School of Pharmacy, Shanxi Medical University, Taiyuan 030001, PR China.
School of Pharmacy, Shanxi Medical University, Taiyuan 030001, PR China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2021 Jul 15;1178:122583. doi: 10.1016/j.jchromb.2021.122583. Epub 2021 Feb 22.
A hollow fiber liquid phase microextraction (HF-LPME) based on a reversed lipid micelle as the extraction phase was proposed and combined with high performance liquid chromatography (HPLC) for the determination of rotigotine in biological matrix. In the proposed procedure, pieces of hollow fibers were fastened on a magnetic stir bar using a thread to provide better precision. Rotigotine was extracted from 5 mL of diluted plasma sample phase with pH 6 into reversed lipid micelle (5 mmol/L of dipalmitoyl phosphatidyl choline in n-octanol/water) impregnated in both the wall pores and the lumen of the hollow fiber. After the extraction at 900 rpm and room temperature for 30 min, the acceptor phase of reversed lipid micelle was collected for HPLC analysis. Various parameters affecting the extraction efficiency, such as type of surfactant and organic solvent, surfactant concentration, sample phase pH, salt amount, extraction time, stirring rate, and dilution factor of the plasma sample, were investigated and optimized. Furthermore, the formed reversed lipid micelle was characterized by fluorescence method. Under the optimal conditions, the linear range of rotigotine was between 2 ng/mL and 100 ng/mL with determination coefficient (r) ≥ 0.9913. It is shown from results of method validation that the satisfactory accuracy (the relative errors between -8.5% and 3.3%), precision (the relative standard deviations from 3.8% to 8.9%), stability and matrix effect were obtained. The enrichment factor (EF) of the reversed lipid micelle-based HF-LPME for rotigotine reached 126. And the feasibility of the proposed method was confirmed by the application to the pharmacokinetic study of rotigotine in rat plasma.
一种基于反相脂质胶束的中空纤维液相微萃取（HF-LPME）被提出，并与高效液相色谱（HPLC）结合，用于测定生物基质中的罗替高汀。在提出的程序中，将空心纤维的片段用线固定在磁性搅拌棒上，以提供更好的精度。罗替高汀从 5ml 稀释后的血浆样品相中，用 pH 值为 6 的溶液萃取到反相脂质胶束（正十六烷/水体系中的 5mmol/L 二棕榈酰磷脂酰胆碱）中，该胶束既浸渍在空心纤维的壁孔中，也浸渍在空心纤维的内腔中。在 900rpm 和室温下萃取 30min 后，收集反相脂质胶束的接受相，用于 HPLC 分析。研究并优化了影响萃取效率的各种参数，如表面活性剂和有机溶剂的类型、表面活性剂浓度、样品相 pH 值、盐量、萃取时间、搅拌速度以及血浆样品的稀释倍数。此外，还通过荧光法对形成的反相脂质胶束进行了表征。在最佳条件下，罗替高汀的线性范围为 2ng/mL 至 100ng/mL，测定系数（r）≥0.9913。方法验证结果表明，该方法具有令人满意的准确度（相对误差在-8.5%至 3.3%之间）、精密度（相对标准偏差为 3.8%至 8.9%）、稳定性和基质效应。反相脂质胶束-HF-LPME 对罗替高汀的富集因子（EF）达到 126。并通过将该方法应用于大鼠血浆中罗替高汀的药代动力学研究，验证了该方法的可行性。
