Automated Online Solid-Phase Extraction Coupled with Sequential Injection-HPLC-EC System for the Determination of Sulfonamides in Shrimp

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.

On-Line Sample Pre-Treatment Procedures Applied to LC–MS

“…Several methods have been developed for the analysis of this class of antibiotics in a variety of food categories including honey, 112 shrimp, 113 eggs 114 and pork. 114 One such example is the analysis of sulphonamides in Chantarateepra, 113 which used electrochemical detection to great success for the analysis of seven sulfonamides (sulfaguanidine, sulfadiazine, sulfamethazine, sulfamonomethoxine, sulfamethoxazole, sulfadimethoxine and sulfaquinoxaline), although the lack of chromatographic resolution meant that sulfaguanidine and sulfadiazine could not be analysed uniquely. The quoted LODs ranged from 1-11 ng/mL.…”

Synthesis of New Azo Compound and its Application for Spectrophotometric Determination of Sulfamethoxazole and Extraction using Cloud Point Extraction

“…1 It is usually used for many infection treatment such as middle ear infections, acute urinary tract infections, eye infections, diarrhea, and bronchitis and as prophylaxis of rheumatic fever. [2][3][4][5] Several techniques are utilized for determination of sulfamethoxazole (SMZ) such as, High-performance liquid chromatography (HPLC), [3][4][5] highperformance thin layer chromatography (HPTLC), 6 solid phase extraction (SPE), 7 flow injection, 8-10 micellar electrokinetic RESEARCH ARTICLE capillary chromatography (MEKC), 11 GC, 12 voltammetry 13 and spectrophotometric methods. [14][15][16][17] Cloud point extraction has grown in popularity in comparison to other extraction techniques due to the advantages of low organic solvent consumption, fast recovery, low cost, high enrichment factor, and rapid phase separation.It is appealing because it reduces the employing and exposures to the solvent, as well as the time and costs of extraction and removal that have been used for pre-concentration of sulfomethoxazole after the formation of an azo compound that is poorly H 2 O-soluble.…”