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Meta-tolyl-N-methylcarbamate ternary signal sensing material as well as preparation method and application thereof

A technology of sensing materials and methacarb, which is applied in the analysis of materials, material impedance, material excitation analysis, etc., can solve the problems of inability to achieve on-site detection, difficult storage of biological enzyme methods, and ineffective detection, so as to reduce detection The cost, the preparation method are simple and easy, and the effect of high reliability

Inactive Publication Date: 2015-08-26
HUAZHONG NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chromatography and bio-enzyme methods are commonly used in pesticide detection. Chromatography includes high-performance liquid chromatography (HPLC), gas chromatography (GC), etc., but these methods are cumbersome to operate, the equipment is relatively expensive, and the detection is not effective and cannot be done. On-site testing
However, the biological enzyme method is not easy to preserve after being heated, and generally can only detect a class of pesticides without the ability to select pesticides

Method used

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  • Meta-tolyl-N-methylcarbamate ternary signal sensing material as well as preparation method and application thereof
  • Meta-tolyl-N-methylcarbamate ternary signal sensing material as well as preparation method and application thereof
  • Meta-tolyl-N-methylcarbamate ternary signal sensing material as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1 2

[0031] Example 1 Preparation of dinaphthalene calix[4] arenes

[0032] For the synthetic route of dinaphthalene calix[4]arene, see figure 1 , the specific process is as follows:

[0033] (1) Preparation of calix[4]arene diyne

[0034] 5.0g (7.7mmol) p-tert-butylcalix[4]arene, 3.3g (23mmol) potassium carbonate, 2.5mL (23mmol) bromopropyne, 150mL acetone were added to the three-necked flask, the reaction was refluxed, and the thin layer was followed until The reaction of p-tert-butylcalix[4]arene was complete. Cooling, suction filtration, washing the filter cake with acetone for several times, the filtrate is spin-dried and recrystallized to obtain 4.2 g of p-tert-butylcalix[4]diyne as a white powder with a yield of 75.4%. 1 H NMR (600MHz, CDCl 3 )δ: 7.07(s, 4H), 6.72(s, 4H), 4.75(d, 4H), 4.37(d, 4H), 3.33(d, 4H), 2.54(s, 2H), 1.32(s, 18H) ), 0.91(s, 18H).

[0035] (2) Synthesis of calix[4]arenediynedibutyl bromide

[0036] 1.0g (1.4mmol) of p-tert-butylcalix[4]diyne, 40m...

Embodiment 2 2

[0039] Example 2 Preparation of dinaphthalene calix[4]arene modified gold interface (NOC4SAMs)

[0040] The schematic diagram of the construction of dinaphthalene calix[4]arene-modified gold interfaces (NOC4SAMs) is shown in figure 2 , the specific process is as follows:

[0041] Immerse the gold electrode in H 2 SO 4 The impurities on the surface of the electrode were removed in the solution for 30 min, and then immersed in ethanol and water for 5 min. After natural air drying, the gold electrode was polished with alumina powder with a particle size of 0.05 μm, and washed in an ultrasonic bath of water, ethanol and water in turn. After 3 minutes, a smooth, clean and fresh gold electrode surface was obtained. After drying, in a three-electrode system, this electrode was inserted at 0.5M H 2 SO 4 , sweep CV for 15 circles at a potential of 0-1.5V and an amplitude of 100mV / s to obtain a stable current signal. Then, it was immersed in a mixed solution of propargylamine and...

Embodiment 3 2

[0042] Example 3 Detection of carbamate pesticides by dinaphthalene calix[4]arene or dinaphthalene calix[4]arene modified gold interface (NOC4SAMs)

[0043] (1) Fluorescence method

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Abstract

The invention discloses a meta-tolyl-N-methylcarbamate ternary signal sensing material as well as a preparation method and application thereof, and belongs to the field of pesticide detection. The ternary signal sensing material adopts a dinaphthyl calix[4]arene modified gold interface, and is prepared by the method which comprises the following steps: using calix[4]arene as a raw material to be reacted with propargyl bromide and 1,2-dibromobutane respectively under the action of potassium carbonate and sodium hydride, and enabling the obtained product to be reacted with alpha-naphthol to obtain dinaphthyl calix[4]arene; modifying a gold material with an azide group, and then using a click chemistry method to modify the gold material with dinaphthyl calix[4]arene, so as to obtain the dinaphthyl calix[4]arene modified gold interface. Meta-tolyl-N-methylcarbamate can be detected by a fluorescent spectrometry with dinaphthyl calix[4]arene and can further be detected by an electrochemical impedance method and a contact angle method with the dinaphthyl calix[4]arene modified gold interface. Meta-tolyl-N-methylcarbamate is recognized by ternary signal output; the meta-tolyl-N-methylcarbamate ternary signal sensing material is reliable in result, high in sensitivity, reusable, and wide in application prospect in recognition and detection of pesticides.

Description

technical field [0001] The invention belongs to the field of pesticide detection, and in particular relates to a three-signal sensing material for kudicarb and a preparation method and application thereof. Background technique [0002] With the development of society, the unreasonable use of pesticides leads to more and more serious environmental pollution. Therefore, the detection of pesticides has always been a matter of concern. The methods often used in pesticide detection are chromatography and biological enzymes. Chromatography includes high performance liquid chromatography (HPLC), gas chromatography (GC), etc., but these methods are more complicated to operate, expensive equipment, and the detection is not practical and cannot be done. On-site inspection. The biological enzyme method is not easy to preserve after being heated, and generally can only detect one type of pesticides without the ability to select and detect pesticides. Therefore, the development of sim...

Claims

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Application Information

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IPC IPC(8): G01N27/02G01N21/64G01N13/00
Inventor 田德美李海兵杨兰兰陈聪
Owner HUAZHONG NORMAL UNIV
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