Abdel-Monem Maha Mohammad, Walash Mohamed I, Kamal El-Deen Asmaa
Pharmaceutical Analytical Chemistry Department, Faculty of Pharmacy, Mansoura University, Mansoura, Egypt.
Phytochem Anal. 2025 Apr;36(3):693-703. doi: 10.1002/pca.3460. Epub 2024 Oct 28.
The simultaneous determination of multiple anticancer drugs in combination therapy poses a significant analytical challenge due to their complex nature and low concentrations. In this study, we propose an in-syringe vortex-assisted liquid-liquid microextraction (IS-VA-LLME), based on a green natural deep eutectic solvent (NaDES) for the simultaneous determination of two coadministered anticancer drugs (resveratrol and chrysin) prior to the HPLC-UV analysis, for the first time. The key parameters affecting the extraction efficiency, such as extraction solvent, vortex time, pH, and ionic strength were optimized. Under optimal conditions, the method demonstrates good linearity over the range of 0.05-15.0 μg/mL for RVT and 0.50-15.0 μg/mL for CHR with low limits of detection (LODs) of 16.78 and 161.60 ng/mL for RVT and CHR, respectively, confirming the high sensitivity of the method. The interday and intraday precision values, expressed as %RSDs, are below 2.0%, indicating good repeatability and reproducibility. Furthermore, the proposed method could be efficiently applied for the determination of the two drugs in human plasma and river water. The obtained results show satisfactory % recoveries (97.80%-102.04%), highlighting the accuracy and reliability of the developed method. The sustainability of the method was comprehensively evaluated using seven different tools. In conclusion, the developed IS-VA-LLME-NaDES allows for enhanced extraction efficiency, reduced extraction time, and improved recovery of the target analytes. This method holds great promise for applications in clinical and environmental research, enabling the precise quantification of these anticancer drugs in complex matrices.
在联合治疗中同时测定多种抗癌药物,因其性质复杂且浓度较低,带来了重大的分析挑战。在本研究中,我们首次提出了一种基于绿色天然深共熔溶剂(NaDES)的注射器内涡旋辅助液液微萃取(IS-VA-LLME)方法,用于在HPLC-UV分析之前同时测定两种共同给药的抗癌药物(白藜芦醇和白杨素)。对影响萃取效率的关键参数,如萃取溶剂、涡旋时间、pH值和离子强度进行了优化。在最佳条件下,该方法对白藜芦醇在0.05 - 15.0μg/mL范围内、对白杨素在0.50 - 15.0μg/mL范围内呈现良好的线性,白藜芦醇和白杨素的检测限(LOD)分别低至16.78和161.60 ng/mL,证实了该方法的高灵敏度。以%RSD表示的日间和日内精密度值均低于2.0%,表明具有良好的重复性和再现性。此外,所提出的方法可有效应用于人体血浆和河水中这两种药物的测定。所得结果显示回收率令人满意(97.80% - 102.04%),突出了所开发方法的准确性和可靠性。使用七种不同工具对该方法的可持续性进行了全面评估。总之,所开发的IS-VA-LLME-NaDES提高了萃取效率,缩短了萃取时间,并改善了目标分析物的回收率。该方法在临床和环境研究应用中具有很大潜力,能够在复杂基质中精确量化这些抗癌药物。