Department of Analytical Chemistry, Research Centre for Agricultural and Food Biotechnology (BITAL), Almería University, Agrifood Campus of International Excellence, ceiA3, E-04071 Almería, Spain.
Talanta. 2012 Jan 30;89:201-8. doi: 10.1016/j.talanta.2011.11.082. Epub 2011 Dec 9.
A multiclass method has been optimized and validated for the simultaneous determination of 20 veterinary drug residues belonging to several classes, as quinolones, sulfonamides, macrolides, anthelmintics, avermectins and diamino derivatives, and benzathine, used as a marker of the presence of penicillin, in muscle chicken. It has been based on QuEChERS methodology (quick, easy, cheap, effective, rugged and safe) and ultra high performance liquid chromatography coupled to triple quadrupole tandem mass spectrometry (UHPLC-MS/MS). Several chromatographic conditions were optimized, obtaining a running time <8.5 min. The developed method was validated on the basis of international guidelines. Mean recoveries ranged from 70 to 120%, except for benzathine (65.6% at 20 μg kg(-1)) and sulfadimidine (69.0% at 100 μg kg(-1)). Repeatability was lower than 20.0% except for sulfachlorpyridazine (22.1% at 20 μg kg(-1)) and tylosin (20.5% and 20.6% at 30 and 50 μg kg(-1), respectively), whereas reproducibility was lower than 25% except for flumequine (27.4% at 20 μg kg(-1)) and benzathine (37.8% and 27% at 20 and 50 μg kg(-1), respectively). Limits of detection (LODs) and quantification (LOQs) ranged from 3.0 to 6.0 μg kg(-1) and 10.0 to 20.0 μg kg(-1), respectively, except for tylosin that showed a LOD and LOQ of 9.0 and 30.0 μg kg(-1). Decision limit (CC(α)) and detection capability (CC(β)) were calculated and CC(β) ranged from 24.1 μg kg(-1) (mebendazole) to 423.6 μg kg(-1) (flumequine). Finally, the method was applied to real samples and traces of some compounds were found in eight samples of chicken and benzathine was detected in one sample at 29.9 μg kg(-1).
一种多类方法已被优化和验证，用于同时测定 20 种属于喹诺酮类、磺胺类、大环内酯类、驱虫药、阿维菌素类和二氨基衍生物以及苯并噻嗪类的兽用药物残留，苯并噻嗪类用于作为青霉素存在的标记物，在肌肉鸡肉中。它基于 QuEChERS 方法（快速、简单、廉价、有效、坚固和安全）和超高效液相色谱与三重四极杆串联质谱联用（UHPLC-MS/MS）。优化了几种色谱条件，得到的运行时间<8.5 分钟。该方法是根据国际指南进行验证的。平均回收率在 70%至 120%之间，除了苯并噻嗪（20μgkg-1 时为 65.6%）和磺胺嘧啶（100μgkg-1 时为 69.0%）。重复性低于 20.0%，除了磺胺氯哒嗪（20μgkg-1 时为 22.1%）和泰乐菌素（30 和 50μgkg-1 时分别为 20.5%和 20.6%）外，再现性低于 25%，除了氟甲喹（20μgkg-1 时为 27.4%）和苯并噻嗪（20 和 50μgkg-1 时分别为 37.8%和 27.0%）外。检测限（LOD）和定量限（LOQ）范围为 3.0 至 6.0μgkg-1 和 10.0 至 20.0μgkg-1，除了泰乐菌素的 LOD 和 LOQ 分别为 9.0 和 30.0μgkg-1。决策限（CC(α)）和检测能力（CC(β)）进行了计算，CC(β)范围为 24.1μgkg-1（苯并咪唑）至 423.6μgkg-1（氟甲喹）。最后，该方法应用于实际样品，在 8 个鸡肉样品中发现了一些化合物的痕迹，并在一个样品中检测到了苯并噻嗪，含量为 29.9μgkg-1。
