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

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

Journal of chromatographic science (2012-02-18)
Adám Tölgyesi, Jenõ Fekete, Szabolcs Fekete, Virender K Sharma, Katalin Békési, Edina Tóth
ABSTRACT

A fast liquid chromatography-tandem mass spectrometry (LC-MS-MS) 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 µg/kg for honey and 0.5 µg/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 LC-MS-MS 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.

MATERIALS
Product Number
Brand
Product Description

Supelco
Lincomycin hydrochloride monohydrate, VETRANAL®, analytical standard
Sigma-Aldrich
Lincomycin hydrochloride, BioReagent, suitable for cell culture
Sigma-Aldrich
Lincomycin hydrochloride, ≥90% (TLC)
Sigma-Aldrich
Lincomycin hydrochloride, 96.0-102.0% (HPLC)
Lincomycin hydrochloride, European Pharmacopoeia (EP) Reference Standard