Liquid Chromatography-Mass Spectrometry Determination of Six 5-Nitroimidazoles in Animal Feedstuff |
| |
Authors: | L F Capitan-Vallvey A Ariza R Checa N Navas |
| |
Institution: | (1) Department of Analytical Chemistry, University of Granada, C/ Fuentenueva s/n, 18071 Granada, Spain;(2) Laboratorio Central de Veterinaria de Santa Fe, Ministerio de Agricultura Pesca y Alimentación, Camino del Jau s/n, Santa Fe, 18320 Granada, Spain |
| |
Abstract: | A liquid chromatography-mass spectrometry method for the determination of the coccidiostats metronidazole, ronidazole, dimetridazole,
secnidazole, tinidazole and ipronidazole in feedstuff was developed. The 5-nitroimidazoles were extracted from animal feed
with a pH 2 phosphate buffer solution followed by a solid phase extraction procedure based on HLB cartridges. The liquid chromatographic
separation of the extracts was performed on a C18 bonded silica column applying a gradient of elution with pH 4.3 ammonium acetate buffer solution and acetonitrile. Quantification
for each 5-nitroimidazole was carried out monitoring its molecular ion M + H]+ obtained by positive electrospray ionisation mode. A pool of feedstuffs was used to optimise and validate the method. Linearity,
quantification limit, intra-day and inter-day reproducibility and accuracy were estimated using this pool of feedstuffs spiked
with the drugs. For the confirmatory assay, several fragment ions from each 5-nitroimidazole were obtained and monitored.
The method was applied successfully to determine 5-nitroimidazoles in feedstuff at level of 0.05 mg kg−1. |
| |
Keywords: | Colomn liquid dromatography-mass chromatography Feed analysis 5-Nitroimidazoles |
本文献已被 SpringerLink 等数据库收录! |
|