超高效液相色谱-串联质谱法测定鸡饲料中地克珠利的含量

本试验建立了鸡饲料中地克珠利(DIC)含量检测的超高效液相色谱-串联质谱分析方法。采用乙腈提取饲料中的药物,经硅胶固相萃取小柱净化后,超高效液相色谱-串联质谱法(UPLC-MS/MS)分析。整个色谱总时间为3.5 min。结果表明,在5、50、500μg/kg(仅配合饲料)和2000μg/kg(仅预混合饲料)的浓度添加水平下,饲料中地克珠利的回收率范围为90.28%～97.16%;日内变异系数范围为9.24%～14.10%,日间变异系数范围为9.73%～14.87%。以3倍信噪比为检测限,10倍信噪比为定量限,得出该方法的检测限为2.0μg/kg,定量限为5.0μg/kg。该方法操作简单,灵敏度、准确度和精密度均符合饲料中药物添加剂分析的技术要求,能够满足饲料中地克珠利的含量测定需求。

Determination of diclazuril in poultry feed by an ultra high performance liquid chromatography-tandem mass spectrometry method

An ultra high performance liquid chromatography-tandem mass spectrometry method(UPLC/MS/MS) for the determination of diclazuril in poultry feed was developed.The diclazuril was extracted with acetonitrile,purified by silica gel solid phase gathers,and then was determined by UPLC/MS/MS.The tolal time lasted 3.5 min.At the fortification levels of 5,50,500 μg/kg(only for compound feed) and 2000 μg/kg(only for premix feed),the mean recoveries of diclazuril ranged from 90.28 % to 97.16 %.The intra-day CV was 9.24 % ～ 14.10 %,the inter-day CV was 9.73 % ～ 14.87 %.Limit of detection(LOD) and limit of quantitative(LOQ) were 2.0 μg/kg and 5.0 μg/kg.The results indicated that this method was simple,sensitive and accurate for the determination of diclazuril in poultry feed.