Programa de Pós-Graduação em Biologia Celular e Molecular, Centro de Biotecnologia do Estado do Rio Grande do Sul, Universidade Federal do Rio Grande do Sul, Porto Alegre, RS, Brazil.
Anal Chim Acta. 2011 Oct 31;705(1-2):24-9. doi: 10.1016/j.aca.2011.02.041. Epub 2011 Feb 24.
In this work a method is proposed and demonstrated for the analysis of the macrocyclic lactones abamectin, doramectin, eprinomectin, ivermectin and moxidectin in bovine milk by liquid chromatography coupled to mass spectrometry (LC-MS/MS) and liquid chromatography with fluorescence detection (LC-FL). The method is based on liquid-liquid extraction followed by a low temperature purification (LLE-LTP) step. Moreover, the proposed method was validated according to the Commission Decision 2002/657/EC, using LC-MS/MS and LC-FL for confirmatory and quantitative analysis, respectively. For LC-MS/MS the recovery rates observed ranged from 101.2 to 141.6% with coefficient of variation from 2.6 to 19.8%. For LC-FL the recovery rates observed ranged from 100.2 to 105% and coefficient of variations from 2.9 to 8.8%. Matrix effects were negligible due to the low temperature purification step. The quantification limits were far below the maximum limits established by regulations of all countries consulted. The proposed method proved to be simple, easy, and adequate for high-throughput analysis of a large number of samples per day at low cost.
本工作提出并验证了一种利用液相色谱-串联质谱（LC-MS/MS）和液相色谱-荧光检测（LC-FL）分析牛奶中环丙氨嗪、多拉菌素、依维菌素、莫昔克丁和埃普里诺菌素等大环内酯类药物的方法。该方法基于液液萃取（LLE）后低温净化（LLE-LTP）步骤。此外，该方法按照欧盟委员会第 2002/657/EC 号决议进行了验证，分别使用 LC-MS/MS 和 LC-FL 进行确证和定量分析。对于 LC-MS/MS，观察到的回收率范围为 101.2%至 141.6%，变异系数范围为 2.6%至 19.8%。对于 LC-FL，观察到的回收率范围为 100.2%至 105%，变异系数范围为 2.9%至 8.8%。由于低温净化步骤，基质效应可以忽略不计。定量限远低于所有咨询国家法规规定的最高限量。该方法简单、易用，可在每天分析大量样品时以低成本实现高通量分析。
