Nunes Kátia S D, Assalin Márcia R, Vallim José H, Jonsson Claudio M, Queiroz Sonia C N, Reyes Felix G R
Department of Food Science, School of Food Engineering, University of Campinas, Rua Monteiro Lobato 80, 13083-862 Campinas, SP, Brazil.
Embrapa Meio Ambiente, P.O. Box 69, 13820-000 Jaguariúna, SP, Brazil.
J Anal Methods Chem. 2018 Mar 1;2018:4506754. doi: 10.1155/2018/4506754. eCollection 2018.
A multiresidue method for detecting and quantifying sulfonamides (sulfapyridine, sulfamerazine, sulfathiazole, sulfamethazine, sulfadimethoxine, sulfamethoxazole, and sulfamethoxypyridazine) and trimethoprim in tilapia fillet () using liquid chromatography coupled to mass spectrometry was developed and validated. The sample preparation was optimized using the QuEChERS approach. The chromatographic separation was performed using a C18 column and 0.1% formic acid in water and acetonitrile as the mobile phase in the isocratic elution mode. Method validation was performed based on the Commission Decision 2002/657/EC and Brazilian guideline. The validation parameters evaluated were linearity ( ≥ 0.99); limits of detection (LOD) and quantification (LOQ), 1 ng·g and 5 ng·g, respectively; intraday and interdays precision (CV lower than 19.4%). The decision limit (CC 102.6-120.0 ng·g and 70 ng·g for sulfonamides and trimethoprim, respectively) and detection capability (CC 111.7-140.1 ng·g and 89.9 ng·g for sulfonamides and trimethoprim, respectively) were determined. Analyses of tilapia fillet samples from fish exposed to sulfamethazine through feed (incurred samples) were conducted in order to evaluate the method. This new method was demonstrated to be fast, sensitive, and suitable for monitoring sulfonamides and trimethoprim in tilapia fillet in health surveillance programs, as well as to be used in pharmacokinetics and residue depletion studies.
建立并验证了一种使用液相色谱-质谱联用技术检测和定量罗非鱼片中磺胺类药物（磺胺吡啶、磺胺甲基嘧啶、磺胺噻唑、磺胺二甲嘧啶、磺胺二甲氧嘧啶、磺胺甲恶唑和磺胺甲氧嗪）和甲氧苄啶的多残留方法。采用QuEChERS方法对样品制备进行了优化。色谱分离使用C18柱，以0.1%甲酸水溶液和乙腈作为流动相，采用等度洗脱模式。根据欧盟委员会第2002/657/EC号决定和巴西指南进行方法验证。评估的验证参数包括线性（r≥0.99）；检测限（LOD）和定量限（LOQ）分别为1 ng·g⁻¹和5 ng·g⁻¹；日内和日间精密度（CV低于19.4%）。确定了决策限（磺胺类药物和甲氧苄啶分别为CCα 102.6 - 120.0 ng·g⁻¹和70 ng·g⁻¹）和检测能力（磺胺类药物和甲氧苄啶分别为CCβ 111.7 - 140.1 ng·g⁻¹和89.9 ng·g⁻¹）。为评估该方法对通过饲料接触磺胺二甲嘧啶的罗非鱼样品（实际污染样品）进行了分析。这种新方法被证明快速、灵敏，适用于健康监测计划中罗非鱼片中磺胺类药物和甲氧苄啶的监测，也可用于药代动力学和残留消除研究。
