CN116337852A - Cr simulating enzyme activity based on two-dimensional MOFs oxide 6+ Rapid detection method and test paper - Google Patents
Cr simulating enzyme activity based on two-dimensional MOFs oxide 6+ Rapid detection method and test paper Download PDFInfo
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Abstract
The invention belongs to the technical field of heavy metal detection, and particularly relates to Cr based on two-dimensional MOFs oxide simulated enzyme activity 6+ A rapid detection method and test paper. The invention firstly utilizes a surfactant-mediated method to prepare the two-dimensional MOFs nano material with a lamellar structure, then mixes the two-dimensional MOFs nano material with BR buffer solution, TMB and halogen ions to form a catalytic reaction system, and then utilizes a method for drawing a quantitative analysis standard working curve to rapidly test Cr of a sample to be tested 6+ Concentration of Cr at the same time 6+ Preparing a rapid detection test paper based on the rapid detection method to realize Cr 6+ Visual inspection of (c). The invention does not depend on large instruments and professional operators, has stable and safe reagent, high sensitivity and simple and convenient test paper operation, and can qualitatively judge Cr as low as 50ppb by naked eyes 6+ The whole process is simple and quick, and can realize Cr in samples such as basic-layer environmental water and the like 6+ And the content is detected on site, rapidly and sensitively.
Description
Technical Field
The invention belongs to the technical field of heavy metal detection, and particularly relates to Cr based on two-dimensional MOFs oxide simulated enzyme activity 6+ A rapid detection method and test paper.
Background
Chromium is widely used in the industries of electroplating, metallurgy, tanning, dyeing and the like in the modern industry. The emission of three wastes in the factory causes the continuous release of heavy metal chromium into the environment, which causes serious harm to human health, and is one of the necessary measurement items for environmental monitoring. Chromium in nature has various valence states, and common Cr 3+ And Cr (V) 6+ The biological activity difference between the two is obvious. Wherein Cr is 3+ Is a trace element essential for human body, and Cr 6+ Is a recognized human respiratory carcinogen because of relatively stronger fluidity and carcinogenic properties and greater harm to human health. In view of this, the world health organization clearly specifies Cr in groundwater 6+ And cannot exceed 50ppb. The traditional heavy metal chromium detection usually depends on large instruments and professional operators, has high detection cost, can only detect the total chromium content in a sample, and can not selectively detect Cr 6+ The method comprises the steps of carrying out a first treatment on the surface of the The quick detection method popularized in the market has low sensitivity, and can not meet the requirement of vast base layers on heavy metal Cr in samples such as environmental water and the like due to the dependence on toxic and harmful reagents such as mercury and the like and expensive reagents such as antibodies and the like 6+ Trace, economical, safe, accurate screening requirements.
The nano enzyme has activity similar to that of natural enzyme, and has higher stability, more flexible structure and composition design compared with the natural enzymeIn recent years, researchers have paid attention to adjustable catalytic activity and the like, and they have been widely used for analysis and detection in the fields of inorganic ions, toxins, bacteria and the like. Metal Organic Frameworks (MOFs) are ordered porous crystalline materials formed by coordination of metal centers and organic ligands, and are a typical class of nano-enzyme materials. They can be classified into two-dimensional MOFs and three-dimensional MOFs according to their structures. Compared with the three-dimensional massive MOFs, the two-dimensional MOFs have ultrathin thickness and huge surface area, can expose more surface active sites, can enhance the interaction with substrate molecules TMB and the like in a nano enzyme chromogenic reaction system, and improve the adsorption capacity of the substrate molecules TMB and the like, thereby providing a powerful condition for improving the catalytic reaction efficiency and the detection sensitivity of targets. Meanwhile, the ultrathin lateral dimension can effectively shorten the diffusion distance of substrate molecules TMB and the like in a color reaction system, and accelerate the catalytic response to the substrate molecules. Therefore, it is necessary to realize Cr using MOFs nanomaterials 6+ Is rapid, simple and highly sensitive.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention realizes Cr by utilizing the activity of the two-dimensional MOFs oxide mimic enzyme based on the mediation effect of halogen ions 6+ Is rapid, simple and highly sensitive.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
the first aspect of the invention provides a Cr-based two-dimensional MOFs oxide-simulated enzyme activity 6+ A rapid detection method comprising the steps of:
s1, dissolving metal ions with variable valence, an organic ligand, a surfactant and benzoic acid in a mixed solvent of ethanol and N, N-dimethylformamide, then performing heating treatment under a stirring condition, and finally washing and resuspension to obtain a two-dimensional MOFs nano material;
s2, mixing the two-dimensional MOFs nano material obtained in the step S1, BR buffer solution, 3', 5' -tetramethyl benzidine (TMB) solution and halide ion solution to prepare a catalytic reaction system, and then adding Cr with different concentrations 6+ The standard solution is reacted, finally ultraviolet is usedVisible absorbance photometer test Cr 6+ The change of absorbance of TMB oxidation product at 652nm after addition is calculated by Cr 6+ Drawing a quantitative analysis standard working curve by taking the concentration as an abscissa and the absorbance change value as an ordinate;
s3, will contain Cr 6+ Adding the sample to be detected into the catalytic reaction system of the step S2, detecting the absorbance value of the sample at 652nm after the reaction, and calculating Cr in the sample to be detected according to the quantitative analysis standard working curve drawn in the step S2 6+ Is a concentration of (3).
The invention takes a surfactant as a mediating molecule, takes metal ions with variable valence states as a metal center, takes an organic ligand and benzoic acid as a regulating molecule, obtains two-dimensional MOFs with lamellar structure, then mixes the MOFs with BR buffer solution, 3', 5' -tetramethyl benzidine (TMB) and halogen ions to form a catalytic reaction system, and adopts Cr based on the mediating effect of the halogen ions 6+ The activity of two-dimensional MOFs oxide mimic enzyme is regulated and controlled to construct the selective detection Cr 6+ The method realizes Cr in samples such as basic layer environmental water and the like 6+ Is rapid, simple and highly sensitive.
Preferably, in step S1, the metal ion of variable valence is selected from Cu 2+ 、Ce 3+ 、Ce 4+ The organic ligand is TCPP, the surfactant is PVP, and the volume ratio of the ethanol to the N, N-dimethylformamide is 1:3.
Preferably, in the step S1, the concentration of the metal ions in the variable valence state is 0.05-0.5mg/mL, the concentration of the organic ligand is 0.1-0.5mg/mL, the concentration of the surfactant is 0.1-1mg/mL, and the concentration of the benzoic acid is 1-10mg/mL.
Preferably, in the step S1, the heating treatment is oil bath heating at 90-95 ℃ for 3-5h.
Preferably, in step S2, the BR buffer has a pH of 2 to 5, the TMB solution has a concentration of 0.5mM to 30mM, the halide solution has a concentration of 0.1M to 2M, and the halide ions in the halide solution are selected from the group consisting of I - 、Cl - 、Br - The method comprises the steps of carrying out a first treatment on the surface of the The volume ratio of the two-dimensional MOFs nano material, the BR buffer solution, the TMB solution and the halide ion solution is 0.5-20:150-170:5-15:5-15。
Preferably, in step S2, cr 6+ The concentrations of the standard solutions were 0.5ppb, 5ppb, 10ppb, 25ppb, 50ppb, 100ppb, 0.25ppm, 0.5ppm, 1ppm, 1.5ppm, 2ppm, 2.5ppm, 3ppm, 4ppm and 5ppm, respectively, the test wavelength of absorbance was 652nm, and the equation of the quantitative analysis standard working curve drawn was: y=0.69973x+0.00415, r 2 0.9989, x is Cr 6+ Concentration, y is the absorbance change value at 652nm, and Cr is detected 6+ The linear range of (2) is 0.5ppb to 2ppm.
Preferably, in step S2, cr is added to the catalytic reaction system 6+ The reaction time after standard solution is 2-5min, and the reaction temperature is 20-25 ℃.
Preferably, in step S1, the washing is sequentially performed with ethanol and water, and the solution used for resuspension is water.
In a second aspect, the present invention provides a Cr-based two-dimensional MOFs oxide-mimetic enzyme activity 6+ Quick test paper, the Cr 6+ The preparation method of the rapid detection test paper comprises the following steps: and (3) placing the test paper in the catalytic reaction system of the first aspect for soaking treatment, and drying to obtain the catalyst.
Cr according to the first aspect of the invention 6+ Based on the rapid detection test method, rapid detection test paper is prepared to realize Cr 6+ Further promote Cr in samples such as basic layer environment water and the like 6+ Is rapid, simple and highly sensitive. In addition, the invention does not need to rely on large-scale instruments and professional operators, has stable reagent, safety, environmental protection and high sensitivity, and can detect Cr as low as 50ppb by naked eyes with test paper 6+ 。
Preferably, the soaking treatment is carried out for 2-5 hours, and the drying is carried out at room temperature.
A third aspect of the present invention provides Cr based on two-dimensional MOFs oxide-mimetic enzyme Activity according to the second aspect 6+ The application of the rapid detection test paper specifically comprises the following steps: cr with different concentrations is firstly added 6+ Dripping standard solution onto rapid test paper to obtain color chart, and according to Cr-containing material 6+ To be treated of (2)The color change of the sample on the rapid detection test paper is directly read out Cr of the sample to be detected through the colorimetric card 6+ Concentration.
Preferably, cr 6+ The concentrations of the standard solutions of (a) were 0, 50, 100, 250, 500, 1000ppb, respectively.
Compared with the prior art, the invention has the beneficial effects that:
the invention discloses a Cr based on two-dimensional MOFs oxide simulated enzyme activity 6+ The rapid detection method and test paper comprises preparing two-dimensional MOFs nano material with lamellar structure by surfactant-mediated method, mixing with BR buffer solution, 3', 5' -tetramethyl benzidine (TMB) and halogen ion to form a catalytic reaction system, and rapidly testing Cr of sample to be tested by drawing quantitative analysis standard working curve 6+ Concentration of Cr at the same time 6+ Preparing a rapid detection test paper based on the rapid detection method to realize Cr 6+ Visual inspection of (c). The two-dimensional MOFs nano material provided by the invention has the advantages of simple synthesis process and good stability; the addition of halogen ions in the invention can well promote Cr 6+ The regulation and control effect on the activity of the two-dimensional MOFs oxide mimic enzyme is further improved, so that the reaction speed is increased, and the reaction sensitivity is improved; cr in the invention 6+ Has regulating and controlling effects on the activity of two-dimensional MOFs oxide mimic enzyme and Cr 3+ Does not exist, thereby fundamentally guaranteeing the Cr 6+ Is selected from the group consisting of (1); the method of the invention does not depend on large instruments and professional operators in the use process, has stable and safe reagent, high sensitivity and simple and convenient test paper operation, and can qualitatively judge Cr as low as 50ppb by naked eyes 6+ The whole process is simple and quick. Thus, cr of the present invention 6+ Rapid detection method and test paper can realize Cr in samples such as basic-level environmental water 6+ And the content is detected on site, rapidly and sensitively.
Drawings
FIG. 1 is a TEM characterization of two-dimensional MOFs nanomaterials;
FIG. 2 is Cr 6+ A detected ultraviolet-visible absorption spectrum;
FIG. 3 is a graph showing the kinetics of the reaction system before (left) and after (right) sodium chloride addition;
FIG. 4 shows the detection of Cr 6+ Is a standard working curve of (2);
FIG. 5 is a diagram showing the detection of Cr 6+ Is (from left to right, the added ions are Pb respectively) 2+ 、Cd 2+ 、Hg 2+ 、As 3+ 、As 5+ 、Ag + 、Fe 3+ 、Zn 2+ 、Mn 2+ 、Cr 3+ 、Br - 、Cr 6+ Wherein Cr 6+ Concentration of 250ppb, other ion concentrations of 1 ppm);
FIG. 6 shows a rapid test strip for Cr concentrations 6+ Response graph (from left to right Cr 6+ The concentration was 0, 50, 100, 250, 500, 1000ppb in order).
Detailed Description
The following describes the invention in more detail. The description of these embodiments is provided to assist understanding of the present invention, but is not intended to limit the present invention. In addition, the technical features of the embodiments of the present invention described below may be combined with each other as long as they do not collide with each other.
The experimental methods in the following examples, unless otherwise specified, are conventional, and the experimental materials used in the following examples, unless otherwise specified, are commercially available.
Example 1Cr which mimics enzymatic Activity based on two-dimensional MOFs oxide 6+ Rapid detection method and test paper
1. Preparation of two-dimensional MOFs nano-material
First, 9mg of Cu (NO 3 ) 2 0.1124g of benzoic acid, 10mg of polyvinylpyrrolidone (PVP) and 4mg of tetra (4-carboxyphenyl) porphine (TCPP) are sequentially added into 5mL of absolute ethyl alcohol and 15mL of N, N-Dimethylformamide (DMF) for ultrasonic dissolution; then, placing the mixture in an oil bath under stirring (1200 rpm) and heating at 95 ℃ for 3-5h; finally, cool to room temperature, wash 3 times with absolute ethanol, deionized water, centrifuge each (8000 rpm,5 min) in sequence, and re-suspend all products in 1The concentration after resuspension was 0.1mg/mL in 0mL deionized water.
TEM test was performed on the two-dimensional MOFs nano-materials synthesized above, and as shown in FIG. 1, the obtained MOFs material had a lamellar structure with wrinkles at some positions.
2、Cr 6+ Fast detection method of (2)
Firstly, 160 mu LBR buffer (pH=4), 10 mu L of two-dimensional MOFs nano-material, 10 mu LTMB solution (10 mM) and 10 mu LNaCl solution (2M) are mixed uniformly at room temperature to form a catalytic reaction system, and then 10 mu L of Cr with different concentrations (0-5 ppm) are continuously added 6+ The standard solution was mixed and reacted for 5min. Finally, cr is tested by means of an ultraviolet-visible absorption photometer 6+ Changes in absorbance values of TMB oxidation products at 652nm absorbance peaks before and after addition.
At 1ppm Cr 6+ For example, the test conditions were: the scanning wavelength range is 800-450nm, and the ultraviolet-visible absorption spectrum chart of the process and the ultraviolet-visible absorption spectrum chart in the presence or absence of sodium chloride are shown in figure 2, wherein the ultraviolet-visible absorption spectrum chart is measured for 3-5 times in parallel. As a result, it was found that the presence of NaCl significantly increased Cr 6+ And the catalytic activity of the two-dimensional MOFs nano material is regulated and controlled. Further by monitoring the presence of sodium chloride, 1ppm Cr is added 6+ And (3) after different reaction times (0-35 min), drawing corresponding reaction kinetics curves by taking the reaction time as an abscissa and the absorbance change value as an ordinate, wherein the absorbance change value of the TMB oxidation product at 652nm is shown in the result of FIG. 3. From the results, the addition of NaCl greatly improves the speed of the color reaction, shortens the reaction saturation time from 30min to 5min, and ensures more complete reaction.
Finally, cr is used as 6+ The concentration is shown on the abscissa (x) and the absorbance change at 652nm is shown on the ordinate (y), and a standard operating curve shown in FIG. 4 was obtained. The curve equation is y=0.69973x+0.00415, r 2 0.9989. Cr detection 6+ The linear range of (2) is 0.5ppb to 2ppm.
In addition, for detecting Cr 6+ A selectivity experiment for common ions was performed. Cr (Cr) 6+ At a concentration of 250ppb, other ions (Pb 2 + 、cd 2+ 、Hg 2+ 、As 3+ 、As 5+ 、Ag + 、Fe 3+ 、Zn 2+ 、Mn 2+ 、Cr 3+ 、Br - ) The concentration of (2) was 1ppm, and the results are shown in FIG. 5. From the test results, it can be seen that common ions are specific to Cr 6+ The detection has little influence, cr 3+ The signal after the addition is very weak and basically can be ignored, which shows that the method can selectively detect Cr 6+ 。
3、Cr 6+ Detection test paper and visual detection method
The conventional filter paper was cut into 0.5cm by 0.5cm sizes and placed in a volume ratio of 16:1:1:1 (pH 4.0), two-dimensional MOFs nano-material, 3', 5' -tetramethyl benzidine (TMB) solution (10 mM) and NaCl solution (2M), soaking for 2h, taking out, and air drying at room temperature to obtain Cr 6+ And (5) rapidly detecting test paper.
Will contain Cr 6+ The standard solutions (0, 50, 100, 250, 500, 1000 ppb) of the above-mentioned materials are dropped onto a rapid test paper, and the color change can be observed after 1-2min of reaction. As shown in FIG. 6, with Cr 6+ The blue color of the test paper is deeper and deeper, and Cr as low as 50ppb can be detected by naked eyes 6+ . It can be seen that by making a standard color chart, the color chart is prepared according to the Cr content 6+ The color change of the solution to be detected on the rapid detection test paper can directly read Cr in the solution to be detected 6+ Concentration.
Example 2 Cr which mimics enzymatic Activity based on two-dimensional MOFs oxides 6+ Application of rapid detection method
The east lake water, mountain spring water and tap water were centrifuged (12000 rpm,5 min) to remove impurities. Next, 100, 500 and 1000ppb Cr were added thereto, respectively 6+ Standard solution as Cr 6+ The samples were simulated, and after thoroughly mixing, cr was performed as in example 1 6+ And (5) detecting. By measuring Cr 6+ Adding the change value of absorbance of TMB oxidation product at 652nm in the system and then calculating Cr in the simulation sample according to the working curve obtained in example 1 6+ The concentration and recovery rate of (2) are shown in Table 1.
From table 1, the recovery rates of the three groups of eastern lake water, the three groups of mountain spring water and the three groups of tap water simulation samples are all between 96% and 103%, and the result shows that the method has good effect in the actual sample detection.
TABLE 1Cr 6+ Test results of simulation samples
In conclusion, the invention utilizes Cr through the mediation of halogen ions 6+ The catalytic activity of the two-dimensional MOFs nano material is effectively regulated and controlled, the efficiency of the color reaction is further improved, and Cr is further improved 6+ Sensitivity of detection. Meanwhile, the visual test paper prepared by the catalytic system is Cr in samples such as wide-large-base environmental water 6+ Provides powerful technical support for on-site, rapid detection of (c).
The embodiments of the present invention have been described in detail above, but the present invention is not limited to the described embodiments. It will be apparent to those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, and yet fall within the scope of the invention.
Claims (10)
1. Cr simulating enzyme activity based on two-dimensional MOFs oxide 6+ The rapid detection method is characterized by comprising the following steps of:
s1, dissolving metal ions with variable valence, an organic ligand, a surfactant and benzoic acid in a mixed solvent of ethanol and N, N-dimethylformamide, then performing heating treatment under a stirring condition, and finally washing and resuspension to obtain a two-dimensional MOFs nano material;
s2, mixing the two-dimensional MOFs nano material, the BR buffer solution, the TMB solution and the halide ion solution in the step S1 to prepare a catalytic reaction system, and then adding Cr with different concentrations 6+ The standard solution is reacted, and finally, an ultraviolet-visible absorbance photometer is used for testing Cr 6 + The change of absorbance of TMB oxidation product at 652nm after addition is calculated by Cr 6+ Drawing a quantitative analysis standard working curve by taking the concentration as an abscissa and the absorbance change value as an ordinate;
s3, will contain Cr 6+ Adding the sample to be detected into the catalytic reaction system of the step S2, detecting the absorbance value of the sample at 652nm after the reaction, and calculating Cr in the sample to be detected according to the quantitative analysis standard working curve drawn in the step S2 6+ Is a concentration of (3).
2. The Cr-based two-dimensional MOFs oxide mimetic enzyme activity of claim 1 6+ A rapid detection method is characterized in that in the step S1, the metal ions with variable valence are selected from Cu 2+ 、Ce 3+ 、Ce 4+ The organic ligand is TCPP, the surfactant is PVP, and the volume ratio of the ethanol to the N, N-dimethylformamide is 1:3.
3. The Cr-based two-dimensional MOFs oxide mimetic enzyme activity of claim 1 6+ The rapid detection method is characterized in that in the step S1, the concentration of the metal ions with variable valence is 0.05-0.5mg/mL, the concentration of the organic ligand is 0.1-0.5mg/mL, the concentration of the surfactant is 0.1-1mg/mL, and the concentration of the benzoic acid is 1-10mg/mL.
4. The Cr-based two-dimensional MOFs oxide mimetic enzyme activity of claim 1 6+ The rapid detection method is characterized in that in the step S1, the heating treatment is oil bath heating at 90-95 ℃ for 3-5h.
5. The Cr-based two-dimensional MOFs oxide mimetic enzyme activity of claim 1 6+ A rapid detection method is characterized in that in step S2, the pH of BR buffer is 2-5, the concentration of TMB solution is 0.5mM-30mM, the concentration of halide ion solution is 0.1M-2M, and halide ions in the halide ion solution are selected from I - 、Cl - 、Br - The method comprises the steps of carrying out a first treatment on the surface of the The volume ratio of the two-dimensional MOFs nano material, the BR buffer solution, the TMB solution and the halide ion solution is 0.5-20:150-170:5-15:5-15.
6. The Cr-based two-dimensional MOFs oxide mimetic enzyme activity of claim 1 6+ The rapid detection method is characterized in that in the step S2, cr is contained in the sample 6+ The concentrations of the standard solutions were 0.5ppb, 5ppb, 10ppb, 25ppb, 50ppb, 100ppb, 0.25ppm, 0.5ppm, 1ppm, 1.5ppm, 2ppm, 2.5ppm, 3ppm, 4ppm and 5ppm, respectively, the test wavelength of absorbance was 652nm, and the equation of the quantitative analysis standard working curve drawn was: y=0.69973x+0.00415, r 2 0.9989, x is Cr 6+ Concentration, y is the absorbance change value at 652nm, and Cr is detected 6+ The linear range of (2) is 0.5ppb to 2ppm.
7. The Cr-based two-dimensional MOFs oxide mimetic enzyme activity of claim 1 6+ A rapid detection method is characterized in that in the step S2, cr is added into a catalytic reaction system 6+ The reaction time after standard solution is 2-5min, and the reaction temperature is 20-25 ℃.
8. Cr simulating enzyme activity based on two-dimensional MOFs oxide 6+ The rapid detection test paper is characterized in that the Cr 6+ The preparation method of the rapid detection test paper comprises the following steps: the test paper is placed in the catalytic reaction system in the step S2 of claim 1 for soaking treatment, and is dried to obtain the catalyst.
9. The Cr-based two-dimensional MOFs oxide mimetic enzyme activity of claim 8 6+ The rapid detection test paper is characterized in that the soaking treatment time is 2-5h, and the drying is room temperature airing.
10. Cr based on two-dimensional MOFs oxide mimic enzymatic activity according to claim 8 or 9 6+ The application of the rapid detection test paper is characterized in that Cr with different concentrations is firstly used 6+ Dripping standard solution onto rapid test paper to obtain color chart, and according to Cr-containing material 6+ Color change of sample to be tested on rapid test paperCr of sample to be measured is directly read out through colorimetric card 6+ Concentration.
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| CN117003293B (en) * | 2023-07-31 | 2024-04-05 | 武汉理工大学 | Modified Co 3 O 4 MOFs composite gas-sensitive material and preparation method and application thereof |
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