4.4 Article

Development of Capillary Electrophoretic Method Combined with Accelerated Solvent Extraction for Simultaneous Determination of Residual Sulfonamides and Their Acetylated Metabolites in Aquatic Products

Journal

FOOD ANALYTICAL METHODS
Volume 6, Issue 4, Pages 1049-1055

Publisher

SPRINGER
DOI: 10.1007/s12161-012-9509-0

Keywords

Capillary electrophoresis; Accelerated solvent extraction; Sulfonamides; Acetylated metabolites; Aquatic products

Funding

  1. Natural Science Foundation of Hebei Province [B2008000583]
  2. sustentation Plan of Science and Technology of Hebei Province [10967126D]

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A rapid and effective method was developed in the first time for the determination of four sulfonamides (SAs) and their N-4-acetylated metabolites in aquatic products using capillary electrophoresis with accelerated solvent extraction (ASE). The eight residues were extracted with acetonitrile at 70 A degrees C under 10.3 MPa pressure and two static cycles with a static time of 5 min. The eight analytes can be baseline separated with 6 min. The standard curves for the determination of eight residues by the capillary electrophoretic method have good linearity (r (2) > 0.999). The method limits of quantification (LOQs) for N-4-acetylsulfadiazine, sulfadiazine, sulfamerazine, sulfamethoxazole, sulfamethazine, N-4-acetylsulfamethazine, N-4-acetylsulfamerazine, and N-4-acetylsulfamethoxazole in aquatic products were 26.4, 33.0, 33.0, 33.0, 39.6, 370, and 1,076 mu g kg(-1), respectively. Intra- and inter-day precision (RSD) were 0.4-2.2 % and 1.4-3.5 %, respectively. Their average recoveries with three spiked levels ranged from 83 % to 116 % with the RSDs less than 4 %. The proposed method provides a rapid and simple extraction procedure with high sensitivity and recoveries, and can permit routine detection of the studied SAs residues in aquatic products at the maximum residue level.

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