Abstract

The use of fully automated online solid-phase extraction (SPE) coupled with sequential injection analysis, high-performance liquid chromatography (HPLC), and electrochemical detection (EC) for the separation and determination of sulfonamides has been developed. A homemade microcolumn SPE system coupled with sequential injection analysis (SIA) was used to automate the sample cleanup and extraction of sulfonamides. The optimal flow rate of sample loading and elution was found to be 10 μL/s, and optimal elution time of zone was 20–24 s. Under the optimal conditions, a linear relationship between peak area and sulfonamide concentrations was obtained in the range of 0.01–8.0 μg mL−1. Detection limits for seven sulfonamides were between 1.2 ng mL−1and 11.2 ng mL−1. The proposed method has been applied for the determination of sulfonamides in shrimp. Recoveries in the range of 84–107% and relative standard deviations (RSDs) below 6.5% for intraday and 13% for inter-day were received for three concentration levels of spiking. The results showed that the present method was simple, rapid, accurate and highly sensitive for the determination of sulfonamides.

Highlights

  • Sulfonamides (SAs) have been widely used as effective chemotherapeutics and growth promoters in animals’ feeding

  • From our previous report [28], methanol was selected as the most suitable eluent for offline solid-phase extraction (SPE) to achieve the complete extraction of sulfonamides (SAs) in shrimp and the mixture of phosphate buffer : acetonitrile : ethanol (80 : 15 : 5; v/v/v) was used as a mobile phase to obtain the high separation efficiency

  • An eluent of 100% methanol was selected as the best eluent for the experiment because this condition led to the complete elution of SAs from SPE column, good separation of seven SAs following their high-performance liquid chromatography (HPLC), and highest electrochemical signals

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Summary

Introduction

Sulfonamides (SAs) have been widely used as effective chemotherapeutics and growth promoters in animals’ feeding. Offline SPE using Oasis HLB material was successfully proposed and applied to extract the residual sulfonamides in shrimp [28]. This material is a hydrophilic-lipophilic balanced (HLB) sorbent that is composed of two monomers (N-vinylpyrrolidone and divinylbenzene). A detailed evaluation of the methodology was developed to demonstrate that this method can be satisfactorily applied to determine residual concentrations of the seven sulfonamides in shrimp using the Oasis HLB SPE material for sample extraction

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