Enantioseparation and determination of flumequine enantiomers in multiple food matrices with chiral liquid chromatography coupled with tandem mass spectrometry

Abstract

The present work firstly described the enantioseparation and determination of flumequine enantiomers in milk, yogurt, chicken, beef, egg, and honey samples by chiral liquid chromatography‐tandem mass spectrometry. The enantioseparation was performed under reversed‐phase conditions on a Chiralpak IC column at 20°C. The effects of chiral stationary phase, mobile phase components, and column temperature on the separation of flumequine enantiomers have been studied in detail. Target compounds were extracted from six different matrices with individual extraction procedure followed by cleanup using Cleanert C18 solid phase extraction cartridge. Good linearity (R2>0.9913) was obtained over the concentration range of 0.125 to 12.5 ng g‐1 for each enantiomer in matrix‐matched standard calibration curves. The limits of detection and limits of quantification of two flumequine enantiomers were 0.015‐0.024 and 0.045‐0.063 ng g‐1, respectively. The average recoveries of the targeted compounds varied from 82.3 to 110.5%, with relative standard deviation less than 11.7%. The method was successfully applied to the determination of flumequine enantiomers in multiple food matrices, providing a reliable method for evaluating the potential risk in animal productions.

Sensitive immunoenzyme assay for the detection of antibiotic flumequine in honey

“…One of the traditional methods for assessing the contamination of honey with antibiotics, including FLU, is highperformance liquid chromatography (HPLC) in combination with various detection methods, mainly LC-MS/MS. [18][19][20][21] These techniques are characterized by high sensitivity, selectivity, and accuracy, but they are time-consuming and require sophisticated equipment and the involvement of qualied personnel. Therefore, there is a lack of methods suitable for quick screening of a large number of samples for the presence of antibiotics.…”

Development and validation of a chiral LC‐MS method for the enantiomeric resolution of (+) and (−)‐medetomidine in equine plasma by using polysaccharide‐based chiral stationary phases

“…A significant number of research works have been published related to the chiral resolution of racemates on a large scale using kinetic resolution by crystallization and enzymatic resolution methods [26][27][28][29] . Liquid chromatography (LC) evolved as a key technique for chiral separations due to the availability of large number of chiral stationary phases and lesser time to establish a method [30][31][32][33][34][35][36][37][38][39] . Despite the recent advances in the development of chiral stationary phases, the enantiomeric analysis of underivatized medetomidine has invited only very little attention.…”