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Simultaneous analysis of spectinomycin, halquinol, zilpaterol, and melamine in feedingstuffs by ion-pair liquid chromatography–tandem mass spectrometry
Journal of Chromatography A ( IF 3.8 ) Pub Date : 2018-07-17 , DOI: 10.1016/j.chroma.2018.07.048
Luciano Molognoni , Naielly Coelho de Souza , Leandro Antunes de Sá Ploêncio , Gustavo Amadeu Micke , Heitor Daguer

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 C18 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.



中文翻译:

离子对液相色谱-串联质谱法同时分析饲料中大观霉素,氟喹诺尔,齐帕特罗和三聚氰胺

建立了一种通过液相色谱-串联质谱法同时分析饲料中兽药残留物(大观霉素,氟喹诺尔和齐帕特罗)和污染物(三聚氰胺)的方法。通过反相液相色谱,化学平衡改变的反相和亲水相互作用(HILIC)作为色谱模式,评估了所有分析物的方法性能。通过考虑最佳色谱方法,按照委员会决定657/2002 / CE进行验证。C 18离子对液相色谱因为固定相导致最低的随机不确定性,有效的分析物分离和更短的分析时间。获得了较低的精度偏差和良好的回收率,因此可以巩固方法的可靠性和灵敏度。方法的适用性通过分析饲料样品(例如牛,猪和家禽饲料,动植物来源的饲料成分以及矿物质饲料)进行评估。一些样品显示出可测定的氟喹诺尔和齐帕特罗浓度,从而增强了这种新的分析控制方法的重要性。

更新日期:2018-07-17
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