Khazri Hassen, Touaylia Samir, Trabelsi-Ayadi Malika, Ternane Riadh, Ghorbel-Abid Ibtissem
Laboratory for Applications of Chemistry to Resources, Natural Substances and Environment (LACReSNE). Carthage University, Faculty of Sciences of Bizerte, Zarzouna, Carthage University, Zarzouna, Tunisia.
Laboratory of Environment Biomonitoring, Life Sciences Department, Faculty of Sciences Bizerte, University of Carthage, Zarzouna, Tunisia.
Biomed Chromatogr. 2025 Sep;39(9):e70187. doi: 10.1002/bmc.70187.
In this study, a pipette tip solid-phase extraction (PT-SPE) method was developed using cork powder as a natural biosorbent for the extraction of five pharmaceutical contaminants: diclofenac, ibuprofen, ketoprofen, bezafibrate, and fenoprofen. The method was applied to both spiked tap water and real river water samples. The cork powder was characterized using Fourier Transform Infrared Spectroscopy (FTIR), Scanning Electron Microscopy (SEM), and Brunauer-Emmett-Teller (BET) analysis to assess its functional groups, morphology, and surface properties. The analytes were separated and quantified using reverse-phase high-performance liquid chromatography (RP-HPLC) with UV detection at 226 nm. Method optimization was performed by evaluating key parameters, including the amount of adsorbent, sample volume, and desorption solvent. The developed method demonstrated low limits of detection (LOD) ranging from 0.68 to 1.22 μg/L and limits of quantification (LOQ) between 2.06 and 3.68 μg/L. The calibration curves exhibited good linearity (R = 0.978-0.996) over the concentration range of 5-200 μg/L. Satisfactory recoveries were obtained, ranging from 80.32% to 103.3%, with relative standard deviations (RSD) below 6.3%. In real river water samples, some analytes were detected even in non-spiked conditions, whereas no contamination was observed in non-spiked tap water.
在本研究中，开发了一种移液器吸头固相萃取（PT-SPE）方法，使用软木粉作为天然生物吸附剂来萃取五种药物污染物：双氯芬酸、布洛芬、酮洛芬、苯扎贝特和非诺洛芬。该方法应用于加标自来水和实际河水样品。使用傅里叶变换红外光谱（FTIR）、扫描电子显微镜（SEM）和布鲁诺尔-埃米特-泰勒（BET）分析对软木粉进行表征，以评估其官能团、形态和表面性质。使用反相高效液相色谱（RP-HPLC）在226nm处进行紫外检测对分析物进行分离和定量。通过评估关键参数（包括吸附剂用量、样品体积和解吸溶剂）进行方法优化。所开发的方法显示出低检测限（LOD），范围为0.68至1.22μg/L，定量限（LOQ）在2.06至3.68μg/L之间。校准曲线在5-200μg/L的浓度范围内呈现出良好的线性（R = 0.978-0.996）。获得了令人满意的回收率，范围为80.32%至103.3%，相对标准偏差（RSD）低于6.3%。在实际河水样品中，即使在未加标的条件下也检测到了一些分析物，而在未加标的自来水中未观察到污染。
