织物相吸附萃取-气相色谱-质谱法测定生物和法医样品中的法匹拉韦

IF 5.2 Q1 CHEMISTRY, ANALYTICAL Advances in Sample Preparation Pub Date : 2023-05-01 DOI:10.1016/j.sampre.2023.100058
Rajeev Jain , Bharti Jain , Abuzar Kabir , Atul Bajaj , Ratnasekhar Ch , Shweta Sharma
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引用次数: 5

摘要

法维匹拉韦是一种吡嗪类似物,被提议在2020年大流行紧急情况下作为抗新冠肺炎感染的主要抗病毒药物。首次开发了织物相吸附萃取(FPSE)与气相色谱-质谱联用(GC-MS)相结合的方法,并将其应用于生物样品(人血浆、血液和尿液)、药物和法医样品中法匹拉韦(FAV)的测定。该方法包括通过FPSE提取FAV,然后用N,O-双(三甲基甲硅烷基)三氟乙酰胺(BSTFA)对其进行衍生和GC-MS分析。基于实验的优化设计分别使用Placket-Burman设计(PBD)和Central Composite设计(CCD)来筛选FPSE的重要因素及其优化。在所有测试的膜中,溶胶-凝胶聚乙二醇(PEG)对FAV的提取效率最高。在最佳条件下,通过GC-MS发现所提出的方法在0.01–10µg mL−1范围内呈线性。通过GC-MS,LOD和LOQ分别低至0.001-0.0026µg mL−1和0.003-0.0086µg mL–1。日内和日间精密度分别低于5%和10%,显示出良好的方法精密度。所提出的方法已成功应用于检测和量化人类尿液、全血和血浆样本以及缴获的法医样本中的FAV。此外,还用ComplexGAPI指数对该方法的绿色性进行了评价。
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Fabric phase sorptive extraction-gas chromatography-mass spectrometry for the determination of favipiravir in biological and forensic samples

Favipiravir, a pyrazine analog, is proposed as providential antiviral agent against the COVID-19 infection during 2020 pandemic emergency. For the first time, a fabric phase sorptive extraction (FPSE) combined with gas chromatography-mass spectrometry (GC-MS) has been developed and applied for the determination of favipiravir (FAV) in biological samples (human plasma, blood and urine), pharmaceutical and forensic samples. The method comprises of extraction of FAV by FPSE followed by its derivatization with N, O-bis (trimethylsilyl) trifluoroacetamide (BSTFA) and GC-MS analysis. Design of experiment-based optimization was performed using Placket-Burman Design (PBD) and Central Composite Design (CCD) for the screening of significant factors of FPSE and their optimization, respectively. Among all tested membranes, sol-gel polyethylene glycol (PEG) has offered the best extraction efficiency for FAV. Under optimum conditions, the proposed method was found to be linear in the range of 0.01–10 µg mL−1 by GC-MS. The LODs and LOQs were as low as 0.001-0.0026 µg mL−1 and 0.003-0.0086 µg mL−1, respectively by GC-MS. Intra-day and inter-day precisions were less than 5 and 10%, respectively, showing good method precision. The proposed method has been successfully applied to detect and quantify FAV in human urine, whole blood and plasma samples along with seized forensic samples. In addition, the proposed method has been evaluated for its green character by ComplexGAPI index.

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