Analysis of eight free progestogens in eggs by matrix solid-phase dispersion extraction and very high pressure liquid chromatography with tandem mass spectrometry

J Chromatogr B Analyt Technol Biomed Life Sci. 2008 Jul 15;870(2):241-6. doi: 10.1016/j.jchromb.2008.06.021. Epub 2008 Jun 20.

Abstract

A rapid method to identify and quantify unconjugated progestogens in eggs is presented. Samples were prepared based on matrix solid-phase dispersion (MSPD) using C18 as dispersant, followed by a clean-up step with graphitized carbon black (GCB) solid-phase extraction (SPE) cartridges. The analytes were separated by very high pressure LC on a BEH C18 column for a period of 5 min. Electrospray ionization tandem mass spectrometry (ESI-MS/MS) was operated in the positive time-scheduled multi-reaction monitoring mode. Recovery studies were performed at two fortification levels. Average recoveries of the target compounds varied from 83.8% to 111.2% and relative standard deviations ranged from 10.5% to 23.7%. The limits of detection (LODs) and limits of quantitation (LOQs) were in the range of 0.2-2.0 microg kg(-1) and 0.6-5.0 microg kg(-1), respectively. Investigation of real samples indicated that the range of progesterone in eggs was 9.9-40.0 microg kg(-1).

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Animals
  • Chromatography, High Pressure Liquid / methods*
  • Eggs / analysis*
  • Progestins / analysis*
  • Solid Phase Extraction / methods*
  • Tandem Mass Spectrometry / methods*

Substances

  • Progestins