Determination of quinolones in bovine kidney using hollow-fiber supported liquid membrane extraction prior to liquid chromatography tandem mass spectrometry

• Main Author: Gaolape, Kefilwe Precious
• Other Authors: Dube, S.
• Format: Others
• Language: en
• Published: 2018
• Subjects: 543.65; Quinolone antibacterial agents; Liquid membranes; Liquid chromatography; Tandem mass spectrometry; Cattle > Health
• Online Access: Gaolape, Kefilwe Precious (2017) Determination of quinolones in bovine kidney using hollow-fiber supported liquid membrane extraction prior to liquid chromatography tandem mass spectrometry, University of South Africa, Pretoria, <http://hdl.handle.net/10500/24958>; http://hdl.handle.net/10500/24958

Focus of this study was on the development of one of the faster, simpler, cost effective and environmentally friendly sample pre-treatment techniques which employs a supported liquid membrane, in this case a Hollow-fiber supported liquid membrane (HF-SLM) for determination of seven (7) quinolone antibiotics (enrofloxacin, ciprofloxacin, danofloxacin, difloxacin, norfloxacin, nalidixic acid and sarafloxacin) in bovine kidney samples followed by LC-MS/MS analysis. The key parameters of the method were optimized and the method was validated following the 2002/657 EC guidelines. The optimum HF-SLM conditions were therefore; NaH2PO4 as a donor phase at pH 7, 0.1% formic acid at pH 3 as acceptor phase. Triethylamine was the optimized liquid membrane and the stirring time was optimized at 1 hour. Separation of the 7 quinolones including 3 internal standards (enrofloxacin-d5, norfloxacin-d5 and difloxacin-d3) was carried out on a Phenomenex Kinetex 2.6 μm XB-C18, 100 mm x 4.6 mm, 100Å column. Validation parameters such as Correlation coefficients (r2) ranging from 0.9714-0.9975 were obtained, while limit of detection (LOD) ranged between 3-39 ug kg-1 and limit of quantification (LOQ) ranged between 10-130 ug kg-1. The obtained limits at which it can be concluded with an error probability of α = 95% that a sample is non-compliant (CCα) ranged from 28 – 422 ug kg-1 while CCβ; the smallest content of the substance that may be detected, identified or quantified in a sample with an error probability of β = 95%, ranged from 29 – 454 ug kg-1. The method was found to be reproducible with CVs ≤ 23 %. The tested samples from Botswana local abattoirs showed no presence of quinolone antibiotics when the method was applied to real bovine kidney samples. Hollow-fiber supported liquid membrane can therefore be used for extraction of biological samples since it is a “greener technique” which uses less solvent which are less harmful to the environment when disposed as compared to dispersive Solid Phase Extraction (dSPE). === Chemistry === M. Sc. (Chemistry)