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Method for separating and analyzing tetracyclines in large-volume environment water sample

A technology for separation and analysis of tetracyclines, applied in material separation, analysis of materials, instruments, etc., can solve problems such as hazards and residues, and achieve the effects of high exposure rate, fast adsorption rate, and simple operation

Active Publication Date: 2019-03-22
GUILIN UNIVERSITY OF TECHNOLOGY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the improper use of antibiotics or the abuse of antibiotics will cause very serious harm. Excessive use will cause TCs to remain in environmental water through animal excrement. Therefore, it is necessary to establish a detection method for TCs in environmental water

Method used

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  • Method for separating and analyzing tetracyclines in large-volume environment water sample
  • Method for separating and analyzing tetracyclines in large-volume environment water sample
  • Method for separating and analyzing tetracyclines in large-volume environment water sample

Examples

Experimental program
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Embodiment

[0028] (1) Synthesis of PANCMA copolymer

[0029] 0.0766gNa 2 SO 3 Add 7.4074g of maleic anhydride to a three-necked flask, then add 13.15mL of acrylonitrile with a density of 0.8060g / mL and 20mL of deionized water, adjust the pH of the solution to 2.0 with commercially available dilute sulfuric acid, and heat to 60°C under nitrogen protection Then add 0.1360g of K 2 S 2 o 8 , reacted for 3 hours, took out the white polymer, rinsed it with water and absolute ethanol 3 times, filtered, and dried it in a vacuum oven (60°C) for 12 hours to obtain the PANCMA polymer. For the reaction process, see figure 1 .

[0030] (2) Synthesis of graphene oxide

[0031] In this experiment, graphene oxide was prepared by the Hummers method. The method is divided into three phases:

[0032]①Low temperature reaction: put the beaker in an ice-water bath below 4°C, add 110mL of concentrated H 2 SO 4 , insert a thermometer, and when the temperature in the beaker drops to 4°C, add 5g of flak...

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Abstract

The invention discloses a method for separating and analyzing tetracyclines in a large-volume environment water sample. An electrostatic spinning technology is adopted to prepare graphene-doped polyacrylonitrile-maleic anhydride copolymer (PANCMA-GO) electrospining nano fibers, sample liquid is stirred for 5 minutes, the trace tetracyclines in the environment water sample are extracted and enriched, analytically-pure methanoic acid / absolute methanol / analytically-pure trichloromethane mixed liquid with a volume ratio of 2 to 4 to 4 is adopted for conducting elution on the tetracyclines which are enriched on the PANCMA-GO electrospining nano fibers, eluant is collected, and is subjected to blow-dry through a termovap sample concentrator, then a methyl alcohol aqueous solution is used for dissolution again, and high performance liquid chromatography-fluorescence spectrum combination is used for analysis and measurement, so that the trace tetracyclines in the large-volume environment watersample are separated and analyzed. The method is simple to operate, good in repeatability, and high in sensibility, has a reliable detection result, and can be applied to accurate detection of traceTCs in various environment water samples.

Description

technical field [0001] The invention belongs to the technical field of separation and analysis of trace target substances in environmental samples, and in particular relates to a method for separation and analysis of trace tetracycline antibiotics in large-volume environmental water samples. The method combines electrospun nanofibers with high-performance liquid chromatography, and is suitable for the extraction, enrichment, separation and detection of trace tetracycline antibiotic targets in environmental water samples and other complex matrices. Background technique [0002] Tetracycline antibiotics (TCs) are produced by a class of terrestrial and powerful prokaryotes that mainly grow in mycelium and reproduce by spores. They are broad-spectrum antibiotics that are hydrogenated tetracene ring derivatives. Strong UV absorption and fluorescence properties, including oxytetracycline (OTC), tetracycline (TC), chlortetracycline (CTC) and doxycycline (DC), etc. These antibiotic...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/08G01N30/74D01D5/00
CPCD01D5/003G01N30/02G01N30/06G01N30/08G01N30/74G01N2030/027G01N2030/062
Inventor 杜甫佑孙灵顺阮贵华
Owner GUILIN UNIVERSITY OF TECHNOLOGY
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