Department of Analytical Chemistry, University of Barcelona, Martí i Franquès 1-11, E-08028 Barcelona, Spain.
J Chromatogr A. 2010 Sep 10;1217(37):5802-7. doi: 10.1016/j.chroma.2010.07.041. Epub 2010 Jul 22.
We present a fast liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the analysis of the coccidiostat amprolium in food samples. Tandem mass spectrometry in a triple quadrupole was used for quantitative purposes, and the information from multiple-stage mass spectrometry in an ion-trap mass analyzer contributed to fragmentation studies. Hydrophilic interaction liquid chromatography (HILIC) in a Fused-Core column using isocratic elution (acetonitrile:formic acid/ammonium formate buffer pH 4, 50 mM (60:40)) successfully analyzed this compound in less than 3 min. The HILIC system was coupled to heated electrospray-MS/MS using highly selective-selected reaction monitoring (H-SRM) to improve sensitivity and selectivity for the analysis of amprolium, after a simple sample treatment based on an "extract and shoot" strategy. Accurate mass measurements were performed to identify the interfering compound responsible for causing matrix ion enhancement in the signal of amprolium. The addition of l-carnitine (the interfering compound) (1 microg L(-1)) to standards and sample extracts allowed the use of the external calibration method for quantitative purposes. The LC-MS/MS (H-SRM) method showed good precision (relative standard deviation, RSD, lower than 13%), accuracy and linearity and allowed the determination of amprolium down to the ppb level (LODs between 0.1 and 0.6 microg kg(-1)).
我们提出了一种快速液相色谱-串联质谱（LC-MS/MS）方法，用于分析食品样品中的抗球虫药安普罗姆。串联质谱在三重四极杆中用于定量目的，而在离子阱质谱分析仪中的多级质谱信息有助于碎片研究。亲水相互作用液相色谱（HILIC）在使用等度洗脱（乙腈：甲酸/甲酸铵缓冲液 pH 4，50 mM（60：40））的熔融核柱中成功地在不到 3 分钟的时间内分析了这种化合物。在简单的基于“提取和注射”策略的样品处理后，HILIC 系统与加热电喷雾-MS/MS 结合使用高度选择性选择反应监测（H-SRM），以提高安普罗姆分析的灵敏度和选择性。进行精确质量测量以鉴定导致安普罗姆信号中基质离子增强的干扰化合物。向标准品和样品提取物中添加 l-肉碱（干扰化合物）（1μg L（-1））允许使用外部校准方法进行定量目的。LC-MS/MS（H-SRM）方法显示出良好的精密度（相对标准偏差，RSD，低于 13%）、准确性和线性，并允许测定安普罗姆的 ppb 水平（LOD 在 0.1 到 0.6μg kg（-1）之间）。
Zotero 插件