Eastern Regional Research Center, US Department of Agriculture, Agricultural Research Service, 600 East Mermaid Lane, Wyndmoor, PA, 19038, USA.
Anal Bioanal Chem. 2018 Jan;410(3):1095-1109. doi: 10.1007/s00216-017-0688-9. Epub 2017 Oct 23.
The way to maximize scope of analysis, sample throughput, and laboratory efficiency in the monitoring of veterinary drug residues in food animals is to determine as many analytes as possible as fast as possible in as few methods as possible. Capital and overhead expenses are also reduced by using fewer instruments in the overall monitoring scheme. Traditionally, the highly polar aminoglycoside antibiotics require different chromatographic conditions from other classes of drugs, but in this work, we demonstrate that an ion-pairing reagent (sodium 1-heptanesulfonate) added to the combined final extracts from two sample preparation methods attains good separation of 174 targeted drugs, including 9 aminoglycosides, in the same 10.5-min ultrahigh-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) analysis. The full method was validated in bovine kidney, liver, and muscle tissues according to US regulatory protocols, and 137-146 (79-84%) of the drugs gave between 70 and 120% average recoveries with ≤ 25% RSDs in the different types of tissues spiked at 0.5, 1, and 2 times the regulatory levels of interest (10-1000 ng/g depending on the drug). This method increases sample throughput and the possible number of drugs monitored in the US National Residue Program, and requires only one UHPLC-MS/MS method and instrument for analysis rather than two by the previous scheme. Graphical abstract Outline of the streamlined approach to monitor 174 veterinary drugs, including aminoglycosides, in bovine tissues by combining two extracts of the same sample with an ion-pairing reagent for analysis by UHPLC-MS/MS.
最大限度地分析范围、样品通量和实验室效率,以监测食品动物中兽药残留的方法是尽可能快地确定尽可能多的分析物,尽可能少的方法。通过在整个监测方案中使用更少的仪器,还可以降低资本和间接费用。传统上,高度极性的氨基糖苷类抗生素需要与其他类别的药物不同的色谱条件,但在这项工作中,我们证明,在两种样品制备方法的组合最终提取物中添加离子对试剂(1-庚烷磺酸钠)可以实现 174 种靶向药物的良好分离,包括 9 种氨基糖苷类药物,在相同的 10.5 分钟超高效液相色谱-串联质谱(UHPLC-MS/MS)分析中。根据美国法规方案,在牛肾、肝和肌肉组织中对全方法进行了验证,在不同类型的组织中,137-146(79-84%)种药物的平均回收率在 70-120%之间,相对标准偏差(RSD)≤25%,在感兴趣的监管水平(10-1000ng/g,取决于药物)的 0.5、1 和 2 倍水平下进行了加标。该方法提高了样品通量和美国国家残留计划中监测的可能药物数量,并且仅需要一种 UHPLC-MS/MS 方法和仪器进行分析,而不是以前方案中的两种。图表摘要 概述了通过将同一样品的两种提取物与离子对试剂结合,用于 UHPLC-MS/MS 分析,从而简化监测牛组织中 174 种兽药(包括氨基糖苷类药物)的方法。