CN111474167B - Cu-MOF-luminol-H 2 O 2 Detection of Pb by chemiluminescence system 2+ Method (2) - Google Patents
Cu-MOF-luminol-H 2 O 2 Detection of Pb by chemiluminescence system 2+ Method (2) Download PDFInfo
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Abstract
Cu-MOF-luminol-H 2 O 2 Detection of Pb by chemiluminescence system 2+ The method belongs to the field of chemical detection, can solve the problems that the existing detection method has low sensitivity, is not suitable for detecting trace lead ions or even lead ions with lower concentration and has high requirement on detection equipment, and uses divalent metal ions Cu (II) and organic ligands 2, 5-dihydroxyterephthalic acid (H) 2 DOBDC) is prepared by a hydrothermal method, and is introduced into luminol-H 2 O 2 A chemical luminescence system consisting of Cu-DOBDC-luminol-H 2 O 2 A chemiluminescent system. When it is Pb 2+ When present, pb 2+ Has stronger coupling ability with Cu-DOBDC, releases the Cu of the active site in the Cu-DOBDC and enhances luminol-H 2 O 2 Chemiluminescence, signal enhancement and Pb of the system 2+ The concentration is directly proportional. The method has the advantages of simple operation, high sensitivity, low detection limit and strong selectivity, and is suitable for rapid field detection.
Description
Technical Field
The invention belongs to the technical field of chemical detection, and particularly relates to Cu-MOF-luminol-H 2 O 2 Detection of Pb by chemiluminescence system 2+ The method of (1).
Background
Lead is a heavy metal element seriously harming human health, can affect various organs such as nerves, hematopoiesis, digestion, urinary system, cardiovascular system, reproduction, bones and the like, and more seriously affects the growth and intelligence development of infants, damages brain functions such as cognitive function, nerve behavior, learning and memory and the like, and causes dementia in severe cases. Therefore, the method has important practical significance for the research of the lead determination method.
The methods for detecting lead ions reported at present are as follows: ultraviolet-visible spectrophotometry, electrochemical analysis, atomic emission spectroscopy, and the like. However, the ultraviolet-visible spectrophotometry and the electrochemical analysis have low sensitivity, are not suitable for detecting trace lead ions or even lead ions with lower concentration, and the atomic emission spectrometry has expensive equipment and higher measurement cost, so that the selection of a more convenient and sensitive measurement mode is particularly important. The chemiluminescence method has the advantages of simple operation, low background, high sensitivity, no need of large-scale instruments and capability of realizing rapid and sensitive detection of lead ions.
Metal organic framework Materials (MOFs) are a composite material formed by the linkage of metal ions and organic ligands through chemical bonds. In recent years, as a new material, MOFs have attracted great attention in designing new materials and detecting due to their characteristics of large specific surface area, porosity, easy modification, mild synthesis conditions, high active sites, high density of contained metal ions, and the like. Recently there has been a move to Pb 2+ The method is suitable for detecting trace lead ions or even lead ions with lower concentration.
Disclosure of Invention
Aiming at the problems that the existing detection method has low sensitivity, is not suitable for detecting trace lead ions or even lead ions with lower concentration and has high requirement on detection equipmentProblem to provide a Cu-MOF-luminol-H 2 O 2 Detection of Pb by chemiluminescence system 2+ The method of (1). The object of the present invention is Pb 2+ Enhanced Cu-MOF-luminol-H 2 O 2 Chemiluminescence of the system, and degree of signal enhancement with Pb 2+ The concentration is in direct proportion, thereby establishing Pb 2+ The method of chemiluminescent analysis of (1).
The invention adopts the following technical scheme:
Cu-MOF-luminol-H 2 O 2 Detection of Pb by chemiluminescence system 2+ The method comprises the following steps:
the first step, preparation of Cu-DOBDC: dissolving copper acetate and 2, 5-dihydroxyterephthalic acid in a mixed solution composed of water, N-dimethylformamide and ethanol according to a certain proportion, and stirring for 1 to 20 min; transferring the mixture into a stainless steel hydrothermal reaction kettle with 200 mL of polytetrafluoroethylene lining for reaction, and washing the reaction product with ultrapure water and absolute ethyl alcohol respectively after the reaction is finished; drying the mixture in a vacuum drying box at the temperature of 30 to 100 ℃ for later use;
second, cu-MOF-luminol-H 2 O 2 Detection of Pb by chemiluminescence system 2+ : diluting step by step to obtain 1.0 × 10 -4 ~1.0×10 -2 mol/L luminol reagent and 1.0X 10 -4 ~1.0×10 -2 mol/L H 2 O 2 A reagent; dissolving Cu-DOBDC in water to obtain a Cu-DOBDC solution, and taking 0.01 to 0.5 mL of the Cu-DOBDC solution and 0.01 to 0.5 mL of Pb to be detected 2+ Uniformly mixing the solution, and standing for 10 to 60 min; measuring 1-20 mu L of Cu-MOF/Pb 2+ Mixing the solutions to be tested, and adding 1 to 20 mu L of H 2 O 2 And (3) dripping 10-100 mu L of luminol solution into the reagent by adopting a flow injection method, detecting chemiluminescence, detecting a luminescence signal by using a photomultiplier, and outputting light signal intensity under analysis software of a computer.
Preferably, the molar ratio of copper acetate to 2, 5-dihydroxyterephthalic acid in the first step is 1:4 to 4:1.
preferably, the volume ratio of the water, the N, N-dimethylformamide and the ethanol in the first step is 1:1:1, the volume of the mixed solution is 15 to 150 mL.
The preferable method is that the reaction temperature in the first step is 50 to 200 ℃, and the reaction time is 12 to 72h.
Preferably, in the second step, the luminol is 3-aminophthalic anhydride and the stock solution concentration is 1.0X 10 -2 mol/L; the preparation method comprises the following steps of weighing 0.1772-1.7716 g of luminol, dissolving the luminol with 0.10 mol/L of NaOH, transferring the luminol into a 100-1000 mL brown volumetric flask, fixing the volume with ultrapure water, keeping the volumetric flask in the dark for more than one week, and gradually diluting the volumetric flask when in use.
The preferable method is that the concentration of the Cu-DOBDC solution in the second step is 5 to 50 mg/mL and the concentration of Pb to be measured is different from that of Pb to be measured 2+ The solution mixing volume ratio is 50:1 to 1:50.
preferably, the Cu-MOF/Pb in the second step is 2+ Mixing the solution to be tested, luminol and H 2 O 2 The mixing volume ratio at the time of the test was 1:1:5 to 1:1:10.
the invention has the following beneficial effects:
1. the invention relates to a method for preparing divalent metal ion Cu (II) and organic ligand 2, 5-dihydroxyterephthalic acid (H) 2 DOBDC) is reacted by a hydrothermal method to obtain the metal organic framework material Cu-DOBDC. The introduction of Cu-MOF into luminol-H 2 O 2 In a chemiluminescence system, cu-MOF p-luminol-H 2 O 2 The system has a certain catalytic effect.
2. When it is Pb 2+ When present, pb 2+ Has stronger coupling capacity with Cu-DOBDC, can release the active site Cu in the Cu-DOBDC and enhance luminol-H 2 O 2 Chemiluminescence of the system, and degree of signal enhancement with Pb 2+ The concentration is in direct proportion, thereby establishing Pb 2+ The method of chemiluminescent analysis of (1).
3. The linear equation of the method is Y = 50.03C +191.28 (R) 2 = 0.9974), wherein Y is the chemiluminescence intensity, and C is Pb 2+ And (4) concentration. The linear range of the method is 0.5-50 nM, and the detection limit is 0.3 nM. The method has the advantages of simple operation, high sensitivity, low detection limit and strong selectivity, and is suitable for rapidly detecting Pb on site 2+ 。
Drawings
FIG. 1 shows Cu-DOBDC-luminol-H 2 O 2 Chemiluminescence of the system.
Fig. 2 is a schematic diagram of the principle of the present invention.
FIG. 3 is a Cu-DOBDC-luminol-H 2 O 2 System for Pb 2+ Chemiluminescence analysis characteristic curve at the time of detection.
FIG. 4 is Cu-DOBDC-luminol-H 2 O 2 System for Pb 2+ Chemiluminescence analysis standard curve during detection.
FIG. 5 is a graph of Cu-DOBDC-luminol-H for different metal ion pairs 2 O 2 Interference of the chemiluminescent system.
Detailed Description
In the following examples, the preparation of the Cu-MOF used was as follows: 0.6 mM (0.1198 g) copper acetate was weighed out and dissolved in 5mL H 2 In O, until it is completely dissolved; weighing 0.3 mM (0.0594 g) 2, 5-dihydroxy terephthalic acid, dissolving in 5mL DMF, adding the above copper acetate solution and 5mL ethanol, and stirring for 10 min; transferring the mixture into a stainless steel hydrothermal reaction kettle with 200 mL of polytetrafluoroethylene lining, and reacting for 24 hours at 120 ℃; washing with ultrapure water and anhydrous ethanol respectively for 3 times; and drying the mixture in a vacuum drying oven at 50 ℃ for later use.
In the following examples, the luminol stock solution was prepared by the following method: weighing 0.1770g of luminol, dissolving with 0.10 mol/L NaOH, transferring into 100 ml brown volumetric flask, and diluting with ultrapure water to constant volume to obtain stock solution with concentration of 1.0 × 10 -2 And (5) mol/L, and storing in dark.
Example 1
Diluting to obtain 1.0 × 10 -3 mol/L luminol reagent, and 30% H 2 O 2 Diluting the reagent step by step to obtain 1.0 × 10 -3 mol/L H 2 O 2 The solution is prepared as it is used. Dissolving 0.01 g of Cu-DOBDC in 1 mL of water to obtain a 10 mg/mL Cu-DOBDC solution, and taking 0.5 mL of Cu-DOBDC and 0.5 mL of Pb to be detected with different concentrations 2+ The solution was mixed well and left for 30 min. Measuring 10 mu L of Cu-MOF/Pb 2+ Mixing the solution to be tested in a glass beaker, adding 10. Mu.L of H 2 O 2 A reagent placed inAnd (3) dripping 50 mu L of luminol solution into the chemiluminescence cassette by adopting a flow injection method to detect chemiluminescence. The luminous signal is detected by a photomultiplier tube, and the intensity of the luminous signal is output under the analysis software of a computer.
Example 2
Diluting to obtain 1.0 × 10 -3 mol/L luminol reagent, and mixing 30% H 2 O 2 Diluting the reagent step by step to obtain 1.0 × 10 -3 mol/L H 2 O 2 The solution is prepared as it is used. Dissolving 0.01 g of Cu-DOBDC in 1 mL of water to obtain a 10 mg/mL Cu-DOBDC solution, and taking 0.5 mL of Cu-DOBDC and 0.5 mL of Pb to be detected with different concentrations 2+ The solution was mixed well and left for 30 min. Measuring 5 mu L of Cu-MOF/Pb 2+ Mixing the solution to be tested in 96 micro-porous plate, adding 5 μ L H 2 O 2 And reagent, which is placed in a chemiluminescence cassette, and 25 mu L of luminol solution is dripped by adopting a flow injection method for chemiluminescence detection. The luminous signal is detected by a photomultiplier tube, and the intensity of the luminous signal is output under the analysis software of a computer.
Example 3
Dilution preparation to give 1.0X 10 -3 mol/L luminol reagent, and mixing 30% H 2 O 2 Diluting the reagent step by step to obtain 1.0 × 10 -3 mol/L H 2 O 2 The solution is prepared as it is used. Dissolving 0.01 g of Cu-DOBDC in 1 mL of water to obtain a 10 mg/mL Cu-DOBDC solution, and taking 0.1 mL of Cu-DOBDC and 0.1 mL of Pb to be detected with different concentrations 2+ The solution was mixed well and left for 30 min. 2.5 mu.L of Cu-MOF/Pb were measured out 2+ Mixing the solution to be tested on Whatman No. 1 filter paper, and adding 2.5. Mu.L of H 2 O 2 And the reagent is placed in a chemiluminescence cassette, and 20 mu L of luminol solution is dripped by adopting a flow injection method for chemiluminescence detection. The luminescence signal is detected by the photomultiplier, and the intensity of the luminescence signal is output under the analysis software of a computer, and the results are shown in fig. 1 and fig. 3.
luminol-H recorded by the chemiluminescence apparatus of FIG. 1 2 O 2 The chemiluminescence phenomenon of the system can be known, copper acetate solution with the same concentration and Cu-DOBDC solution are selected for comparison, and Cu is added 2+ The chemiluminescence intensity of the system is greater than Cu-DOBDCThe chemiluminescence intensity of the system proves the active site Cu in Cu-DOBDC 2+ After release, the luminol-H can be effectively enhanced 2 O 2 Chemiluminescence of the system.
When it is Pb 2+ When present, pb 2+ Has stronger coupling capacity with Cu-DOBDC, and can lead the active site Cu in the Cu-DOBDC to be 2+ Is released of Cu 2+ p-luminol-H 2 O 2 Has strong catalytic action, and the reaction principle is shown in figure 2.
As can be seen from FIG. 3, when Pb is reached 2+ Cu-DOBDC-luminol-H when the concentration is changed within the range of 0.5 to 50 nM 2 O 2 Chemical reflection intensity of system with Pb 2+ Increased concentration and degree of enhancement with Pb 2+ The concentration is directly proportional.
As can be seen from FIG. 4, when Pb is present 2+ When the concentration is changed within the range of 0.5-50 nM, the chemiluminescence intensity has a better linear relation with the concentration. The linear equation is Y = 50.03C +191.28 (R) 2 = 0.9974), wherein Y is the chemiluminescence intensity, and C is Pb 2+ Concentration, detection limit is 0.3 nM.
As can be seen from FIG. 5, a series of 10 times Pb was performed for 10 nM lead ions 2+ Other metal ion (Cd) 2+ 、Cr 3 + 、Hg 2+ 、Zn 2+ 、Ni 2+ 、Mn 2+ 、Mg 2+ 、Na + 、K + ) Interference experiments of (4). As a result, it was found that Cd was measured 2+ 、Cr 3+ 、Hg 2+ 、Zn 2+ 、Ni 2+ 、Mn 2+ For Cu-DOBDC-luminol-H 2 O 2 The chemiluminescence intensity of the system is inhibited. At the same time, mg 2+ 、Na + 、K + Also on Cu-DOBDC-luminol-H 2 O 2 The chemiluminescence intensity of the system is free from interference. Therefore, other metal ions have no obvious interference effect on the determination of lead ions.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (7)
1. Cu-MOF-luminol-H 2 O 2 Detection of Pb by chemiluminescence system 2+ The method is characterized in that: the method comprises the following steps:
step one, preparing Cu-DOBDC: dissolving copper acetate and 2, 5-dihydroxy terephthalic acid in a mixed solution composed of water, N-dimethylformamide and ethanol according to a certain proportion, and stirring for 1 to 20 min; transferring the mixture into a stainless steel hydrothermal reaction kettle with 200 mL of polytetrafluoroethylene lining for reaction, and washing the mixture with ultrapure water and absolute ethyl alcohol respectively after the reaction is finished; drying the mixture in a vacuum drying box at 30 to 100 ℃ for later use;
second step, cu-MOF-luminol-H 2 O 2 Detection of Pb by chemiluminescence system 2+ : diluting step by step to obtain 1.0 × 10 -4 ~1.0×10 -2 mol/L luminol reagent and 1.0X 10 -4 ~1.0×10 -2 mol/L H 2 O 2 A reagent; dissolving Cu-DOBDC in water to obtain a Cu-DOBDC solution, and taking 0.01 to 0.5 mL of the Cu-DOBDC solution and 0.01 to 0.5 mL of Pb to be detected 2+ Uniformly mixing the solution, and standing for 10 to 60 min; measuring 1-20 mu L of Cu-MOF/Pb 2+ Mixing the solutions to be tested, and adding 1 to 20 mu L of H 2 O 2 And (3) dripping 10-100 mu L of luminol solution into the reagent by adopting a flow injection method, detecting chemiluminescence, detecting a luminescence signal by using a photomultiplier, and outputting light signal intensity under analysis software of a computer.
2. The Cu-MOF-luminol-H of claim 1 2 O 2 Detection of Pb by chemiluminescence system 2+ The method is characterized in that: the molar ratio of copper acetate to 2, 5-dihydroxyterephthalic acid in the first step is 1:4 to 4:1.
3. according to the rightThe Cu-MOF-luminol-H of claim 1 2 O 2 Detection of Pb by chemiluminescence system 2+ The method of (2), characterized by: in the first step, the volume ratio of the water to the N, N-dimethylformamide to the ethanol is 1:1:1, the volume of the mixed solution is 15 to 150 mL.
4. The Cu-MOF-luminol-H according to claim 1 2 O 2 Detection of Pb by chemiluminescence system 2+ The method is characterized in that: in the first step, the reaction temperature is 50 to 200 ℃, and the reaction time is 12 to 72h.
5. The Cu-MOF-luminol-H according to claim 1 2 O 2 Detection of Pb by chemiluminescence system 2+ The method of (2), characterized by: in the second step, the luminol is 3-aminophthalic anhydride, and the concentration of the stock solution is 1.0 multiplied by 10 -2 mol/L; the preparation method comprises the following steps of weighing 0.1772-1.7716 g of luminol, dissolving the luminol with 0.10 mol/L of NaOH, transferring the luminol into a 100-1000 mL brown volumetric flask, fixing the volume with ultrapure water, keeping the volumetric flask in the dark for more than one week, and gradually diluting the volumetric flask when in use.
6. The Cu-MOF-luminol-H according to claim 1 2 O 2 Detection of Pb by chemiluminescence system 2+ The method is characterized in that: in the second step, the concentration of the Cu-DOBDC solution is 5 to 50 mg/mL, and the concentration of Pb to be measured is different from that of Pb to be measured 2+ The solution mixing volume ratio is 50:1 to 1:50.
7. the Cu-MOF-luminol-H according to claim 1 2 O 2 Detection of Pb by chemiluminescence system 2+ The method of (2), characterized by: the Cu-MOF/Pb in the second step 2+ Mixing the solution to be tested, luminol and H 2 O 2 The mixing volume ratio when tested was 1:1:5 to 1:1:10.
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