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Organic framework material containing zinc metal as well as preparation method and application of organic framework material

An organic framework and zinc metal technology, applied in the field of detection of methyl parathion using metal organic framework materials containing zinc, can solve the problems of unsuitable detection of large batches of samples, high technical quality requirements of personnel, and many influencing factors, etc., to achieve Sensitive detection, avoiding inaccurate detection results, and improving detection efficiency

Inactive Publication Date: 2017-06-30
ZHEJIANG ACADEMY OF AGRICULTURE SCIENCES
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Problems solved by technology

These methods have their own advantages and disadvantages. Chromatography is accurate but needs to be equipped with expensive large-scale analytical instruments. At the same time, it requires extremely high technical quality of personnel, which is difficult for general units to meet, and is not suitable for rapid and easy detection of large quantities of samples. The ELISA method uses many reagents, the operation is cumbersome, time-consuming, and there are many influencing factors

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  • Organic framework material containing zinc metal as well as preparation method and application of organic framework material
  • Organic framework material containing zinc metal as well as preparation method and application of organic framework material
  • Organic framework material containing zinc metal as well as preparation method and application of organic framework material

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preparation example Construction

[0033] The invention provides a method for preparing a metal-organic framework material containing zinc, comprising the following steps:

[0034] Mixing porphyrin, 4-carboxyphenylbenzene, zinc nitrate and N,N-dimethylformamide under ultrasonic conditions to obtain a mixed solution;

[0035] The mixed solution is subjected to a hydrothermal reaction to obtain a zinc-containing metal organic framework material.

[0036] In the invention, porphyrin, benzenecarboxybenzene, zinc nitrate and N, N-dimethylformamide are mixed under ultrasonic conditions to obtain a mixed solution. In the present invention, the porphyrin is preferably medium-tetra-(4-carboxyphenyl) porphyrin, four (4-aminophenyl) porphyrin or four (4-nitrophenyl) porphyrin; Benzene carboxybenzene is preferably 1,3,5-tri(4-carboxyphenyl)benzene or 1,2,4,5-tetra(4-carboxyphenyl)benzene; the zinc nitrate is preferably zinc nitrate hydrate, more Zinc nitrate hexahydrate is preferred.

[0037] In the present invention, t...

Embodiment 1

[0061] Get porphyrin 182mg, 1,2,4,5 phenylcarboxybenzene 255mg and Zn(NO 3 ) 2 ·6H 2 O 150mg in a beaker, add DMF25mL, ultrasonic 15min to make it uniform; pour the uniformly mixed solution into the reaction kettle, and react at 100°C for 24h; after the hydrothermal reaction is completed, the product is centrifuged to remove the upper liquid, and the ethanol is repeatedly centrifuged and washed 3 times; 60 The ZnPO-MOF solid powder can be obtained by drying at ℃ for 10 h.

[0062] The obtained ZnPO-MOF material was analyzed by scanning electron microscope, and the obtained results are as follows: figure 1 shown; according to figure 1 It can be seen that the ZnPO-MOF prepared by the present invention is polycrystalline stacked crystal particles;

[0063] The obtained ZnPO-MOF material is detected using an X-ray diffractometer, and the obtained XRD pattern is as follows figure 2 shown; according to figure 2 It can be seen that the peak shape of the XRD spectrum is better...

Embodiment 2

[0066] a. Weigh 1mg of the ZnPO-MOF material prepared in Example 1 into a 2mL centrifuge tube, add 1mL of absolute ethanol to make 1mg mL -1 ZnPO-MOF solution, diluted 100 times for later use;

[0067] b. Using absolute ethanol as a solvent, configure a 100ppm standard solution of methyl parathion;

[0068] c. Add 10 μg mL to 96 microwell plates numbered A1, A2, A3, and A4 respectively -1 Add 10 μL of absolute ethanol to well A1, add 10 μL of methyl parathion with a concentration of 100 ppm to well A2, add 10 μL of medicarb with a concentration of 100 ppm to well A3, and add Add phoxim 10 μ L that concentration is 100ppm, detect fluorescence intensity on microplate reader (detection condition: excitation wavelength 275nm, fluorescence wavelength 398nm), draw fluorescence intensity curve, obtained result is as follows Figure 4 Shown, wherein curve a is the fluorescence response curve of sample A1 (without adding any pesticide), curve b is the fluorescence response curve of s...

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Abstract

The invention provides a preparation method of an organic framework material containing zinc metal. The method comprises steps as follows: porphyrin, (4-carboxyphenyl)benzene, zinc nitrate and N,N-dimethylformamide are mixed under the ultrasonic condition, and a mixed solution is obtained; the mixed solution is subjected to a hydrothermal reaction, and the organic framework material containing zinc metal is obtained. The organic framework material containing zinc metal is prepared from raw materials including porphyrin, (4-carboxyphenyl)benzene and zinc nitrate, the preparation method is simple, few steps are used, fluorescent signals of the organic framework material containing zinc metal can be quenched by parathion-methyl, the fluorescence quenching degree is linearly correlated with logarithms of the content of parathion-methyl, the organic framework material containing zinc metal is used for detecting parathion-methyl, so that parathion-methyl can be rapidly, simply and sensitively detected.

Description

technical field [0001] The invention relates to the technical field of pesticide residue detection, in particular to a fluorescence method for detecting methyl parathion by using a zinc-containing metal organic framework material. Background technique [0002] Methyl parathion is a highly toxic organophosphate pesticide, its residues cause serious pollution and harm to the ecological environment. After humans eat vegetables and foods contaminated by pesticides, the pesticides remaining in them will accumulate in the human body or Enrichment, when enriched to a certain concentration, will cause acute or chronic poisoning, disease, cancer, and even death in the human body. With the improvement of living standards, people pay more and more attention to food hygiene and safety. In the import and export trade of food safety, environment and agricultural products, methyl parathion is listed as an important pollution detection substance, and it is particularly important to establi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G83/00C09K11/06G01N21/64
CPCC08G83/008C09K11/06C09K2211/188G01N21/6402G01N21/643G01N2021/6432
Inventor 徐霞红王新全王祥云王强杨华郭玉娜齐沛沛汪志威
Owner ZHEJIANG ACADEMY OF AGRICULTURE SCIENCES
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