Abstract：
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 C18 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-1 for all analytes while the precision was less than 11.8 % in all cases. For all analytes, the LOD values were 17 ng mL-1. 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.
摘要：
胶囊相微萃取（CPME）是一种有效的生物分析技术，可通过将过滤和搅拌机构直接集成到设备中来简化样品制备。一种新型复合吸附剂，旨在对目标分析物具有选择性，该吸附剂由通过溶胶-凝胶技术合成的混合模式吸附剂化学组成，具有良好的前景，并且优于常规的C18吸附剂。在这里，我们描述了离子液体（IL）/Carbowax20M功能化的溶胶-凝胶吸附剂（溶胶-凝胶IL/Carbowax20M）在多孔聚丙烯管的内腔中的封装，用于三种磷酸二酯酶-5抑制剂的胶囊相微萃取，即avanafil，西地那非,人血清和尿液样本中的他达拉非。通过扫描电子显微镜（SEM）和傅立叶变换红外光谱（FT-IR）对CPME器件进行了表征。CPME程序的实验参数(例如样品pH和离子强度，提取时间,搅拌速率,仔细优化洗脱溶剂和体积），以实现分析物的最高提取效率。方法验证是在精度方面进行的，线性度准确度,基体效应，定量下限，和检测限（LOD）。在所有分析物的50-1000ngmL-1范围内研究了方法线性，而在所有情况下精密度均小于11.8％。对于所有分析物，LOD值为17ngmL-1.IL/CW20M功能化的微萃取胶囊可重复使用至少25次用于尿液和血清样品。使用ComplexGAPI和BAGI指标评估了所提出方法的绿色特性和适用性。优化的CPME方案显示出减少的有机溶剂消耗和废物的产生，成本效益，和简单。最后,该方法已成功应用于含药物制剂给药后人尿中西地那非的分析。
