Method for detecting amide and triazine herbicide residues in water body by utilizing graphene

A technology of triazines and herbicides, which is applied in the field of pesticide residue analysis in water bodies, can solve the problems of adverse effects on the environment and operators, cumbersome operation process, and large amount of solvent, so as to avoid pre-leaching activation, use less amount, Avoid the effect of repeated extraction

Inactive Publication Date: 2010-12-15
CHINA AGRI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] For the analysis of amide and triazine herbicide residues in water, the most traditional pretreatment technology is the liquid-liquid partition method, but this method consumes a large amount of solvent, which is a waste of cost, and will cause adverse effects on the environment and operators, and also To repeatedly extract, the operation process is more cumbersome
Another traditional and widely used pretreatment technology for the analysis of herbicide residues in water is solid-phase extraction, which usually uses a relatively large amount of fillers, such as adsorbents C18, C8, Florisil, and carbon black, which are commonly used in the analysis of pesticide residues. , PSA, etc., the amount of these adsorbents is generally hundreds of milligrams or more, and the small column needs to be activated by pre-drenching with solvent in advance, which wastes solvent. The small column is disposable, and the cost is relatively high

Method used

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  • Method for detecting amide and triazine herbicide residues in water body by utilizing graphene
  • Method for detecting amide and triazine herbicide residues in water body by utilizing graphene
  • Method for detecting amide and triazine herbicide residues in water body by utilizing graphene

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Effect test

Embodiment 1

[0027] Add standard solutions of alachlor, acetochlor, pretilachlor, butachlor, and metolachlor to 20 mL of deionized water so that the concentration in the water is 100 μg / L, and dilute the water sample with dilute hydrochloric acid. The pH of the sample was adjusted to 3, and then 30 mg of graphene was added to the water sample, stirred and left to stand for 60 minutes. Then the water sample was quickly passed through the filter device, and after being drained, it was eluted with 10 mL of ethyl acetate: acetone (V: V = 1: 1), the flow rate was controlled at 1 mL / min, and the elution solvent was inoculated with 2 g of anhydrous sodium sulfate. Put it into a chicken heart bottle, then rotary evaporate at 30°C to nearly dry, then blow dry with nitrogen, and finally use 2mL of n-hexane to make up the volume, pour it into the sample injection vial and use Agilent GC-MS detection, HP-5MS column, sample injection Port temperature: 290°C; column temperature: 120°C for 1min, rise to ...

Embodiment 2

[0029]Add standard solutions of atrazine, simazine, and colazine to 200 mL of deionized water, so that the concentration in the water is 50 μg / L, adjust the pH of the water sample to 11 with dilute ammonia water, and then add Add graphene 10mg in the sample, leave standstill for 5 minutes after stirring. Then the water sample was quickly passed through the filter device, pumped, and eluted with 3mL of n-hexane with a flow rate of 0.4mL / min. Evaporate to nearly dryness, then blow dry with nitrogen, and finally use 2mL of methanol to make up the volume, pour it into the sample injection vial and use Shimadzu HPLC-UVD detection, Shimadzu C18 reverse-phase chromatographic column, mobile phase: A pure water, B acetonitrile, Gradient elution conditions: 5% B for 2 min, B becomes 25% after 8 min, 70% after 8 min, 100% after 7 min, flow rate 1mL / min, injection volume: 20μL, detection wavelength: 215nm. The used graphene and the small column were washed twice with 10 mL of ethyl aceta...

Embodiment 3

[0031] In 1000mL of deionized water, add standard solutions of promethazine, proprazine, ketazine, terbuthine, prometon, isopropyl, and methoxypropane, so that the concentration in the water is 0.1 μg / L, Adjust the pH to 7, then add 50 mg of graphene to the water sample, stir and let stand for 30 minutes. Then the water sample was quickly passed through the filter device, and after being drained, it was eluted with 15mL of dichloromethane, the flow rate was controlled at 8mL / min, and the elution solvent was passed through 5g of anhydrous sodium sulfate into a chicken heart bottle, and then spun at 60°C. Evaporate to nearly dryness, then blow dry with nitrogen, and finally use 1mL ethyl acetate to make up the volume, pour it into the injection vial and use Agilent GC-NPD to detect, HP-5 column, injection port temperature: 230°C, detector: 300°C , column temperature: keep at 60°C for 2min, increase to 150°C at a rate of 15°C / min, then increase to 260°C at a rate of 15°C / min, and...

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Abstract

The invention discloses a method for detecting amide and triazine herbicide residues in a water body by utilizing graphene, which belongs to the field of analysis on pesticide residues in water bodies. The method comprises the following steps: adsorbing the amide and the triazine herbicide in the water body by using the graphene, filtering, eluting, concentrating and detecting, thereby realizing detection of the amide and the triazine herbicide in the water body. By using the graphene as an adsorbing material, the invention has the advantages of small use amount, strong adsorptive capacity and low preparation cost; the operation is simple, convenient and quick, and avoids reextraction and pre-activation; the use amount of solvent is small, the graphene and extraction columns can be recycled, thus, the invention has the advantages of environmental protection and cost saving; and the invention has high accuracy, and the recovery rate is 80-110%.

Description

technical field [0001] The invention belongs to the field of analysis of pesticide residues in water bodies, and in particular relates to a method for detecting residues of amides and triazine herbicides in water bodies by using graphene. Background technique [0002] Graphene is a new carbon material in which carbon atoms are tightly packed into a single-layer two-dimensional honeycomb lattice structure. The thickness of this graphite crystal film is only 0.335nm, which is only 1 / 200,000 of hair. The basic unit of several carbonaceous materials (such as zero-dimensional fullerene, one-dimensional carbon nanotubes, and three-dimensional graphite), with excellent crystallinity and electrical properties. Perfect graphene is two-dimensional and only includes hexagonal cells (equal hexagons); if there are pentagonal cells and heptagonal cells, it will constitute a defect in graphene; the existence of a small amount of pentagonal cells will make graphite The ene warps into shape...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06
Inventor 马永强王倩张红艳辛卓孟丽萱
Owner CHINA AGRI UNIV
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