Visible-light electrochemical analysis method by employing calixarene-modified electrode

A modified electrode and photoelectrochemical technology, applied in the direction of color/spectral characteristic measurement, etc., can solve the problems of unstable electrodes and detection methods, detection of non-electrochemically active substances, unsuitable for biomolecular detection, etc., to reduce the degree of photocorrosion, The effect of cheap and portable instrument and simple method

Inactive Publication Date: 2012-12-19
TONGJI UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, we have noticed that although the photoelectrochemical sensing technology has solved the disadvantage that electrochemical sensing cannot be used for the detection of non-electrochemically active substances, the high energy characteristics of ultraviolet light make many modified electrodes have the disadvantage of photocorrosion. , causing the instability of electrodes and detection methods, especially not suitable for the detection of biomolecules, so it is of great significance to develop photocatalytic electrode materials with visible light response
At the same time, we also realized that due to the disadvantage of photocatalytic oxidation itself with poor selectivity, this detection method does not have good selectivity. Therefore, it is necessary to functionalize the molecular recognition ability of the electrode surface to endow the electrode surface with excellent selectivity, thereby improving The specificity of photoelectrochemical detection makes it more suitable for the detection ability of actual samples with complex components

Method used

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  • Visible-light electrochemical analysis method by employing calixarene-modified electrode
  • Visible-light electrochemical analysis method by employing calixarene-modified electrode

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Embodiment 1

[0028] TiO used in the present invention 2 The NTs electrode is referred to in the literature by Maggie Paulose et al. (Anodic Growth of Highly Ordered TiO 2 Nanotube Arrays to 134 nm in Length, Maggie Paulose, Karthik Shankar et al, J.Phys.Chem.B, 2006, 110, 16179-16184) reported in the anodic oxidation method prepared, and carried out corresponding improvements, specifically The ground and polished Ti plate was used as the anode, the Pt sheet was used as the cathode, and 0.27M HF aqueous solution was used as the electrolyte, and the pre-oxidation was carried out for 1 h in a two-electrode system with an electrode distance of 1 cm and a voltage of 20 V. After pre-oxidation, in the same system, use 0.27M NH 4 The ethylene glycol solution of F is the electrolyte, and the anodic oxidation is continued for 2 hours. TiO obtained by anodic oxidation 2 NTs were sintered at 500 °C in an oxygen atmosphere with a heating rate of 1 °C / min.

[0029] References (Photoluminescence and...

Embodiment 2

[0031] A 0.1M PBS buffer solution with pH=6.98 was prepared with double distilled water, and a series of standard solutions of profenofos with different concentrations were obtained by adding different amounts of profenofos mother liquor, and 0.1M AA was added as an electron donor. The profenofos solution containing a certain concentration was used as the electrolyte in turn, and stirred for 10 minutes to rapidly and selectively enrich the profenofos on the surface of the working electrode. Stand still, under visible light, set the applied potential of 0V (Vs.SCE), adopt the method of i-t curve, measure the visible light current and record it. The used working electrode can be fully washed with ethanol and water to renew and regenerate the electrode surface. According to the concentration of profenofos and the corresponding photocurrent change rate ((i-i 0 ) / i 0 ) to draw the working curve, the detection limit of profenofos can reach 10 -9 mol L -1 .

[0032] figure 1 It...

Embodiment 3

[0034] For the determination of the actual sample, first use tap water or river water (after preliminary filtration) to prepare the actual sample, set the concentration of profenofos to 0.1 μM, adjust the pH=6.98 with 0.1M PBS buffer, and add 0.1MAA as the electron donor . Using the test conditions set in Example 2, measure the visible light current of the solution, and calculate the concentration of profenofos in the actual sample according to the working curve drawn in Example 2. The results show that the deviation between the measured concentration and the theoretical concentration is less than 5%, reflecting the good selectivity and sensitivity of the photoelectric sensing electrode.

[0035] figure 2 Functionalization of TiO for p-tert-butylcalix[4]arene 2 The change of visible photocurrent of NTs electrode before and after adding electron donor AA, the lower curve is the visible photocurrent without adding AA, and the upper curve is the visible photocurrent after addi...

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Abstract

The invention relates to a visible-light electrochemical analysis method by employing a calixarene-modified electrode. The method employs a p-tert-butylcalix[4]arene-modified TiO2 NTs electrode as a working electrode, and performs visible-light electrochemical detection on endocrine discrupting chemicals-profenofos of a real sample, with a detection sensitivity reaching 10<-9> mol.L<-1>. Compared with a conventional method, the visible-light electrochemical analysis method firstly uses p-tert-butylcalix[4]arene-functionalized TiO2 NTs in photoelectrochemical sensor electrode, particularly use in visible-light electrochemical analysis. At the same time, calixarene modification greatly improves selectivity and detection sensitivity of the electrode; interference of a plurality of co-existing small molecules can be eliminated; the detection limitation reaches to an order of magnitude of 10<-9>; the electrode is stable; and the detection method has good repeatability.

Description

technical field [0001] The invention relates to the technical fields of nanometer materials, photoelectrochemical analysis and environmental monitoring, in particular to a visible photoelectrochemical analysis method using calixarene modified electrodes. Background technique [0002] Profenofos is a broad-spectrum insecticide and an effective agent for controlling resistant cotton bollworms. It can have contact and stomach poisoning effects on pests by inhibiting acetylcholinesterase of insects. Although a small amount of profenofos residues will not cause immediate and direct poisoning to the human body, the molecular structure of profenofos is relatively stable, and it is difficult to be metabolized and excreted in organisms. Long-term consumption of water or vegetables polluted by it may cause It is an important endocrine disrupting chemical (Endocrine Disrupting Chemicals, namely EDCs), which can cause diseases such as cancer, infertility, and endocrine disorders. Vario...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/31
Inventor 史慧杰赵国华刘梅川
Owner TONGJI UNIV
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