Patakidou Christina, Ntorkou Marianna, Zacharis Constantinos K
Laboratory of Pharmaceutical Analysis, Department of Pharmacy, Aristotle University of Thessaloniki, Thessaloniki, Greece.
Laboratory of Analytical Chemistry, Department of Chemistry, Aristotle University of Thessaloniki, Thessaloniki, Greece.
J Sep Sci. 2025 Jul;48(7):e70223. doi: 10.1002/jssc.70223.
Herein, a switchable solubility solvent (sodium salicylate) was employed for the microextraction of "profenoid" drugs (i.e., ketoprofen, fenoprofen, and flurbiprofen) from human urine samples. This approach utilizes the phase transition of salicylic acid (0.75 mol/L) by altering the sample's pH (addition of 10 µL of HPO 10 M), facilitating efficient dispersion and phase separation in a single step. The solidified salicylic acid was easily collected using a syringe filter (nylon). In addition, the extensive contact area between the solidified solvent and the sample solution ensured effective extraction of the target analyte. The critical experimental parameters affecting the extraction performance of the analytes were examined. The separation of the drugs was carried out on a C analytical column using gradient elution. Excellent linearity was observed in the dynamic range of 50-3000 ng/mL while the precision (%RSD) was less than 14.3% in all cases. The intraday and interday trueness were satisfactory, being in the range of 82.3%-110.1%. The green potential of the proposed analytical scheme was examined based on AGREEprep, ComplexMoGAPI, CACI, and AGREE metric tools. The developed method was utilized for the analysis of authentic urine samples after oral administration of a ketoprofen-containing formulation.
在此,采用一种可切换溶解度的溶剂(水杨酸钠)从人尿液样本中微萃取“类布洛芬”药物(即酮洛芬、非诺洛芬和氟比洛芬)。该方法通过改变样品的pH值(加入10 μL 10 M的HPO)利用水杨酸(0.75 mol/L)的相变,在一步中促进高效分散和相分离。使用注射器滤器(尼龙)可轻松收集固化的水杨酸。此外,固化溶剂与样品溶液之间广泛的接触面积确保了目标分析物的有效萃取。研究了影响分析物萃取性能的关键实验参数。在C分析柱上使用梯度洗脱进行药物分离。在50 - 3000 ng/mL的动态范围内观察到极佳的线性,而在所有情况下精密度(%RSD)均小于14.3%。日内和日间准确性令人满意,范围为82.3% - 110.1%。基于AGREEprep、ComplexMoGAPI、CACI和AGREE度量工具对所提出分析方案的绿色潜力进行了研究。所开发的方法用于分析口服含酮洛芬制剂后的真实尿液样本。