Department of Analytical Chemistry, Faculty of Pharmacy, Sivas Cumhuriyet University, Sivas, Turkey.
Department of Analytical Chemistry, Faculty of Pharmacy, Erciyes University, Kayseri, Turkey.
Pharmacol Rep. 2023 Apr;75(2):456-464. doi: 10.1007/s43440-023-00465-5. Epub 2023 Feb 25.
The analysis of drug active molecules and residues in the treatment of cancer is important for the sustainability of human life and therapeutic effects. For this purpose, a new magnetic sorbent was developed to use in solid phase extraction prior to conventional high-performance liquid chromatography (HPLC) analysis of Paclitaxel (PAC) and Gemcitabine (GEM) molecules.
In this study, a separation and pre-concentration approach based on magnetic solid phase extraction (MSPE) was proposed for PAC and GEM by means of using a newly synthesized magnetic sorbent. After the MSPE procedure, an HPLC system with a diode array detector (DAD) was used to analyze trace amounts of PAC and GEM anticarcinogenic drugs in urine samples. Surface modification of magnetic FeO nanoparticles was carried out by diaminobenzidinetetrachloro hydrate (DABTC) for the first time and a useful sorbent was obtained for MSPE experiments.
In the proposed method, PAC and GEM molecules were retained on the c in the presence of a pH 5.0 medium and desorbed to 300 μL of acetonitrile: methyl alcohol (1:1) eluent phase before HPLC-DAD analysis. Under the optimized conditions, the limit of detection (LOD) values for PAC and GEM were 1.38 and 1.44 ng mL while the enhancement factor for PAC and GEM were 139.5 and 145.3, respectively. The relative standard deviations (RSD %) for PAC and GEM were below 3.50% in inter-day repeated experiments by means of model solutions containing 100 ng mL drug active ingredients.
Synthesis and characterization of DABTC-FeO nanoparticles were performed using suitable methodologies. Optimization of MSPE was done step by step. And finally, the developed method was successfully applied to urine samples with quantitative recoveries in the range of 99.0% and 105.0%.
分析癌症治疗中的药物活性分子和残留物质对于人类生命的可持续性和治疗效果至关重要。为此,开发了一种新的磁性吸附剂,用于在传统高效液相色谱(HPLC)分析紫杉醇(PAC)和吉西他滨(GEM)分子之前进行固相萃取(SPE)。
在这项研究中,通过使用新合成的磁性吸附剂,提出了一种基于磁性固相萃取(MSPE)的分离和预浓缩方法,用于 PAC 和 GEM。在 MSPE 程序之后,使用带有二极管阵列检测器(DAD)的 HPLC 系统分析尿液样品中痕量的 PAC 和 GEM 抗癌药物。首次使用二氨基联苯四氯水合物(DABTC)对磁性 FeO 纳米粒子进行表面修饰,得到了用于 MSPE 实验的有用吸附剂。
在所提出的方法中,PAC 和 GEM 分子在 pH 5.0 介质的存在下被保留,并在 HPLC-DAD 分析之前用 300μL 的乙腈:甲醇(1:1)洗脱剂相洗脱。在优化条件下,PAC 和 GEM 的检测限(LOD)值分别为 1.38 和 1.44ng mL,而 PAC 和 GEM 的增强因子分别为 139.5 和 145.3。通过含有 100ng mL 药物活性成分的模型溶液进行日内重复实验,PAC 和 GEM 的相对标准偏差(RSD%)均低于 3.50%。
使用合适的方法对 DABTC-FeO 纳米粒子进行了合成和表征。逐步优化了 MSPE。最后,该方法成功应用于尿液样品,定量回收率在 99.0%和 105.0%范围内。