Laboratory of Analytical Chemistry, Department of Chemistry, Aristotle University of Thessaloniki, GR-54124 Thessaloniki, Greece.
Laboratory of Operative Dentistry, Department of Dentistry, Aristotle University of Thessaloniki, GR-54124 Thessaloniki, Greece.
J Chromatogr B Analyt Technol Biomed Life Sci. 2022 Jan 1;1188:123073. doi: 10.1016/j.jchromb.2021.123073. Epub 2021 Nov 30.
A rapid and simple fabric phase sorptive extraction (FPSE) procedure is developed for the simultaneous extraction of four monomers (Bisphenol A, BPA; Triethylene glycol dimethacrylate, TEGDMA; Urethane dimethacrylate, UDMA; Bisphenol A-glycidyl methacrylate, BisGMA) in human saliva, prior to the determination by high pressure liquid chromatography with an ultraviolet-visible detector. FPSE is a green sample preparation technique, harmonized with the principles of Green Analytical Chemistry (GAC), which utilizes a flexible surface, such as cellulose, chemically coated with a polymeric material using sol-gel technology. FPSE membranes are characterized by superior chemical stability and any solvent or solvent mixture can be used for elution. Among twelve different sol-gel coated membranes, an FPSE membrane coated with sol-gel polytetrahydrofuran (sol-gel PTHF) was found optimum to extract four target compounds from saliva samples, which were first centrifuged. Parameters with most significant impact on the extraction efficiency of FPSE including elution solvent, utilization of magnetic stirring, extraction time have been comprehensively studied and optimized. The studied compounds' separation was carried out by a Perfect Sil 120 ODS-2 chromatographic column (250 mm × 4.0 mm, 5 μm), using a mobile phase constituting of acetonitrile-water 70:30 % v/v (isocratic elution). The total analysis time was 10 min. Detection was achieved by an ultraviolet-visible detector at 220 nm. The method was validated in terms of sensitivity, linearity, trueness, precision, selectivity and stability of samples. For all four compounds, the limit of detection and the limit of quantification were 0.075 ng/μL and 0.25 ng/μL, respectively. Relative recovery rates were between 90.0 and 106.7%, while RSD values were <8.1 and 12% for interday and intraday repeatability, respectively. Youden & Steiner approach was applied to study method's ruggedness and reusability of the media was tested, which enhanced the green nature of technique.
一种快速而简单的纤维相固相萃取（FPSE）程序被开发出来，用于同时萃取人唾液中的四种单体（双酚 A、BPA；三乙二醇二甲基丙烯酸酯、TEGDMA；尿烷二甲基丙烯酸酯、UDMA；双酚 A-甲基丙烯酸缩水甘油酯、BisGMA），然后通过高压液相色谱法与紫外可见检测器进行测定。FPSE 是一种绿色的样品制备技术，与绿色分析化学（GAC）的原则相协调，它利用纤维素等柔性表面，通过溶胶-凝胶技术用聚合物材料化学涂覆。FPSE 膜具有优异的化学稳定性，可以使用任何溶剂或溶剂混合物进行洗脱。在十二种不同的溶胶-凝胶涂覆膜中，发现用溶胶-凝胶聚四氢呋喃（溶胶-凝胶 PTHF）涂覆的 FPSE 膜最适合从唾液样品中提取四种目标化合物，这些样品首先经过离心处理。对 FPSE 萃取效率影响最大的参数包括洗脱溶剂、使用磁力搅拌、萃取时间等，均进行了全面研究和优化。在所研究的化合物的分离中，采用 Perfect Sil 120 ODS-2 色谱柱（250mm×4.0mm，5μm），使用由乙腈-水 70:30%（v/v）（等度洗脱）组成的流动相。总分析时间为 10 分钟。通过在 220nm 处的紫外可见检测器进行检测。该方法在灵敏度、线性、准确性、精密度、选择性和样品稳定性方面进行了验证。对于所有四种化合物，检测限和定量限分别为 0.075ng/μL 和 0.25ng/μL。相对回收率在 90.0%至 106.7%之间，日内和日间重复性的 RSD 值分别小于 8.1%和 12%。应用 Youden & Steiner 方法研究方法的稳健性，并测试了介质的可重复使用性，这增强了该技术的绿色特性。
