A fabric phase sorptive extraction method for the LC-UV determination of bisphenol A and leaching monomers from dental materials in human saliva

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 x 4.0 mm, 5 mu m), 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/mu L and 0.25 ng/mu L, 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.

Automated summary

A rapid and simple fabric phase sorptive extraction (FPSE) method using sol-gel technology was developed for the simultaneous extraction of four monomers in human saliva. The optimized FPSE method demonstrated excellent extraction efficiency and stability. The developed method was successfully validated in terms of sensitivity, linearity, trueness, precision, selectivity, and stability of samples. The method's green nature was enhanced by the robustness and reusability of the media.