Analysis of Sub  g/kg Lincomycin in Honey, Muscle, Milk, and Eggs Using Fast Liquid Chromatography-Tandem Mass Spectrometry

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.

Quantification of T-2 and HT-2 mycotoxins in cereals by liquid chromatography-multimode ionization-tandem mass spectrometry

“…ME (%) = [(slope of matrix-matched curve)/(slope of matrix-free curve) − 1] × 100. After the optimized clean-up the co-eluted matrices resulted in 37.7% ion suppression for T-2, which value is acceptable when complex matrices are analyzed [27,28]. However, the matrix effect for HT-2 could be minimized (0.2% ion suppression) using this approach.…”

“…Generally, the advantages of core-shell type column compared to fully porous ones lie in their better resolution and sensitivity caused by the increased mass transfer, reduced longitudinal diffusion and more favorable eddy dispersion [31]. Kinetex XB column has been successfully applied for the separation of basic molecules (lincomycin, nitroimidazoles, sulfonamides, trimethoprim) in food and feed matrices [27,29]. In this study we tested this column for T-2 and HT-2 that do not contain acidic or basic functional groups (Fig.…”

“…This ion source contains both ESI and APCI parts, and therefore, its geometry radically differs to adequate ones [23]. Significantly, LC-MMI-MS/MS methods require thorough optimizations to reach good sensitivity for target compounds and to detect such low levels set by EU [24,[26][27][28][29][30].…”

Core-Shell Columns in High-Performance Liquid Chromatography: Food Analysis Applications

“…There are many recent methods developed in this direction. Tolgyesi et al, 2012 [ 61 ], demonstrated that the use of a C18 core-shell particle column in the detection of lincomycin in honey, muscle, milk, and eggs by LC-MS-MS resulted in an analysis time and in LODs at least three times lower than the previous methods.…”

Simultaneous determination of eight corticosteroids in bovine tissues using liquid chromatography–tandem mass spectrometry

“…Recently, we have demonstrated that the pH is one main parameter to reduce the matrix compounds during the sample cleanup [10,13,29,30]. The corticosteroids are non-polar and neutral molecules, however, matrix compounds generally can be ionized in the sample extracts depending on pH, therefore mixed-mode ion exchange SPE cartridges can be chosen for sample cleanup and concentration.…”