Food Safety Department, Teagasc Food Research Centre, Ashtown, Dublin 15, Ireland; Team Elucidate, Department of Chemistry, Cork Institute of Technology, Bishopstown, Cork, Ireland.
Department of Life, Health and Environmental Sciences, University of L'Aquila, L'Aquila, Italy.
J Chromatogr B Analyt Technol Biomed Life Sci. 2014 Jun 1;960:105-15. doi: 10.1016/j.jchromb.2014.04.024. Epub 2014 Apr 20.
An UHPLC-MS/MS method was developed for the quantitative confirmatory analysis of residues of nitroimidazole drugs (dimetridazole, ipronidazole, metronidazole, ornidazole and ronidazole) and their corresponding hydroxy metabolites (HMMNI, ipronidazile-OH and metronidazole-OH) in aquaculture tissue. Samples were extracted by shaking in acetonitrile, water, MgSO4 and NaCl before being defatted with n-hexane pre-saturated with acetonitrile and concentrated under nitrogen. Nitroimidazole residues were determined by UHPLC-MS/MS operating in positive electrospray ionisation mode using a reversed phase BEH C18 column. The method was validated according to the EU Commission Decision 2002/657/EC guidelines. The following performance studies were carried out: specificity, selectivity, linearity, within laboratory repeatability (WLr)/reproducibility (WLR), accuracy, precision, decision limit (CCα), detection capability (CCβ), absolute recovery and stability. The analytical range of the method is 0.1-20 μg kg(-1). Accuracy and precision of the method, under within-laboratory reproducibility conditions, ranged from 83 to 105% and 2.3 to 14.0%, respectively. CCα were 0.07-1.0 μg kg(-1) depending on analyte and matrix. A total of 50 samples can be analysed in a single day using the assay. The method has been extensively evaluated through application to real test samples.
建立了一种超高效液相色谱-串联质谱（UHPLC-MS/MS）方法，用于定量确证水产组织中硝基咪唑类药物（二甲硝唑、异丙硝唑、甲硝唑、奥硝唑和罗硝唑）及其相应羟基代谢物（HMMNI、异丙硝唑-OH 和甲硝唑-OH）残留的分析。样品在乙腈、水、MgSO4 和 NaCl 中振荡提取，然后用正己烷预饱和乙腈脱脂，并在氮气下浓缩。硝基咪唑类药物残留采用正电喷雾离子化模式的 UHPLC-MS/MS 进行测定，使用反相 BEH C18 柱。该方法按照欧盟委员会 2002/657/EC 号决定的指南进行验证。进行了以下性能研究：特异性、选择性、线性、实验室内部重复性（WLr）/再现性（WLR）、准确度、精密度、决策限（CCα）、检测能力（CCβ）、绝对回收率和稳定性。该方法的分析范围为 0.1-20 μg kg(-1)。在实验室内部再现性条件下，方法的准确度和精密度范围分别为 83-105%和 2.3-14.0%。取决于分析物和基质，CCα 为 0.07-1.0 μg kg(-1)。该方法每天可分析 50 个样本。该方法已通过实际测试样品的应用进行了广泛评估。
