Analysis of sub g/kg lincomycin in honey, muscle, milk, and eggs using fast liquid chromatography-tandem mass spectrometry

Ádám Tölgyesi, Jenõ Fekete, Szabolcs Fekete, Virender K. Sharma, Katalin Békési, Edina Tóth

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Abstract

A fast liquid chromatographytandem mass spectrometry (LCMSMS) method is developed to determine lincomycin (LM) in honey, muscle, milk, and egg. Samples are cleaned-up at pH 4.7 using Strata-X-C mixed-mode polymeric strong cation exchange solid-phase extraction (SPE) cartridges, which could selectively adsorb the lincomycin from matrices under the acidic condition. LM is separated on the recently introduced Kinetex XB core-shell type HPLC column using isocratic elution mode with a mobile phase containing 0.1 formic acid in water/acetonitrile (93/7, v/v, pH 2.6) at a flow rate of 0.7 mL/min. The subsequent MS/MS detection has decreased ion effect, which allows the limit of detection (LOD) of LM for honey to be 0.05 g/kg for honey and 0.5 g/kg for muscle, milk, and egg. These LODs are much lower than those reported previously. The other main advantage of the developed method is the analysis time of only 3.5 min, which is about three times shorter than other reported LCMSMS methods. Recoveries varies between 94.2 and 125.2 and in-house reproducibility ranges from 3.7 to 28.7. The developed method is validated according to European Union (EU) Commission Decision 2002/657/EC using a matrix-comprehensive validation strategy. All studied analytical parameters fulfills the EU guidelines.

Original languageEnglish
Pages (from-to)190-198
Number of pages9
JournalJournal of chromatographic science
Volume50
Issue number3
DOIs
Publication statusPublished - Mar 1 2012

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ASJC Scopus subject areas

  • Analytical Chemistry

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