title: Rapid separation and highly sensitive detection methodology for sulfonamides in shrimp using a monolithic column coupled with BDD amperometric detection.
abstract: In this report, we aimed to extend our previous efforts toward the evaluation of sulfonamides (SAs) with a boron-doped diamond (BDD) electrode. We improved this method by reducing the analysis time using a monolithic column coupled with amperometric detection to determine seven sulfonamides (sulfaguanidine, sulfadiazine, sulfamethazine, sulfamonomethoxine, sulfamethoxazole, sulfadimethoxine and sulfaquinoxaline). Because of its rapid separation, low back-pressure and high separation efficiency compared to a particle-packed column, a monolithic column (100 mm x 4.6mm) was used for sulfonamide separation. Chromatographic separation was performed in less than 8 min. The analysis was carried out using phosphate buffer (0.1M, pH 3): acetonitrile: methanol in a ratio of 80:15:5 (v/v/v) as the mobile phase with a flow rate of 1.5 mL min(-1). The optimal detection potential using hydrodynamic voltammetry was found to be 1.2V versus Ag/AgCl. The method was applied to determine seven sulfonamides in shrimp after sample preparation by solid-phase extraction. The recoveries of the sulfonamides in spiked shrimp samples at 1.5, 5 and 10 microg g(-1) were in the range of 81.7 to 97.5% with a relative standard deviation (R.S.D.) between 1.0 and 4.6%. Our methodology produced results that were highly correlated with HPLC-MS data. Therefore, we propose a method that can be used for the rapid, selective and sensitive evaluation of sulfonamides in contaminated food.
authors.affiliation: Department of Chemistry, Faculty of Science, Chulalongkorn University, Patumwan, Bangkok 10330, Thailand.
authors.forename: Haruthai
authors.initials: H
authors.lastname: Sangjarusvichai
authors.forename: Wijitar
authors.initials: W
authors.lastname: Dungchai
authors.forename: Weena
authors.initials: W
authors.lastname: Siangproh
authors.forename: Orawon
authors.initials: O
authors.lastname: Chailapakul
mesh_terms: D000818:Animals; D001895:Boron / Q000737:chemistry*; D002851:Chromatography, High Pressure Liquid; D018130:Diamond / Q000737:chemistry*; D004563:Electrochemistry; D004566:Electrodes; D005504:Food Analysis / Q000379:methods*; D005506:Food Contamination / Q000032:analysis*; D006863:Hydrogen-Ion Concentration; D013058:Mass Spectrometry; D033561:Penaeidae / Q000737:chemistry*; D015203:Reproducibility of Results; D012758:Shellfish / Q000032:analysis*; D052616:Solid Phase Extraction; D013449:Sulfonamides / Q000032:analysis* / Q000737:chemistry / Q000302:isolation & purification; D013997:Time Factors
chemical_list: D013449:Sulfonamides; D018130:Diamond; D001895:Boron