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Moxidectin residues in lamb tissues: Development and validation of analytical method by UHPLC-MS/MS
Journal of Chromatography B ( IF 3 ) Pub Date : 2017-12-02 , DOI: 10.1016/j.jchromb.2017.11.041
Michelle Del Bianchi A. Cruz , Maria A.M. Fernandes , Patricia A. de C. Braga , Alda L.G. Monteiro , Daniela Daniel , Felix G.R. Reyes

The development and validation of a throughput method for the quantitation of moxidectin residues in lamb target tissues (muscle, kidney, liver and fat) was conducted using ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC–MS/MS). To achieve higher recovery of the analyte from the matrices, a modified QuEChERS method was used for sample preparation. The chromatographic separation was achieved using a Zorbax Eclipse Plus C18 RRHD column with a mobile phase comprising 5 mM ammonium formate solution +0.1% formic acid (A) and acetonitrile +0.1% formic acid (B) in a linear gradient program. Method validation was performed based on the Commission Decision 2002/657/EC and VICH GL49. To quantify the analyte, matrix-matched analytical curves were constructed with spiked blank tissues, with a limit of quantitation of 5 ng g−1 and limit of detection of 1.5 ng g−1 for all matrices. The linearity, decision limit, detection capability accuracy, and inter- and intra-day repeatability of the method are reported. The method was successfully applied to incurred lamb tissue samples (muscle, liver, kidney and fat) in a concentration range from 5 to 200 μg kg−1, which demonstrated its suitability for monitoring moxidectin residues in lamb tissues in health surveillance programs, as well as for pharmacokinetics and residue depletion studies.



中文翻译:

羊组织中莫昔克丁残留:UHPLC-MS / MS分析方法的开发和验证

使用超高效液相色谱-串联质谱法(UHPLC–MS / MS)进行了通量方法的开发和验证,该方法用于定量测定羔羊靶组织(肌肉,肾脏,肝脏和脂肪)中莫昔克丁的残留量。为了从基质中获得更高的分析物回收率,改良的QuEChERS方法用于样品制备。使用Zorbax Eclipse Plus C18 RRHD色谱柱进行色谱分离,该色谱柱的流动相包括线性梯度程序中的5 mM甲酸铵溶液+ 0.1%甲酸(A)和乙腈+ 0.1%甲酸(B)。根据委员会决定2002/657 / EC和VICH GL49进行方法验证。为了定量分析物,用加标的空白组织构建基质匹配的分析曲线,定量限为5 ng g-1和所有基质的检出限为1.5 ng g -1。报告了该方法的线性,决策极限,检测能力准确性以及日间和日内重复性。该方法已成功应用于浓度为5至200μgkg -1的羔羊组织样本(肌肉,肝,肾和脂肪),证明了其在健康监测程序中也适用于监测羔羊组织中莫昔克丁残留量。至于药代动力学和残留物消耗研究。

更新日期:2017-12-02
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