Electrochemically controlled in-tube solid phase microextraction of naproxen from urine samples using an experimental...

Area of Science:

• Analytical Chemistry
• Separation Science
• Electrochemistry

Background:

• Solid phase microextraction (SPME) is a widely used technique for sample preparation.
• Traditional SPME methods can be time-consuming and may lack sufficient sensitivity for certain analytes.
• Combining electrochemistry with in-tube SPME offers potential for improved performance.

Purpose of the Study:

• To develop and validate a new electrochemically controlled in-tube SPME (EC in-tube SPME) method.
• To enhance the sensitivity and reduce the analysis time for naproxen detection.
• To apply the developed method for the analysis of naproxen in urine samples.

Main Methods:

• Electropolymerization of pyrrole on a stainless steel tube to create a polypyrrole (PPy)-coated in-tube SPME device.
• On-line coupling of the PPy-coated in-tube SPME with high-performance liquid chromatography (HPLC) for automated analysis.
• Application of constant potential during the extraction step to enhance efficiency.
• Optimization of extraction parameters using Plackett-Burman and Box-Behnken designs.

Main Results:

• The EC in-tube SPME-HPLC method significantly increased extraction efficiency for naproxen.
• The optimized method achieved a linear range of 0.5-1000 μg L⁻¹ and a detection limit of 0.07 μg L⁻¹.
• The method demonstrated successful application in the analysis of naproxen in real urine samples.

Conclusions:

• EC in-tube SPME is a sensitive and efficient technique for sample preparation.
• The developed automated EC in-tube SPME-HPLC system offers reduced analysis time and enhanced sensitivity.
• This method provides a viable analytical tool for the determination of pharmaceuticals in biological fluids.