US Department of Agriculture, Agricultural Research Service, Eastern Regional Research Center, Wyndmoor, PA 19038, USA.
Drug Test Anal. 2012 Aug;4 Suppl 1:91-102. doi: 10.1002/dta.1359.
Traditionally, regulatory monitoring of veterinary drug residues in food animal tissues involves the use of several single-class methods to cover a wide analytical scope. Multi-class, multi-residue methods (MMMs) of analysis tend to provide greater overall laboratory efficiency than the use of multiple methods, and liquid chromatography-tandem mass spectrometry (LC-MS/MS) of targeted drug analytes usually provides exceptional performance even for complicated sample extracts. In this work, an LC-MS/MS method was optimized and validated in a test of 120 drug analytes from 11 different classes in bovine kidney. The method used 10 ml of 4/1 acetonitrile/water for extraction of 2 g samples and cleanup with hexane partitioning. Quantitative and qualitative performance was assessed for the analytes at fortification levels of 10, 50, 100, and 200 ng/g. With the method, 66 drugs gave 70-120% recovery with ≤ 20% RSD at all levels over the course of 3 days. At the 200 ng/g level, 89 drugs met these same standards. Limits of detection were ≤ 10 ng/g for 109 of the analytes in the kidney matrix in validation experiments. Qualitatively, MS/MS identification criteria were set that ion ratios occur within ± 10% (absolute value) from those of the analyte reference standards. At the 10 ng/g level, 57% of the drugs met the identification criteria, which improved to 84% at the 200 ng/g level. The method serves as an efficient and useful additional option among the current monitoring methods available.
传统上,食品动物组织中兽药残留的监管监测涉及使用几种单类方法来覆盖广泛的分析范围。多类、多残留分析方法 (MMMs) 往往比使用多种方法提供更高的整体实验室效率,而针对药物分析物的液相色谱-串联质谱 (LC-MS/MS) 通常即使对复杂的样品提取物也能提供出色的性能。在这项工作中,优化和验证了一种针对牛肾中 11 种不同类别 120 种药物分析物的 LC-MS/MS 方法。该方法使用 10 ml 4/1 乙腈/水提取 2 g 样品,并用正己烷分配进行净化。在 10、50、100 和 200 ng/g 的添加水平下,对分析物的定量和定性性能进行了评估。该方法在 3 天的时间内,在所有水平下,66 种药物的回收率为 70-120%,相对标准偏差(RSD)≤20%。在 200 ng/g 水平下,89 种药物达到了相同的标准。在验证实验中,在肾脏基质中,109 种分析物的检测限≤10 ng/g。定性方面,设定了 MS/MS 鉴定标准,即离子比在分析物参考标准的±10%(绝对值)范围内。在 10 ng/g 水平下,57%的药物符合鉴定标准,在 200 ng/g 水平下提高到 84%。该方法是当前可用监测方法的有效且有用的附加选择。