Laboratory of Pharmaceutical Analysis, Department of Pharmacy, Aristotle University of Thessaloniki, 54124 Thessaloniki, Greece.
Laboratory of Analytical Chemistry, Department of Chemistry, Aristotle University of Thessaloniki, Thessaloniki 54124, Greece.
J Chromatogr B Analyt Technol Biomed Life Sci. 2024 Oct 15;1247:124320. doi: 10.1016/j.jchromb.2024.124320. Epub 2024 Sep 14.
Herein, we describe the utilization of an ionic liquid (IL)/Carbowax 20 M-functionalized sol-gel sorbent for the capsule phase microextraction of doxycycline in authentic human urine samples. This green sample preparation method combines stirring and filtration in a single, standalone sample preparation device, streamlining the sample preparation process. Additionally, it provides rapid extraction kinetics and high extraction efficiency. The experimental conditions (i.e. sorbent type, sample pH and volume, extraction time, ionic strength, elution solvent, and volume) affecting the extraction efficiency of the analyte were studied and optimized. The method was linear in the range of 0.1 - 5.0 μg/mL with a coefficient of determination higher than 0.995. The achieved LOD was found to be 0.02 μg/mL while the lower limit of quantitation (LLOQ) was 0.1 μg/mL. The IL/Carbowax 20 M-functionalized microextraction capsules were reusable at least 30 times for urine samples. The relative recoveries (% RR) ranged between 93.4 - 115.9 % while the precision (expressed as % RSD) was better than 8.1 % in all cases. The robustness of the microextraction procedure and the instrumental HPLC method were separately investigated using Plackett-Burman experimental designs. The analytical protocol demonstrated cost-effectiveness, ease of handling, and speed, leading to increased sample throughput. The green character of the developed method was evaluated using the Green Analytical Procedure Index (GAPI) and Blue Applicability Grade Index (BAGI). Finally, the method's applicability was demonstrated by analyzing authentic human urine samples after oral administration of a doxycycline-containing pharmaceutical formulation.
在此，我们描述了一种利用离子液体（IL）/Carbowax 20 M 功能化溶胶-凝胶固定相在真实人体尿液样品中胶囊相微萃取强力霉素的方法。这种绿色的样品制备方法将搅拌和过滤结合在一个独立的样品制备装置中，简化了样品制备过程。此外，它还提供了快速的萃取动力学和高的萃取效率。实验条件（即吸附剂类型、样品 pH 值和体积、萃取时间、离子强度、洗脱溶剂和体积）影响分析物的萃取效率，对其进行了研究和优化。该方法在 0.1-5.0μg/mL 范围内呈线性，相关系数高于 0.995。测定的检出限为 0.02μg/mL，定量下限（LLOQ）为 0.1μg/mL。IL/Carbowax 20 M 功能化微萃取胶囊在尿液样品中至少可重复使用 30 次。在所有情况下，相对回收率（% RR）在 93.4-115.9%之间，精密度（以% RSD 表示）均优于 8.1%。分别使用 Plackett-Burman 实验设计对微萃取程序和仪器高效液相色谱法的稳健性进行了研究。该分析方案具有成本效益、易于操作和快速的特点，提高了样品通量。使用绿色分析程序指数（GAPI）和蓝色适用性等级指数（BAGI）评估了所开发方法的绿色特性。最后，该方法通过分析口服含有强力霉素的药物制剂后的真实人体尿液样品证明了其实用性。
