cleaned with ethanol for three times, and the rare earth metal organic framework material fluorescent probe is obtained.
Referring to fig. 1, a schematic diagram of a synthetic route of the rare earth metal organic framework material fluorescent probe is shown in fig. 2, which is an SEM electron microscope image, wherein the rare earth metal organic framework material fluorescent probe is regular particles, has uniform size, has a length of about 500nm and a width of about 200nm, and is easy to be dispersed in water.
Referring to fig. 3, the excitation and emission spectra of the rare earth metal organic framework material fluorescent probe can be seen to have an emission peak around 515 nm.
Referring to fig. 4, the fluorescence intensity of the rare earth metal organic framework material fluorescent probe is changed along with the concentration of the bivalent mercury ions, and fig. 5 is a standard curve obtained by fitting. In the embodiment, firstly preparing 0.2mg/mL terbium metal organic framework nano material aqueous suspension, adding bivalent mercury ions (0-50 mu M) with different concentrations into the aqueous suspension, and then detecting the fluorescence intensity of a product at 515nm under 320nm of excitation light, wherein the fluorescence emission intensity gradually decreases with the increase of the bivalent mercury ion concentration and the correlation is in a linear relation, so that the detection of the bivalent mercury ion concentration can be realized through the rare earth metal organic framework material fluorescent probe.
Referring to FIG. 6, the fluorescence spectrum of the rare earth metal organic framework material fluorescence probe when 200. Mu.M of different kinds of small organic molecules are added. In this example, the divalent mercury ion concentration was first configured as a 0.2mg/mL suspension, then different metal ions (sodium ion, ferric ion, lead ion, manganese ion, cobalt ion, cadmium ion and calcium ion) of the same solubility (200 μm) were added to the suspension, and the fluorescence intensities were detected separately, and the fluorescence intensities were significantly reduced only when the divalent mercury ion was added; therefore, the fluorescent probe can specifically detect the concentration of bivalent mercury ions in water.
Referring to fig. 7, a schematic diagram of a mechanism analysis of the rare earth metal organic framework material fluorescent probe for detecting bivalent mercury ions is shown, wherein 2-amino terephthalic acid in the fluorescent probe is used as a supporting ligand of the metal organic framework material, terbium ions are used as metal nodes, and the fluorescent probe has fluorescent performance in water. The bivalent mercury ions can be specifically combined with amino groups on the 2-amino terephthalic acid, so that fluorescence of the metal framework material is quenched, and the fluorescence intensity is reduced along with the increase of the addition amount of the bivalent mercury ions. The addition of other metal ions does not significantly reduce the fluorescence performance of the fluorescent probe, so that the fluorescent probe can specifically detect the bivalent mercury ion concentration in water.
Example 2
A method for detecting divalent mercury ions, the method comprising the steps of:
s1, constructing a standard curve for representing the relation between the concentration of bivalent mercury ions and fluorescence intensity;
dispersing the rare earth metal organic framework material fluorescent probe in water to prepare a standard detection solution with the concentration of 0.2mg/mL, equally dividing the standard detection solution into 7 parts with the volume of V, and respectively adding bivalent mercury ions with the concentration of 1, 5, 10, 20, 30, 40, 50 and mu M with the volume of V into the 1 st to 7 th standard detection solutions; stirring uniformly, standing for 10 minutes, and respectively detecting the fluorescence intensity of the product at 515nm under 320nm of excitation light; curve fitting is carried out by taking the concentration of the bivalent mercury ions and the fluorescence intensity as the horizontal coordinate and the vertical coordinate respectively, so that a standard curve representing the relationship between the concentration of the bivalent mercury ions and the fluorescence intensity is obtained, and the results are shown in figures 4 and 5.
S2, dispersing the rare earth metal organic framework material fluorescent probe in water to prepare a detection solution with the concentration of 0.2 mg/mL;
s3, diluting a sample of the bivalent mercury ions to be detected with water to prepare a sample solution, mixing 1mL of the detection solution obtained in the step S2 with 1mL of the sample solution, uniformly stirring, standing for 10 minutes, detecting the fluorescence intensity of a product at 515nm under 320nm of excitation light, and finally calculating according to a standard curve to obtain the concentration of the bivalent mercury ions in the sample.
Although embodiments of the present invention have been disclosed above, it is not limited to the use of the description and embodiments, it is well suited to various fields of use for the invention, and further modifications may be readily apparent to those skilled in the art, and accordingly, the invention is not limited to the particular details without departing from the general concepts defined in the claims and the equivalents thereof.
Claims (9)
1. The method is characterized in that a rare earth metal organic framework material fluorescent probe is adopted to detect the bivalent mercury ions;
the rare earth metal organic framework material fluorescent probe is prepared by the following method:
dissolving 2-amino terephthalic acid in ethanol to obtain a solution A, dissolving terbium trichloride hexahydrate in water to obtain a solution B, mixing the solution A and the solution B, uniformly stirring, transferring to an ultrasonic cleaning instrument, carrying out reaction under ultrasonic, and cleaning the product after the reaction by using water and ethanol in sequence to obtain the rare earth metal organic framework material fluorescent probe.
2. The method for detecting divalent mercury ions according to claim 1, wherein the rare earth metal organic framework material fluorescent probe is prepared by the following method:
dissolving 2-amino terephthalic acid in ethanol to obtain a solution A, dissolving terbium trichloride hexahydrate in water to obtain a solution B, mixing the solution A and the solution B, uniformly stirring for 1-4 hours, transferring to an ultrasonic cleaning instrument, reacting for 0.5-3 hours under ultrasonic, and cleaning the product sequentially by using water and ethanol to obtain the rare earth metal organic framework material fluorescent probe.
3. The method for detecting divalent mercury ions according to claim 2, wherein the rare earth metal organic framework material fluorescent probe is prepared by the following method:
dissolving 0.5-2g of 2-amino terephthalic acid in 15-60mL of ethanol to obtain a solution A, dissolving 1-4g of terbium trichloride hexahydrate in 15-60mL of water to obtain a solution B, mixing the solution A and the solution B, uniformly stirring for 1-4 hours at normal temperature, transferring to an ultrasonic cleaner, reacting for 0.5-3 hours under ultrasonic, and cleaning the product with water and ethanol for several times sequentially to obtain the rare earth metal organic framework material fluorescent probe.
4. The method for detecting divalent mercury ions according to claim 3, wherein the rare earth metal organic framework material fluorescent probe is prepared by the following method:
1g of 2-amino terephthalic acid is dissolved in 30mL of ethanol to obtain solution A, 2g of terbium trichloride hexahydrate is dissolved in 30mL of water to obtain solution B, then the solution A and the solution B are mixed, stirred uniformly for 2 hours at normal temperature and then transferred into an ultrasonic cleaner, the reaction is carried out for 1.5 hours under ultrasonic, the product is firstly cleaned with water for three times and then is cleaned with ethanol for three times, and the rare earth metal organic framework material fluorescent probe is obtained.
5. The method for detecting divalent mercury ions according to claim 1, comprising the steps of:
s1, constructing a standard curve for representing the relation between the concentration of bivalent mercury ions and fluorescence intensity;
s2, dispersing the rare earth metal organic framework material fluorescent probe in water to prepare a detection solution;
s3, diluting a sample of the bivalent mercury ions to be detected with water to prepare a sample solution, mixing the detection solution obtained in the step S2 with the sample solution, uniformly stirring, standing, detecting the fluorescence intensity of the product at 515nm under the excitation light of 320nm, and finally calculating according to a standard curve to obtain the concentration of the bivalent mercury ions in the sample.
6. The method for detecting divalent mercury ions according to claim 5, comprising the steps of:
s1, constructing a standard curve for representing the relation between the concentration of bivalent mercury ions and fluorescence intensity;
s2, dispersing the rare earth metal organic framework material fluorescent probe in water to prepare a detection solution with the concentration of 0.1-0.8 mg/mL;
s3, diluting a sample of the bivalent mercury ions to be detected with water to prepare a sample solution, then taking 0.5-2mL of the detection solution obtained in the step S2, mixing with 0.5-2mL of the sample solution, uniformly stirring, standing for 5-20 minutes, detecting the fluorescence intensity of the product at 515nm under the excitation light of 320nm, and finally calculating according to a standard curve to obtain the concentration of the bivalent mercury ions in the sample.
7. The method for detecting divalent mercury ions according to claim 6, comprising the steps of:
s1, constructing a standard curve for representing the relation between the concentration of bivalent mercury ions and fluorescence intensity;
s2, dispersing the rare earth metal organic framework material fluorescent probe in water to prepare a detection solution with the concentration of 0.2 mg/mL;
s3, diluting a sample of the bivalent mercury ions to be detected with water to prepare a sample solution, mixing 1mL of the detection solution obtained in the step S2 with 1mL of the sample solution, uniformly stirring, standing for 10 minutes, detecting the fluorescence intensity of a product at 515nm under the excitation light of 320nm, and finally calculating according to a standard curve to obtain the concentration of the bivalent mercury ions in the sample.
8. The method for detecting divalent mercury ions according to claim 7, wherein said step S1 is specifically: dispersing the rare earth metal organic framework material fluorescent probe in water to prepare a standard detection solution, and uniformly dividing the standard detection solution into a plurality of parts; then adding bivalent mercury ions with different concentrations into each standard detection solution, uniformly stirring, and respectively detecting the fluorescence intensity of the product at 515nm under the excitation light of 320 nm; and (3) taking the concentration of the bivalent mercury ions and the fluorescence intensity as the horizontal coordinate and the vertical coordinate respectively, and performing curve fitting to obtain a standard curve for representing the relationship between the concentration of the bivalent mercury ions and the fluorescence intensity.
9. The method for detecting divalent mercury ions according to claim 8, wherein step S1 specifically comprises: dispersing the rare earth metal organic framework material fluorescent probe in water to prepare a standard detection solution with the concentration of 0.2mg/mL, equally dividing the standard detection solution into 7 parts with the volume of V, and respectively adding bivalent mercury ions with the concentration of 1, 5, 10, 20, 30, 40 and 50 mu M with the volume of V into the 1 st to 7 th standard detection solutions; stirring uniformly, standing for 10 minutes, and respectively detecting the fluorescence intensity of the product at 515nm under the excitation light of 320 nm; and (3) taking the concentration of the bivalent mercury ions and the fluorescence intensity as the horizontal coordinate and the vertical coordinate respectively, and performing curve fitting to obtain a standard curve for representing the relationship between the concentration of the bivalent mercury ions and the fluorescence intensity.
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| CN105753891A (en) * | 2016-03-23 | 2016-07-13 | 浙江大学 | Rare earth organic framework material for fluorescence detection of trace water and preparation method of rare earth organic framework material |
| CN106188110A (en) * | 2016-07-13 | 2016-12-07 | 北京化工大学 | A kind of metallic organic framework functional fluorescence material and preparation method and applications |
| CN108610488A (en) * | 2018-05-29 | 2018-10-02 | 南昌大学 | The preparation method of Schiff base rare-earth coordination polymer fluorescence probe and its mercury ion detecting application |
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| US11124529B2 (en) * | 2019-07-03 | 2021-09-21 | King Fahd University Of Petroleum And Minerals | Europium based metal organic framework for palladium sensing |
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| CN105753891A (en) * | 2016-03-23 | 2016-07-13 | 浙江大学 | Rare earth organic framework material for fluorescence detection of trace water and preparation method of rare earth organic framework material |
| CN106188110A (en) * | 2016-07-13 | 2016-12-07 | 北京化工大学 | A kind of metallic organic framework functional fluorescence material and preparation method and applications |
| CN108610488A (en) * | 2018-05-29 | 2018-10-02 | 南昌大学 | The preparation method of Schiff base rare-earth coordination polymer fluorescence probe and its mercury ion detecting application |
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