Determination of five macrolide antibiotic residues in milk by micellar electrokinetic capillary chromatography with field amplified sample stacking

Abstract

The aim of this study is to develop a new micellar electrokinetic capillary chromatography with field amplified sample stacking for the determination of five kinds of macrolide antibiotic residues in milk. The main factors that affect the separation and enrichment of these analytes were optimized. The optimum running buffer was composed of 60 mM phosphate, 5 mM sodium cholate, and 1.0 mM cetyltrimethyl ammonium bromide at pH 7.0. The separation voltage was 20 kV and the sample was electrokinetically injected at 10 kV for 120 s. The detection wavelength was set at 195 nm. Under the optimized conditions, the enrichment factor of tilmicosin, erythromycin, clarithromycin, roxithromycin, and tylosin were 866, 565, 908, 702, and 675, respectively. The limits of detection ranged from 0.002 to 0.004 mg/kg. The method shall meet the requirement of their maximum residue limits ruled by China, the European Union, the United States, and other countries. Practical applications The developed method has been applied successfully to the determination of the milk samples spiked at 0.05 and 0.1 mg/kg. The recoveries ranging from 72.8 to 93.7% demonstrate that the method can be applied to the detection of tilmicosin, erythromycin, clarithromycin, roxithromycin, and tylosin residues in milk.

Advances in the Analysis of Veterinary Drug Residues in Food Matrices by Capillary Electrophoresis Techniques

“…However, off-line or on-line pre-concentration steps were the ideal approach to overcome the derivatization step required to obtain a high sensitivity by CE. Among the on-line pre-concentration techniques, FASS represented a promising solution, as demonstrated in the analysis of TIL, erythromycin, clarithromycin, roxithromycin, and tylosin residues in milk samples by a FASS-MEKC-UV method (LOD range of 0.002-0.004 mg/kg) [83]. CZE-DAD was recently proposed to analyze macrolides (TYL and TIL) in chicken fat samples, reaching LOQ values of a few µg/kg thanks to a preconcentration step that consisted of an evolution of the DLLME procedure: In fact, the extraction and the preconcentration occurred in an ionic liquid by using ultrasound instead of dispersive solvents (this procedure is named reverse ultrasound-assisted emulsification-microextraction, R-USAEME).…”

Recent progress of sample stacking in capillary electrophoresis (2016–2018)

“…Hong et al. developed an FASS‐MEKC method for the analysis of five macrolide antibiotic residues (tilmicosin, erythromycin, clarithromycin, roxithromycin and tylosinin) in milk. The BGE was composed of 60 mM phosphate, 5 mM sodium cholate and 1.0 mM CTAB at pH 7.0.…”

Recent advances in enhancing the sensitivity of electrophoresis and electrochromatography in capillaries and microchips (2016–2018)

“…FASS and FASI are usually the first choice among all stacking techniques due to their simplicity and high compatibility with different CE modes such as CZE , EKC , CGE , CEC as well as microchip electrophoresis . An uncomplicated buffer system used in FASS and FASI allows to utilize a whole range of detectors including UV , LED‐IF , LIF , C4D , and amperometric .…”

“…FASS and FASI are usually the first choice among all stacking techniques due to their simplicity and high compatibility with different CE modes such as CZE , EKC , CGE , CEC as well as microchip electrophoresis . An uncomplicated buffer system used in FASS and FASI allows to utilize a whole range of detectors including UV , LED‐IF , LIF , C4D , and amperometric . The sample matrix effect is reduced or eliminated since the sample clean‐up is necessary to lower the conductivity of the sample and thus, FASS and FASI can be used in analysis of biological , pharmaceutical , environmental , food , industrial , and forensic samples .…”

“…An uncomplicated buffer system used in FASS and FASI allows to utilize a whole range of detectors including UV , LED‐IF , LIF , C4D , and amperometric . The sample matrix effect is reduced or eliminated since the sample clean‐up is necessary to lower the conductivity of the sample and thus, FASS and FASI can be used in analysis of biological , pharmaceutical , environmental , food , industrial , and forensic samples . In addition, combination of FASS and FASI with other stacking techniques is popularly used in multi‐stacking approaches which will be discussed further in this review.…”