Laboratory of Pharmaceutical Analysis, School of Pharmacy, Aristotle University of Thessaloniki, 54124 Thessaloniki, Greece.
International Forensic Research Institute, Department of Chemistry and Biochemistry, Florida International University, Miami, FL, USA.
J Chromatogr A. 2024 Aug 16;1730:465157. doi: 10.1016/j.chroma.2024.465157. Epub 2024 Jul 9.
Capsule phase microextraction (CPME) is an efficient bioanalytical technique that streamlines the sample preparation by integrating the filtration and stirring mechanism directly into the device. A novel composite sorbent designed to be selective towards the target analytes consisting of mixed-mode sorbent chemistry synthesized by sol-gel technology is found promising and superior to the conventional C sorbents. Herein we describe the encapsulation of an ionic liquid (IL)/Carbowax 20M-functionalized sol-gel sorbent (sol-gel IL/Carbowax 20 M) in the lumen of porous polypropylene tubes for the capsule phase microextraction of three phosphodiesterase-5 inhibitors namely avanafil, sildenafil, and tadalafil in human serum and urine samples. The CPME device was characterized by Scanning Electron Microscopy (SEM) and Fourier-Transform Infrared Spectroscopy (FT-IR). The experimental parameters of CPME procedure (e.g. sample pH and ionic strength, extraction time, stirring rate, elution solvent and volume) were carefully optimized to achieve the highest possible extraction efficiency for the analytes. Method validation was conducted in terms of precision, linearity, accuracy, matrix effect, lower limits of quantification, and limits of detection (LOD). The method linearity was investigated in the range of 50-1000 ng mL for all analytes while the precision was less than 11.8 % in all cases. For all analytes, the LOD values were 17 ng mL. The IL/CW 20M-functionalized microextraction capsules could be reused at least 25 times both for urine and serum samples. The green character and the applicability of the proposed method were evaluated using the ComplexGAPI and BAGI indexes. The optimized CPME protocol exhibited reduced consumption of organic solvent and generation of waste, cost-effectiveness, and simplicity. Finally, the proposed method was successfully applied to the analysis of sildenafil in human urine after administration of drug-containing formulation.
胶囊相微萃取 (CPME) 是一种高效的生物分析技术，通过将过滤和搅拌机制直接集成到装置中，简化了样品制备过程。一种新型的复合吸附剂，由溶胶-凝胶技术合成的混合模式吸附剂化学物质设计而成，对目标分析物具有选择性，被发现比传统的 C 吸附剂更有前途。本文描述了将离子液体 (IL)/Carbowax 20M 功能化的溶胶-凝胶吸附剂 (溶胶-凝胶 IL/Carbowax 20M) 封装在多孔聚丙烯管的内腔中，用于胶囊相微萃取三种磷酸二酯酶-5 抑制剂，即阿伐那非、西地那非和他达拉非在人血清和尿液样本中的应用。CPME 装置通过扫描电子显微镜 (SEM) 和傅里叶变换红外光谱 (FT-IR) 进行了表征。CPME 程序的实验参数（例如样品 pH 值和离子强度、萃取时间、搅拌速度、洗脱溶剂和体积）经过仔细优化，以实现对分析物的最高可能萃取效率。该方法在精密度、线性、准确性、基质效应、定量下限和检测限 (LOD) 方面进行了验证。该方法的线性范围为所有分析物的 50-1000ng/mL，所有情况下的精密度均小于 11.8%。所有分析物的 LOD 值均为 17ng/mL。IL/CW 20M 功能化微萃取胶囊可在尿液和血清样本中至少重复使用 25 次。使用 ComplexGAPI 和 BAGI 指数评估了该方法的绿色特性和适用性。优化后的 CPME 方案显示出有机溶剂消耗和废物产生减少、成本效益高、简单易用的特点。最后，该方法成功应用于含药制剂给药后人尿中西地那非的分析。
