Doctoral School of Exact and Natural Sciences, Jagiellonian University, Łojasiewicza 11, 30-348, Kraków, Poland.
Department of Analytical Chemistry, Faculty of Chemistry, Jagiellonian University, Gronostajowa 2, 30-387, Kraków, Poland.
Environ Sci Pollut Res Int. 2024 Aug;31(37):49546-49559. doi: 10.1007/s11356-024-34466-5. Epub 2024 Jul 30.
An automated flow analysis-solid phase extraction (FA-SPE) system and methodology of ultra-high-performance liquid chromatography with tandem mass spectrometry (UHPLC-MS/MS) analysis were developed for the determination of selected antiviral drugs (acyclovir, amantadine, rimantadine, and oseltamivir) in water samples. The proposed FA-SPE approach enables the integration of various extraction stages and elimination of the sample evaporation step and offers individual customisation of SPE parameters, inter alia sample, and eluate flow rate and volume. Using the developed FA-SPE procedure, e.g. a 100-fold preconcentration of the target analytes in 1 h was achieved. A method for chromatographic analysis was also developed to determine the selected antiviral drugs in combination with the use of the FA-SPE system. The developed FA-SPE UHPLC-MS/MS method was validated including the determination of linearity of analytical graphs, limits of detection (5.5-99.9 pg mL) and quantification (18.3-329.8 pg mL), intra-day (1.8-8.3%) and inter-day (3.0-9.2%) precision, recovery (95.6-105.3%), and matrix effects (- 12.9 to 13.2%). The proposed method was successfully applied to analyse tap, drinking, and river water samples, revealing the presence of amantadine at a concentration of 40.1 pg mL in one sample. The environmental impact of the developed FA-SPE sample preparation procedure was also assessed using the AGREEprep metric tool and compared with five other literature methods, achieving the most sustainable outcome.
建立了一种自动化流动分析-固相萃取(FA-SPE)系统和超高效液相色谱-串联质谱(UHPLC-MS/MS)分析方法,用于测定水样中的几种抗病毒药物(阿昔洛韦、金刚烷胺、金刚乙胺和奥司他韦)。所提出的 FA-SPE 方法能够整合多个萃取阶段并消除样品蒸发步骤,并且可以单独定制 SPE 参数,例如样品和洗脱液的流速和体积。使用开发的 FA-SPE 程序,例如,可以在 1 小时内将目标分析物进行 100 倍浓缩。还开发了一种用于结合 FA-SPE 系统同时测定所选抗病毒药物的色谱分析方法。该开发的 FA-SPE-UHPLC-MS/MS 方法进行了验证,包括分析图谱的线性度、检测限(5.5-99.9 pg mL)和定量限(18.3-329.8 pg mL)、日内(1.8-8.3%)和日间(3.0-9.2%)精密度、回收率(95.6-105.3%)和基质效应(-12.9 至 13.2%)。该方法成功应用于分析自来水、饮用水和河水样品,在一个样品中发现金刚烷胺的浓度为 40.1 pg mL。还使用 AGREEprep 度量工具评估了开发的 FA-SPE 样品制备程序的环境影响,并与其他五种文献方法进行了比较,达到了最可持续的结果。