Department of Chemistry and Physics (Analytical Chemistry Area), Research Centre for Agricultural and Food Biotechnology (BITAL), University of Almería, Agrifood Campus of International Excellence, Almería, Spain.
Anal Bioanal Chem. 2013 Aug;405(20):6543-53. doi: 10.1007/s00216-013-7060-5. Epub 2013 May 28.
A fast and generic method has been developed for the simultaneous monitoring of >250 pesticides and veterinary drugs (VDs) in animal feed. A 'dilute-and-shoot' extraction with water and acetonitrile (1% formic acid) followed by a clean-up step with Florisil cartridges was applied. The extracts were analysed by ultra-high performance liquid chromatography coupled to hybrid analyser quadrupole-time-of-flight mass spectrometry using both positive and negative electrospray ionisation. The detection of the residues was accomplished by retention time and accurate mass using an in-house database. The identification of the detected compounds was carried out by searching of fragment ions for each compound and isotopic pattern. The optimised method was validated and recoveries ranged from 60% to 120% at three concentrations (10, 50 and 100 μg kg(-1)) for 30%, 68% and 80% of compounds, respectively, included in the database (364) in chicken feed. Document SANCO 12495/2011 and Directive 2002/657/CE were used as guidelines for method validation. Intra-day and inter-day precisions, expressed as relative standard deviations, were lower than 20% for more than 90% of compounds. The limits of quantification ranged from 4 to 200 μg kg(-1) for most analytes, which are sufficient to verify compliance of products with legal tolerances. The applicability of the procedure was further tested on different types of feed (chicken, hen, rabbit and horse feed), evaluating recoveries and repeatability. Finally, the method was applied to the analysis of 18 feed samples, detecting some VDs (sulfadiazine, trimethoprim, robenidin and monensin Na) and only one pesticide (chlorpyrifos).
已经开发出一种快速且通用的方法，用于同时监测动物饲料中的>250 种农药和兽药 (VDs)。采用水和乙腈（1%甲酸）的“稀释后直接进样”提取方法，然后用 Florisil 小柱进行净化。采用超高效液相色谱-混合分析四极杆飞行时间质谱联用仪，正、负离子喷雾电离模式下对提取物进行分析。通过保留时间和准确质量（使用内部数据库）进行残留检测。通过对每种化合物的碎片离子和同位素模式进行搜索，对检测到的化合物进行鉴定。对优化后的方法进行验证，在所包括的数据库（364 种化合物）中，鸡肉饲料中 30%、68%和 80%的化合物在三个浓度（10、50 和 100μg/kg）下的回收率在 60%至 120%之间。SANCO 12495/2011 和 2002/657/CE 指令被用作方法验证的指南。日内和日间精密度（以相对标准偏差表示）对于超过 90%的化合物低于 20%。大多数分析物的定量限为 4 至 200μg/kg，足以验证产品是否符合法定公差。该程序的适用性还通过评估回收率和重复性，在不同类型的饲料（鸡、母鸡、兔子和马饲料）上进行了进一步测试。最后，该方法应用于 18 个饲料样品的分析，检测到一些 VDs（磺胺嘧啶、甲氧苄啶、罗比那丁和莫能菌素 Na）和一种农药（毒死蜱）。
