Wroclaw Medical University Department of Forensic Medicine, 4 J. Mikulicza-Radeckiego Street, Wroclaw 50345, Poland.
Institute of Toxicology Research, 45 Kasztanowa Street, Borowa 55093, Poland.
J Chromatogr B Analyt Technol Biomed Life Sci. 2021 Aug 1;1179:122860. doi: 10.1016/j.jchromb.2021.122860. Epub 2021 Jul 23.
Diclofenac is one of the most frequently prescribed nonsteroidal anti-inflammatory drugs (NSAID) worldwide. Although it is considered a relatively safe drug, it exhibits high toxicity to some animal populations (e.g., raptors). An ultra-sensitive gas chromatography method, coupled with tandem mass spectrometry (GC-QqQ-MS/MS) with an electron impact (EI) ionization source for diclofenac determination in whole blood samples without a derivatization procedure, was developed and fully validated. Diclofenac-d was used as an internal standard. The determination of analytes was performed in the multiple-reaction monitoring (MRM) mode. The method was linear in the range from 0.1 to 200 ng/mL, with a coefficient of determination of 0.999 (R). The lower limit of quantification was 0.1 ng/mL, and the detection limit was 0.05 ng/mL. The blood samples (200 µL) were prepared by liquid-liquid extraction (pH3) with ethyl acetate. The intra- and interday accuracies and precisions did not exceed 15%. Recovery and matrix effect values were in the range of 92.2-105.9% and -7.8 to 5.9%, respectively. The developed method was applied in authentic blood samples. A simple and precise GC-QqQ-MS/MS method can be potentially applied for routine clinical, toxicological and environmental analysis.
双氯芬酸是世界上使用最广泛的非甾体类抗炎药（NSAID）之一。尽管它被认为是一种相对安全的药物，但它对一些动物种群（如猛禽）表现出很高的毒性。本研究建立并充分验证了一种无需衍生化处理，采用带电子轰击（EI）电离源的串联三重四极杆气相色谱-质谱（GC-QqQ-MS/MS）法，对全血样品中的双氯芬酸进行超灵敏检测。双氯芬酸-d 被用作内标。分析物的测定采用多反应监测（MRM）模式。该方法在 0.1-200ng/mL 范围内呈线性，相关系数为 0.999（R）。定量下限为 0.1ng/mL，检测限为 0.05ng/mL。采用乙酸乙酯（pH3）进行液液萃取（LLE）处理 200µL 血样。日内和日间精密度和准确度不超过 15%。回收率和基质效应值分别在 92.2-105.9%和-7.8 至 5.9%范围内。所建立的方法已应用于真实血样。该方法简单、准确，可应用于常规临床、毒理学和环境分析。
