Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Method for analyzing and detecting four heterocyclic pesticides in environmental water sample

A detection method and a heterocyclic technology, applied in the directions of analyzing materials, measuring devices, material separation, etc., can solve the problems of long time, complicated extraction process, large amount of extraction agent, etc., and achieve simple operation, cheap and easy to obtain raw materials, good The effect of adsorption efficiency

Pending Publication Date: 2020-02-28
QINGDAO TECHNOLOGICAL UNIVERSITY +1
View PDF4 Cites 6 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The Chinese patent application number 201310026727.2 discloses a method for rapid detection of phenoxycarboxylic acid herbicides in water. This method uses solid phase extraction to pretreat water samples. The extraction process of this method is relatively complicated and the amount of extractant used is large.
longer time

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method for analyzing and detecting four heterocyclic pesticides in environmental water sample
  • Method for analyzing and detecting four heterocyclic pesticides in environmental water sample
  • Method for analyzing and detecting four heterocyclic pesticides in environmental water sample

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] The analysis and detection method of four kinds of phenoxycarboxylic acid pesticides in the environmental water sample that embodiment relates specifically comprises the following steps:

[0046] S1. Preparation of metal-organic framework material MIL-53 and MIL-53 film:

[0047] (1) Dissolve 3g of aluminum nitrate nonahydrate in 44mL of DMF, then add 1g of terephthalic acid and 16mL of ultrapure water, and fully stir to dissolve;

[0048] (2) reacting the mixture prepared in step (1) at 110-150° C. in a solvothermal reactor for 48 hours, washing the prepared mixture in the solvothermal reactor with DMF to obtain a MIL-53 mixed solution, The metal-organic framework material MIL-53 was prepared by vacuum drying at 100° C. for 12 hours.

[0049] (3) Weigh 0.12g of MIL-53 powder. Add 5mL of acetone to dissolve. Polyvinylidene fluoride and DMF are prepared in proportion as a mixed solvent. Add 2 mL of mixed solvent to the MIL-53 solution;

[0050] (4) Apply the mixed s...

Embodiment 2

[0057] This embodiment investigates the main factors affecting the extraction recovery of four phenoxycarboxylic acid pesticides, calculates the optimum value of each factor when the extraction recovery is the highest, and then determines the four phenoxycarboxylic acid pesticides under the conditions of the optimum value of each factor. The working curve related parameters and method detection limit and precision of oxycarboxylic acid pesticides, the specific process includes the following steps:

[0058] S1, calculate the optimal value of each factor when the extraction recovery rate of four kinds of phenoxycarboxylic acid pesticides is the highest:

[0059] (1) The investigation of the amount of adsorbent to the extraction recovery

[0060] The present invention investigates the influence of the amount of MOF on the extraction recovery rate, and the invention weighs 60, 80, 100, 120, and 140 mg of metal-organic framework material MIL-53 to prepare MOF membranes, and the con...

Embodiment 3

[0077]Determination of four phenoxycarboxylic acid pesticide residues in laboratory tap water, Laoshan Reservoir in Qingdao City, and seawater. After collecting 3 kinds of water samples, filter them with fast qualitative filter paper with a pore size of 80-120 μm, and then filter with a 0.45 μm filter membrane. The filtered water sample is measured by the method described in Example 1, and the accuracy test is carried out with the method described in Example 2, and the concentrations of four kinds of heterocyclic pesticides are respectively prepared as 1 μg / L, 10 μg / L, 40 μg / L The actual water samples with low, medium and high concentrations of L were subjected to standard addition recovery test, and each concentration point was measured 3 times, and the average value, relative standard deviation and standard recovery rate of the three determinations were calculated; among them, the three kinds of water None of the four phenoxycarboxylic acid pesticides were detected in the sam...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
lengthaaaaaaaaaa
diameteraaaaaaaaaa
Login to View More

Abstract

The invention relates to a method for analyzing and determining four heterocyclic pesticides in a water sample, and belongs to the field of pesticide detection. The method specifically comprises the following steps: preparing a metal organic framework material MIL-53 and an MIL-53 membranes; and analyzing four phenoxy carboxylic acid pesticides in the water sample by using solid-phase extraction via the metal organic framework material MIL-53 in combination of high performance liquid chromatography. The organic framework material MIL-53 with high adsorption efficiency for the four phenoxy carboxylic acid pesticides is used, and serves as a membrane solid-phase extraction material, a high performance liquid chromatography-ultraviolet fluorescence detector is adopted, the analysis method ofthe four phenoxy carboxylic acid pesticides in the water sample is established, the method is simple and convenient to operate, the analysis time and cost are greatly reduced, the extraction effect isgood, the analysis result is accurate, and the reproducibility is good; and raw materials are cheap and easy to obtain, the material preparation process is simple, the reaction conditions are mild, the application environment is friendly, and the market prospect is wide.

Description

Technical field: [0001] The invention belongs to the field of pesticide detection, and relates to an analysis and determination method for four kinds of phenoxycarboxylic acid pesticides in water samples, which utilizes membrane solid phase extraction technology and adopts metal organic framework material MIL-53 solid phase extraction-high performance liquid chromatography To determine 2,4-dichlorophenoxyacetic acid, 2-methyl-4-chlorophenoxyacetic acid, 2,4-dipropionic acid and 4-(2,4-dichlorophenoxy)-butanol in environmental water samples acid four heterocyclic pesticides. Background technique: [0002] Phenoxycarboxylic acid herbicides are the first selective herbicides put into commercial production, mainly used as stem and leaf treatment agents, applied to cereal crop fields, coniferous forests, non-cultivated land, pastures, lawns, etc., to control annual and Perennial broadleaf weed. In 1941, 2,4-dichlorophenoxyacetic acid, the first phenoxycarboxylic acid herbicide,...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/86
CPCG01N30/02G01N30/06G01N30/8679G01N2030/062
Inventor 马继平姜名珊吴阁格郭亮杨超马志伟
Owner QINGDAO TECHNOLOGICAL UNIVERSITY
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products