Ninga Ederina, Sapozhnikova Yelena, Lehotay Steven J, Lightfield Alan R, Monteiro Sergio H
Department of Toxicology and Residues Monitoring, Food Safety and Veterinary Institute, 1001 Tirana, Albania.
Eastern Regional Research Center, Agricultural Research Service, United States Department of Agriculture, 600 East Mermaid Lane, Wyndmoor, Pennsylvania 19038, United States.
J Agric Food Chem. 2021 Feb 3;69(4):1169-1174. doi: 10.1021/acs.jafc.0c00995. Epub 2020 Jun 8.
The goal of this study was to develop and validate a new method for simultaneous determination of 106 veterinary drugs and 227 pesticides and their metabolites plus 16 polychlorinated biphenyls (PCBs) at and below their regulatory levels established for catfish muscle in the European Union and U.S.A. To do this, two different QuEChERS-based methods for veterinary drugs and pesticides and PCBs were modified and merged into a single mega-method dubbed "QuEChERSER" (more than QuEChERS), which is presented here for the first time. The mega-method was validated in catfish at four different spiking levels with 10 replicates per level. Sample extraction of 2 g test portions was made with 10 mL of 4:1 (v/v) acetonitrile/water, and then an aliquot was taken for ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) analysis of 106 veterinary drugs and 125 pesticides, including metabolites. The remaining extract after salting out was subjected to automated mini-solid-phase extraction cleanup (Instrument Top Sample Preparation) for immediate injection in low-pressure gas chromatography-tandem mass spectrometry (LPGC-MS/MS). The cleanup was conducted in parallel with the 10 min LPGC-MS/MS analysis for 167 PCBs, pesticides, and metabolites, which was conducted in parallel with the 10 min UHPLC-MS/MS analysis for 231 analytes to increase sample throughput (49 analytes were included in both techniques). In MS/MS, three ion transitions were monitored for nearly all targeted analytes to provide unambiguous identification as well as quantification. Satisfactory recoveries (70-120%) and relative standard deviations of ≤20% were achieved for 98 (92%) of the veterinary drugs and their metabolites and for 222 (91%) of pesticides, metabolites, and PCBs, demonstrating that the developed method is applicable for the analysis of these contaminants in fish as part of regulatory monitoring programs and other purposes.
本研究的目标是开发并验证一种新方法，用于同时测定106种兽药、227种农药及其代谢物以及16种多氯联苯（PCBs），其含量处于欧盟和美国为鲶鱼肌肉设定的监管水平及以下。为此，对两种基于QuEChERS的不同方法（分别用于兽药和农药及多氯联苯）进行了修改，并合并为一种名为“QuEChERSER”（比QuEChERS更强大）的单一超级方法，本文首次介绍该方法。该超级方法在鲶鱼中进行了验证，设置了四个不同的加标水平，每个水平重复测定10次。取2 g测试部分样品，用10 mL 4:1（v/v）乙腈/水进行提取，然后取一份等分试样用于106种兽药和125种农药（包括代谢物）的超高效液相色谱-串联质谱（UHPLC-MS/MS）分析。盐析后的剩余提取物进行自动微型固相萃取净化（仪器顶部样品制备），以便立即注入低压气相色谱-串联质谱（LPGC-MS/MS）进行分析。净化过程与167种多氯联苯、农药和代谢物的10分钟LPGC-MS/MS分析并行进行，而该分析又与231种分析物的10分钟UHPLC-MS/MS分析并行进行，以提高样品通量（两种技术共包含49种分析物）。在串联质谱分析中，几乎所有目标分析物均监测三个离子跃迁，以实现明确的定性和定量。98种（92%）兽药及其代谢物以及222种（91%）农药、代谢物和多氯联苯的回收率令人满意（70 - 120%），相对标准偏差≤20%，这表明所开发的方法适用于作为监管监测计划及其他目的一部分的鱼类中这些污染物的分析。
