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Preparation method of alpha-cypermethrin upconversion fluorescent sensing material

A technology of cis-cypermethrin and fluorescent sensing, which is applied in the direction of luminescent materials, material analysis and material analysis through optical means, can solve the problems of long degradation cycle, long-term existence, large dosage, etc., and achieve high selectivity and low cost , highly selective effect

Active Publication Date: 2019-01-29
TIANJIN UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to its large dosage, long degradation cycle, and high toxicity, it can exist in food and the environment for a long time, and its potential harm to human health cannot be ignored.

Method used

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  • Preparation method of alpha-cypermethrin upconversion fluorescent sensing material
  • Preparation method of alpha-cypermethrin upconversion fluorescent sensing material
  • Preparation method of alpha-cypermethrin upconversion fluorescent sensing material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] (1) 1mmol rare earth acetate RE(C 2 h 3 o 2 ) 3 (RE=78%Y, 20%Yb, 2%Er), 17mL 1-octadecene, 6mL oleic acid were placed in a 100mL three-neck flask, under stirring, raise the temperature of the system to 160°C and react for 30min; stop heating , naturally cooled to room temperature, then slowly dropwise added 10mL of methanol mixed solution containing 4mmol ammonium fluoride and 2.5mmol NaOH into the three-necked flask, and kept stirring vigorously at room temperature for 30min, then raised the system temperature to 75°C, remove methanol; after the methanol is removed, quickly raise the temperature to 300°C, and react at this temperature for 1 hour. After the reaction is completed, cool the system naturally to room temperature, then precipitate the product with excess ethanol, and wash the product three times with ethanol , and finally put the product into a vacuum drying oven at 55°C for 12 hours to obtain UCNPs;

[0036] (2) Firstly, 50 mg of the up-conversion mater...

Embodiment 2

[0044] To study the dynamic properties of the sensing material such as Figure 8 . Weigh 1 mg of imprinted polymer MIP and non-imprinted polymer NIP, place at the bottom of a 4 mL centrifuge tube and add 12 mg L -1 cis-cypermethrin standard solution 2mL each, seal the centrifuge tube with parafilm and fix it on a horizontal shaker for different time (10min, 20min, 30min, 40min, 50min, 60min, 70min, 80min), then immediately excite it with an external 980nm The fluorescent spectrophotometer of the instrument was used to measure the fluorescence intensity of the material before and after adsorption, and the adsorption kinetic curve of the fluorescent imprinted polymer material was drawn. Such as Figure 8 As shown, in the process of adsorbing cis-cypermethrin, with the extension of time, the F of the fluorescent imprinted polymer material MIP and the fluorescent non-imprinted polymer NIP 0 / F value keeps rising, when the adsorption time is 50min, F 0 The value of / F basically...

Embodiment 3

[0046] To study the adsorption performance of the sensing material (such as Figure 9 , 10 shown), weighed 1mg of imprinted polymer MIP and non-imprinted polymer NIP, placed at the bottom of a 4mL centrifuge tube, and added 2mL of different concentrations (0.1mg L -1 , 2 mg L -1 , 4 mg L -1 , 6mgL -1 , 8mgL -1 , 10 mg L -1 , 12 mg L -1 , 14 mg L -1 , 16 mg L -1 , 18 mg L -1 , 20 mg L -1 ) of the standard solution of cis-cypermethrin-acetonitrile, each concentration was set to five parallels, then the centrifuge tube was sealed with a parafilm, fixed on a horizontal shaker at room temperature and fully oscillated for 50min, and then the fluorescence spectrophotometry was performed with an external 980nm exciter The fluorescence intensity of the two polymer materials before and after adsorption was measured by the instrument, and the adsorption equilibrium curves of the fluorescent imprinted polymer material and the non-imprinted polymer material were drawn respectivel...

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Abstract

The invention provides a preparation method of an upconversion fluorescent sensing material for detecting alpha-cypermethrin. The preparation method comprises the following steps: firstly, dissolvingalpha-cypermethrin and acrylamide in a methanol / acetonitrile mixed solution, meanwhile, dissolving an upconversion-metal organic framework composite material in a methanol / acetonitrile mixed solution,carrying out ultrasonic for 1 hour, then dropwise adding the mixed solution with the dissolved alpha-cypermethrin and acrylamide into the mixed solution with the dissolved upconversion-metal organicframework composite material, adding divinyl benzene and azodiisobutyronitrile, then introducing nitrogen to remove oxygen for 30 minutes, carrying out Soxhlet extraction for 48 hours by using a mixedsolution of methanol and acetic acid after a reaction is finished, finally putting the obtained substance into a vacuum drying oven at a temperature of 50 DEG C, and carrying out drying for 12 hoursto obtain the imprinted polymer with high selectivity to alpha-cypermethrin. The preparation method has the advantages that the fluorescent composite material with high selectivity, high sensitivity,low cost and rapid fluorescence sensing detection is synthesized, and the fluorescent composite material is expected to be used as a rapid detection technology of alpha-cypermethrin (alpha-CPM) for being applied to field detection of food safety.

Description

technical field [0001] The invention belongs to the research field of optical sensing material preparation technology and pesticide residue detection method, and in particular relates to a preparation method of an upconversion-metal organic framework molecularly imprinted fluorescent sensing material and the detection of cis-cypermethrin in fruits and vegetables. Background technique [0002] In recent years, since highly toxic organochlorine and organophosphorus pesticides were banned, pyrethroid pesticides have more room for use, and the usage and sales volume of cypermethrin ranks in the forefront among pyrethroid pesticides. Cypermethrin includes 8 isomers, among which cis-cypermethrin has the characteristics of strong insecticidal ability (about 1-3 times higher than cypermethrin) and long-lasting drug effect, and is widely used in the production of agricultural products such as wheat, corn, fruits and vegetables, etc. pest control. However, due to its large dosage, lo...

Claims

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Application Information

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IPC IPC(8): C08G83/00C09K11/02G01N21/64
CPCC08G83/008C09K11/025G01N21/643
Inventor 方国臻胡雪莲赵悦清赵鹏王硕
Owner TIANJIN UNIVERSITY OF SCIENCE AND TECHNOLOGY
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