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Selective photoelectrochemical analysis method for microcystin MC-LR in water

A MC-LR, microcystin technology, applied in the field of photoelectrochemical analysis and environmental detection, can solve the problems of complex sample pretreatment and unsatisfactory accuracy, and achieve improved photoelectrochemical performance, good selectivity and sensitivity, low cost effect

Inactive Publication Date: 2017-03-01
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the detection method for MC-LR in this patent has high sensitivity, the sample pretreatment is relatively complicated, and the detection accuracy is not ideal due to the indiscriminate oxidation of OH during chromatographic analysis.

Method used

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  • Selective photoelectrochemical analysis method for microcystin MC-LR in water

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Experimental program
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Effect test

Embodiment 1

[0033] A new method for selective photoelectrochemical analysis of microcystin MC-LR in water, the specific preparation process of the working electrode is as follows:

[0034] (1) Synthesis of alkyne-modified graphene (G-alkyne): Graphene oxide (GO) was prepared by the Hummers method, prepared into a 2g / L aqueous solution, ultrasonically dispersed for 3h, and then added with a concentration of 1v / v% N 2 h 4 ·H 2 GO is reduced by O, and the NH 3 ·H 2 O adjusted the pH of the mixture to 11.00, and the mixture was stirred and reacted at 90° C. for 1 h. Then 4-ethynylaniline and isoamyl nitrite were added to make the concentrations respectively 0.5wt% and 0.6v / v%, and the mixture was stirred vigorously at 80°C overnight. Then cooled to room temperature, centrifuged and filtered. The filtrate was washed with deionized water and dilute HCl until the filtrate was clear, and dried under vacuum at 50 °C overnight.

[0035] (2) Graphene on TiO 2 Assembly of the surface of NTs: A...

Embodiment 2

[0039] Using the traditional three-electrode system, the Aptamer / G / TiO prepared in Example 1 2 NTs is the working electrode, the saturated calomel electrode is the reference electrode, the platinum wire electrode is the counter electrode, and 0.1M PBS buffer solution with a pH of 7.4 is used as the supporting electrolyte. Different concentrations of MC-LR standard solutions are added to the system to control the MC- The interaction time between LR and aptamer was 45min at room temperature. Under the excitation of visible light, a bias voltage of 0.3V was applied, and the photocurrent of the system containing different concentrations of MC-LR was measured by I-t curve method, which was converted into photocurrent density (j) according to the working area of ​​the electrode. Within a certain range of MC-LR concentration, as the concentration of MC-LR increases, the photocurrent density also increases correspondingly. Part of the aptamer is caused to dissociate from the electrod...

Embodiment 3

[0041] Aptamer / G / TiO prepared with 2 NTs were used as working electrodes, saturated calomel electrodes were used as reference electrodes, platinum wire electrodes were used as counter electrodes, and 0.1M PBS buffer solution with pH 7.4 was used as supporting electrolyte. Apply 0.3V bias voltage under visible light excitation, and use I-t curve method to measure the photocurrent of 99.5pg / L MC-LR solution and interfering substance system respectively. The interfering substance system is a mixed solution of MC-LR and interfering substance. The concentration of MC-LR in the system is 99.5pg / L, the concentration of interfering substances is 100 times of the molar concentration of MC-LR, and the relative photocurrent ratio (R) is calculated to obtain the selectivity of the sensor. Interfering substances include monosultap, atrazine, glyphosate, omethoate, paraquat, trichlorfon, and acetamidin. The results show that when interfering substances are monosultap, atrazine, glyphosate,...

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Abstract

The present invention relates to a selective photoelectrochemical analysis method for microcystin MC-LR in water. According to the present invention, graphene is chemically bonded to TiO2NTs through clicking chemistry so as to substantially improve the photoelectrochemical performance of the base electrode, the graphene modified TiO2NTs electrode and a MC-LR nucleic acid aptamer construct a MC-LR photoelectrochemical aptamer sensor, and the standard working curve of MC-LR is determined by using the photoelectrochemical analysis method, such that the MC-LR concentration in the sample to be detected can be detected by detecting the photocurrent density of the sample to be detected and combining the standard working curve; and compared to the method in the prior art, the method of the present invention has advantages of high detection sensitivity, simple detection method, high selectivity, and the like.

Description

technical field [0001] The invention relates to the technical field of photoelectrochemical analysis and environmental detection, in particular to a selective photoelectrochemical analysis method of microcystin MC-LR in water. Background technique [0002] In the past few decades, with the eutrophication of surface water and the change of global climate, a large number of cyanobacterial blooms have been caused every year. Microcystins (MCs) are biologically active monocyclic heptapeptide compounds produced by blue-green algae such as Microcystis, Anabaena, and Oscillatoria in water. Microcystin has a stable chemical structure and is easy to accumulate and enrich in organisms. Among more than 90 kinds of microcystins whose structures have been discovered and confirmed, microcystin-LR (MC-LR) is the most common and the most toxic. The molecular formula of MC-LR is C 49 h 74 N 10 o 12 , the molecular weight is 995.2. MC-LR exhibits strong hepatotoxicity, enters the liver...

Claims

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Application Information

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IPC IPC(8): G01N27/30
Inventor 刘梅川于静赵国华
Owner TONGJI UNIV
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