LC-MS/MS methods for sulfadimethoxine and ormetoprim analysis in feed and fish fillet and a leaching study for feed after alternative procedures for the incorporation of drugs

Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2017 Apr;34(4):501-508. doi: 10.1080/19440049.2016.1267875. Epub 2016 Dec 16.

Abstract

This paper describes the method development for sulfadimethoxine (SDM) and ormetoprim (OMP) quantitation in fish feed and fish fillet employing LC-MS/MS. In order to assess the reliability of the analytical method, valuation was undertaken as recommended by guidelines proposed by the Brazilian Ministry of Agriculture. The calibration curve for the quantification of both drugs in feed showed adequate linearity (r > 0.99), precision (CV < 12%) and trueness ranging from 97% to 100%. The method for the determination of SDM and OMP residues in fish fillet involved a simple sample preparation procedure that had adequate linearity (r > 0.99), precision (CV < 16%) and trueness around 100%, with CCα < 100.2 ng g-1 and CCβ < 100.4 ng g-1. With a goal of avoiding the risk of drug leaching from feed into the aquatic environment during fish medication via the oral route, different procedures for drug incorporation into feed were evaluated. Coating feed pellets with ethyl cellulose polymer containing the drug showed promising results. In this case, medicated feed released drugs to water at a level below 6% when the medicated feed stayed in the water for up to 15 min.

Keywords: Food contaminants; LC-MS/MS; antimicrobial drugs; aquaculture; ormetoprim; sulfadimethoxine; veterinary drug residues.

MeSH terms

  • Animal Feed / analysis*
  • Animals
  • Anti-Infective Agents / administration & dosage
  • Anti-Infective Agents / analysis*
  • Anti-Infective Agents / metabolism
  • Biotransformation
  • Brazil
  • Cellulose / analogs & derivatives
  • Cellulose / chemistry
  • Characiformes
  • Chromatography, Liquid
  • Coated Materials, Biocompatible / chemistry
  • Drug Liberation
  • Drug Residues / analysis*
  • Drug Residues / metabolism
  • Guidelines as Topic
  • Humans
  • Kinetics
  • Limit of Detection
  • Liquid-Liquid Extraction / methods
  • Meat / analysis*
  • Pyrimidines / administration & dosage
  • Pyrimidines / analysis*
  • Pyrimidines / metabolism
  • Sulfadimethoxine / administration & dosage
  • Sulfadimethoxine / analysis*
  • Sulfadimethoxine / metabolism
  • Tandem Mass Spectrometry

Substances

  • Anti-Infective Agents
  • Coated Materials, Biocompatible
  • Pyrimidines
  • Sulfadimethoxine
  • ethyl cellulose
  • Cellulose
  • ormetoprim