Department of Chemistry, Faculty of Basic Sciences, Azarbaijan Shahid Madani University, Tabriz, Iran.
Department of Chemistry, Faculty of Basic Sciences, Azarbaijan Shahid Madani University, Tabriz, Iran.
J Chromatogr B Analyt Technol Biomed Life Sci. 2023 Jun 1;1225:123757. doi: 10.1016/j.jchromb.2023.123757. Epub 2023 May 19.
3D printed solid phase microextraction scaffolds as a novel sorbent were introduced for the extraction of antifungal drugs in wastewater and human plasma prior to their determination by HPLC-UV. The designed adsorbent was prepared as cubic scaffolds using fused deposition modeling (FDM) 3D printer and Polylactic acid (PLA) filament. Scaffold surface was chemically modified using alkaline ammonia solution (Alkali treatment). The application of this new design in the extraction of three antifungal drugs ketoconazole, clotrimazole and miconazole was investigated. Alkali surface modification time was optimized (0.5-5hr) and 4hr selected as the best-modification time. Morphology of the modified surface and its chemical changes were studied using Field Emission Scanning Electron Microscope (FE-SEM) and Attenuated Total Reflectance Fourier Transform Infrared spectroscopy (ATR-FTIR), respectively. Surface wettability of scaffolds was measured by Water Contact Angel (WCA) and the porosity created in the scaffolds was studied by N adsorption/desorption studies analysis. Analytical performance of the method, under optimum conditions (extraction time: 25 min, desorption solvent: methanol, volume of desorption solvent: 2 mL, desorption time: 10 min, solution pH: 8, solution temperature: 40 °C, salt concentration: 3 mol L) were obtained as 3.10 and 10.0 µg L for LOD and LOQ, respectively. The calibration graphs were linear in the range of 10-150 µg L and 10-100 µg L for wastewater and plasma, respectively.
3D 打印固相微萃取支架作为一种新型吸附剂，用于萃取废水和人血浆中的抗真菌药物，然后用 HPLC-UV 进行测定。设计的吸附剂采用熔融沉积建模（FDM）3D 打印机和聚乳酸（PLA）长丝制成立方支架。支架表面用碱性氨溶液进行化学改性（碱处理）。研究了这种新设计在提取三种抗真菌药物酮康唑、克霉唑和咪康唑中的应用。优化了碱表面改性时间（0.5-5 小时），选择 4 小时为最佳改性时间。采用场发射扫描电子显微镜（FE-SEM）研究了改性表面的形貌及其化学变化，采用衰减全反射傅里叶变换红外光谱（ATR-FTIR）研究了其化学变化。采用水接触角（WCA）测量支架的表面润湿性，通过氮气吸附/解吸研究分析研究支架中产生的孔隙率。在最佳条件下（萃取时间：25 分钟，解吸溶剂：甲醇，解吸溶剂体积：2 毫升，解吸时间：10 分钟，溶液 pH：8，溶液温度：40°C，盐浓度：3mol L），该方法的分析性能分别为 3.10 和 10.0µg L，LOD 和 LOQ 分别为 10-150µg L 和 10-100µg L。废水和血浆的校准曲线在 10-150µg L 和 10-100µg L 范围内均呈线性。
