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Determination of Phenols in Natural and Waste Waters by Capillary Electrophoresis (CAT#: STEM-ET-0157-ZJF)

Introduction

An efficient sorbent for magnetic solid-phase extraction was developed from Fe3O4 nanoparticles covered with aminated hypercrosslinked polystyrene. The sorbent has a saturation magnetization of 47 emu/g and a surface area of 509 mg/g and was tested for the extraction of 11 phenols from aqueous media. The optimum conditions were as follows: pH 3; adsorbent mass, 20.0 mg; adsorption time, 30 min; eluent (acetone) volume, 0.5 mL; and desorption time, 5 min. The enrichment factor after desorption reached 1595-1716 and the maximum adsorption capacity was 501-909 mg/g. Capillary electrophoresis was applied successively to separate 11 phenols after solid-phase extraction. The best separation was achieved using a fused silica capillary and borate buffer (pH 10.7) as a supporting electrolyte. After optimization, the linearity range was from 0.2 to 950 μg/L, and the limits of detection were 0.05-0.2 μg/L. The relative standard deviation varied from 6.1 to 8.7% (C = 1 μg/L) and from 2.9 to 3.5% (C = 500 μg/L). The determination of phenols is complicated in eutrophic water and spring water with a high content of humic and fulvic acids.




Principle

Capillary Electrophoresis (CE) is physical method of analysis which performs in a separation channel of elastic quartz capillary, under the influence of a high voltage direct current field. Charged analytes dissolved in an electrolyte solution are separated based on differences in mobility and/or distribution behavior of components. The migration velocity of an analyte under an electric field is determined by the electrophoretic mobility of the analyte and the electro-osmotic mobility of the buffer inside the capillary. The electrophoretic mobility of a solute depends on the characteristics of the solute (electric charge, molecular size and shape) and those of the buffer in which the migration takes place (type and ionic strength of the electrolyte, pH, viscosity and additives). Capillary electrophoresis provides greater resolution, higher sensitivity and online detection. It enables single-cell analysis and even single-molecule analysis, optimizing separation and analysis of biological macromolecules.

Applications

Biomedical, clinical, pharmaceutical, forensic, industrial, and food analysis

Procedure

1. Preparation: Preheat the capillary electrophoresis apparatus and flush the capillary with no voltage applied. Prepare mixed standard samples and buffer solution.
2. Sample Application: Put the appropriate amount of mixed standard samples in the sample tube at the corresponding position at the inlet of the capillary electrophoresis apparatus, and put the appropriate amount of buffer in the sample tube at the corresponding position of the apparatus.
3. Electrophoresis: Switch on the electrophoresis apparatus and set the voltage and program. Initiate automatic sampling, electrophoresis, and analysis.
4. Determination: Record and analyze the migration of each component. Capillary electrophoresis apparatus can be connected with various detectors to detect the separation. The most widely used is the UV-visible spectrophotometric detector. After the experiment, flush the capillary again.

Materials

• Capillary electrophoresis apparatus
• Sample solution
• Buffer solution

Notes

1. When an electric field is applied through the capillary filled with buffer, a flow of solvent is generated inside the capillary, called electro-osmotic flow (EOF). The reproducibility of CE separation will be seriously affected by small changes in EOF. For some applications, it is important to control EOF by modifying the inner wall of the capillary or by changing the concentration, composition and/or pH of the buffer solution.
2. The definition and automation of the injection process are critical for precise quantitative analysis. Modes of injection include gravity, pressure or vacuum injection and electrokinetic injection.
3. The employed electrolytic solution should be filtered to remove particles and degassed to avoid bubble formation that could interfere with the detection system or interrupt the electrical contact in the capillary during the separation run.
4. A rigorous rinsing procedure should be developed to achieve reproducible migration times of the solutes.