Multiresidue method for simultaneous analysis of aflatoxin M1, avermectins, organophosphate pesticides and milbemycin in milk by ultra-performance liquid chromatography coupled to tandem mass spectrometry

Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2016 Jun;33(6):995-1002. doi: 10.1080/19440049.2016.1175227. Epub 2016 May 24.

Abstract

A method developed for the simultaneous analysis of aflatoxin M1, abamectin, doramectin, eprinomectin, ivermectin, moxidectin, acephate, azinphos-ethyl, azinphos-methyl, diazinon, methamidophos, methidathion, mevinphos, pirimiphos-ethyl and pirimiphos-methyl in whole raw milk, based on the QuEChERS method for extraction and clean-up, with detection and quantification by ultra-performance liquid chromatography coupled to tandem mass spectrometry (UPLC-MS/MS) is described. The method was validated according to parameters of the Analytical Quality Assurance Manual from the Brazilian Ministry of Agriculture and Commission Decision 2002/657/EC, and proved suitable for analysis of these analytes within the proposed working range, with recovery values between 77% and 110%, a standard deviation lower than 20%, limits of detection between 0.05 and 0.99 µg l(-)(1), and limits of quantification between 0.15 and 1.98 µg l(-1). Samples from animals treated with abamectin, doramectin, ivermectin and diazinon were analysed by the validated method. Residues of aflatoxin M1 were also found in field samples at levels below the established maximum residue limit.

Keywords: QuEChERS; UPLC-MS/MS; aflatoxin M1; macrocyclic lactones; milk; organophosphate pesticides.

MeSH terms

  • Aflatoxin M1 / analysis*
  • Animals
  • Brazil
  • Chromatography, High Pressure Liquid / methods*
  • Food Contamination / analysis
  • Ivermectin / analogs & derivatives
  • Ivermectin / analysis
  • Macrolides / analysis
  • Milk / chemistry*
  • Organophosphates / analysis
  • Pesticide Residues / analysis*
  • Reproducibility of Results
  • Tandem Mass Spectrometry

Substances

  • Macrolides
  • Organophosphates
  • Pesticide Residues
  • Aflatoxin M1
  • Ivermectin
  • avermectin
  • moxidectin