Escola de Veterinária, Universidade Federal de Minas Gerais (UFMG), Av. Antônio Carlos, 6627, Belo Horizonte, MG 30123-970, Brazil.
Laboratório Nacional Agropecuário (Lanagro-MG), Av. Rômulo Joviano, s/n°, Pedro Leopoldo, MG 33600-000, Brazil.
Talanta. 2017 Aug 15;171:307-320. doi: 10.1016/j.talanta.2017.05.012. Epub 2017 May 8.
A quantitative and confirmatory multiresidue method for determining the presence of avermectins, benzimidazoles and nitroimidazoles in bovine muscle tissue by ultra-high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) was developed, optimized and validated, using a QuEChERS extraction. The evaluated performance parameters were linearity, selectivity, matrix effect, decision limits (CCα), detection capability (CCβ), limits of detection (LOD), limits of quantification (LOQ), accuracy, precision and robustness. The validated method exhibited linearity with coefficient of determination (R) higher than 0.90 in the working range from 0.5 to 2.0 times the maximum residue limit (MRL) or the minimum required performance level (MRPL) for the studied analytes, except for closantel, for which the linear study range was defined from 50 to 200µgkg. The method was selective in the presence of macrolides and lincosamides for all the studied analytes. The LOD varied from 0.007 to 66.715µgkg, whereas LOQ values ranging from 0.011 to 113.674µgkg were found. The results of the evaluation of the accuracy and precision were satisfactory for all the studied analytes, and according to the assessment of the robustness, the method was not robust only for the analytes abamectin, moxidectin, doramectin fenbendazole sulfone, closantel, thiabendazole, hydroxyl-metronidazole and ronidazole. The performance parameters demonstrated total method adequacy for the detection and quantification of avermectins, benzimidazoles and nitroimidazoles residues in bovine muscle tissues.
建立并优化了一种超高效液相色谱串联质谱法(UHPLC-MS/MS),用于定量确证检测牛肌肉组织中阿维菌素类、苯并咪唑类和硝基咪唑类药物残留,采用 QuEChERS 提取法。评估的性能参数包括线性、选择性、基质效应、决策限(CCα)、检测能力(CCβ)、检测限(LOD)、定量限(LOQ)、准确度、精密度和稳健性。验证方法在研究分析物的最大残留限量(MRL)或最低性能水平(MRPL)的 0.5 至 2.0 倍工作范围内,除氯硝柳胺外,其余分析物均表现出良好的线性关系,决定系数(R)均高于 0.90。该方法在存在大环内酯类和林可酰胺类药物的情况下,对所有研究分析物均具有选择性。LOD 范围为 0.007 至 66.715µgkg,LOQ 值范围为 0.011 至 113.674µgkg。对所有研究分析物的准确度和精密度评估结果均令人满意,根据稳健性评估,该方法仅对阿维菌素、莫昔克丁、多拉菌素、芬苯达唑砜、氯硝柳胺、噻苯达唑、羟基甲硝唑和罗硝唑这 7 种分析物不稳健。该方法的性能参数完全适用于检测和定量牛肌肉组织中的阿维菌素类、苯并咪唑类和硝基咪唑类药物残留。