A kind of metacarb three-signal sensing material and its preparation method and application

A technology of sensing material and kumetcarb, which is applied in analysis materials, material impedance, material excitation analysis, etc., can solve the problems of biological enzymatic method being difficult to preserve, unable to perform on-site detection, and ineffective in detection, etc., to achieve the preparation method. Simple and easy to implement, reduce detection cost, and high reliability

Inactive Publication Date: 2017-07-11
HUAZHONG NORMAL UNIV
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  • Description
  • Claims
  • Application Information

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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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  • A kind of metacarb three-signal sensing material and its preparation method and application
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  • A kind of metacarb three-signal sensing material and its preparation method and application

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Embodiment 1 2

[0031] The preparation of embodiment 1 dinaphthalene calix [4] arene

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

[0033] (1) Preparation of calix[4]arenediynes

[0034] 5.0g (7.7mmol) p-tert-butylcalix [4]arene, 3.3g (23mmol) potassium carbonate, 2.5mL (23mmol) propyne bromide, and 150mL acetone were added to the three-necked flask, reflux reaction, TLC until The reaction of p-tert-butylcalix[4]arene is complete. Cool, filter with suction, wash the filter cake several times with acetone, spin the filtrate and recrystallize 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]arenediyne dibutyl bromide

[0036] Add 1.0g (1.4mmol) p-tert-butylcalix[4]diyne, 40mL anhydrous DMF, 0.28g (11.7mmol) NaH into the ...

Embodiment 2 2

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

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

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

Embodiment 3 2

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

[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 methiocarb three-signal sensing material, a preparation method and application thereof. Background technique [0002] With the development of society, the irrational use of pesticides leads to more and more serious environmental pollution. Therefore, the detection of pesticides has always been a problem worthy of attention. 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. To the scene inspection. However, 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 pesticides. Therefore, the developme...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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