Validation of a confirmatory method for the determination of melamine in egg by gas chromatography-mass spectrometry and ultra-performance liquid chromatography-tandem mass spectrometry

Anal Chim Acta. 2009 Oct 5;651(2):196-200. doi: 10.1016/j.aca.2009.08.025. Epub 2009 Aug 25.

Abstract

A sensitive and reliable method was developed and validated for detection and confirmation of melamine in egg based on gas chromatography-mass spectrometry (GC-MS) and ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Trichloroacetic acid solution was used for sample extraction and precipitation of proteins. The aqueous extracts were subjected to solid-phase extraction by mixed-mode reversed-phase/strong cation-exchange cartridges. Using ultra-performance liquid chromatography and electrospray ionization in the positive ion mode, melamine was determined by LC-MS/MS, which was completed in 5 min for each injection. For the GC-MS analysis, extracted melamine was derivatized with N,O-bis(trimethylsilyl)trifluoracetamide prior to selected ion monitoring detection in electron impact mode. The average recovery of melamine from fortified samples ranged from 85.2% to 103.2%, with coefficients of variation lower than 12%. The limit of detection obtained by GC-MS and UPLC-MS/MS was 10 and 5 microg kg(-1), respectively. This validated method was successfully applied to the determination of melamine in real samples from market.

Publication types

  • Research Support, Non-U.S. Gov't
  • Validation Study

MeSH terms

  • Chromatography, High Pressure Liquid / methods*
  • Eggs / analysis*
  • Gas Chromatography-Mass Spectrometry / methods*
  • Solid Phase Extraction
  • Tandem Mass Spectrometry / methods*
  • Triazines / analysis*
  • Trichloroacetic Acid / chemistry

Substances

  • Triazines
  • Trichloroacetic Acid
  • melamine