Food and Drug Administration, Department of Health, Taipei, Taiwan, ROC.
J Chromatogr B Analyt Technol Biomed Life Sci. 2012 Jan 15;881-882:12-9. doi: 10.1016/j.jchromb.2011.11.005. Epub 2011 Nov 16.
An ultraperformance liquid chromatography-electrospray tandem mass spectrometry (UPLC-MS/MS) method for the simultaneous detection and confirmation of 23 veterinary (multiclass) drugs in milk was developed and validated. The analytes were extracted by acetonitrile, evaporated and injected into the UPLC-MS/MS system on a Waters UPLC HSS T3 column in gradient mode. Data acquisition under MS/MS was achieved by applying multiple reaction monitoring (MRM) of two ion transitions per compound to provide a high degree of specificity. Results showed good repeatability, and recoveries for the 12 macrolide, 7 β-lactam and 2 lincosamide antibiotics and 2 other veterinary drugs (morantel, orbifloxacin) used in milk averaged 51.8-139.0%, 51.5-100.6%, 82.4-102.5% and 87.5-99.4%, respectively. The coefficients of variation (C.V.) of the recoveries were less than 15% for intraday and interday precisions. The limits of quantification (LOQs) were all lower than 5 ng/ml. This method was applied to 17 fresh milk samples and only lincomycin was found in milk samples under allowable levels. Overall, this method is a suitable and rapid tool to confirm the presence of 23 veterinary drug residues in milk.
建立并验证了一种超高效液相色谱-电喷雾串联质谱法(UPLC-MS/MS)，用于牛奶中 23 种兽药（多类）药物的同时检测和确证。采用乙腈提取，蒸发后进样到 Waters UPLC HSS T3 柱上，在梯度模式下进行 UPLC-MS/MS 系统分析。通过对每个化合物的两个离子转换进行多重反应监测（MRM），实现了 MS/MS 下的数据采集，从而提供了高度的特异性。结果表明，12 种大环内酯类、7 种β-内酰胺类和 2 种林可酰胺类抗生素以及 2 种其他兽药（莫能菌素、氧氟沙星）在牛奶中的重复性良好，回收率平均为 51.8-139.0%、51.5-100.6%、82.4-102.5%和 87.5-99.4%。日内和日间精密度的回收率变异系数（C.V.）均小于 15%。定量限（LOQs）均低于 5 ng/ml。该方法应用于 17 个新鲜牛奶样品中，仅在允许水平下的牛奶样品中发现林可霉素。总的来说，该方法是一种适合且快速的工具，可用于确证牛奶中 23 种兽药残留的存在。
