Ministério da Agricultura, Pecuária e Abastecimento, Laboratório Nacional Agropecuário, Seção Laboratorial Avançada de São José (SLAV/SC/LANAGRO/RS), São José, SC 88102-600, Brazil; Instituto Catarinense de Sanidade Agropecuária (ICASA), Florianópolis, SC 88034-000, Brazil.
Universidade Federal de Santa Catarina (UFSC), Centro de Ciências Físicas e Matemáticas, Departamento de Química, Florianópolis, SC 88040-900, Brazil.
J Chromatogr A. 2018 Sep 28;1569:110-117. doi: 10.1016/j.chroma.2018.07.048. Epub 2018 Jul 17.
A method for the simultaneous analysis of veterinary drug residues (spectinomycin, halquinol, and zilpaterol) and contaminants (melamine) in feedingstuffs by liquid chromatography-tandem mass spectrometry was developed. Method performance for all analytes was evaluated by reversed-phase liquid chromatography, reversed-phase with altered chemical equilibrium, and hydrophilic interaction (HILIC) as chromatographic modes. Validation was in accordance to Commission Decision 657/2002/CE, by considering the best chromatographic approach. Ion-pair liquid chromatography with C as stationary phase led to the lowest random uncertainties, effective analyte separation and shorter time of analysis. Low precision deviations and good recovery rates were obtained and thus method reliability and sensitivity could be consolidated. Method applicability was evaluated by the analysis of samples of feedingstuffs, such as cattle, pig, and poultry feeds, feed ingredients of both animal and vegetable origins, and mineral feeds. Some samples showed quantifiable concentrations of halquinol and zilpaterol, reinforcing the importance of this new analytical control method.
建立了一种同时分析饲料中兽药残留（壮观霉素、卤羟喹和齐帕特罗）和污染物（三聚氰胺）的液相色谱-串联质谱法。通过反相液相色谱、反相改变化学平衡和亲水相互作用（HILIC）作为色谱模式评估所有分析物的方法性能。验证符合委员会第 657/2002/CE 号决定，通过考虑最佳色谱方法进行验证。使用 C 作为固定相的离子对液相色谱导致最低的随机不确定度、有效的分析物分离和更短的分析时间。获得了低的精密度偏差和良好的回收率，从而可以巩固方法的可靠性和灵敏度。通过分析牛、猪和家禽饲料等饲料样品、动物和植物来源的饲料成分以及矿物质饲料，评估了方法的适用性。一些样品显示出可量化的卤羟喹和齐帕特罗浓度，这强调了这种新的分析控制方法的重要性。
