Development and validation of a method using on-line solid-phase extraction and liquid chromatography with ultraviolet detection for the determination of bisphenol A, octylphenol, and nonylphenol in groundwater.

Abstract

Alkylphenols are nonbiodegradable metabolites arising from various pathways of aerobic and anaerobic degradation of the nonionic surfactants alkylphenol ethoxylates. A method based on the use of on-line solid-phase extraction (SPE) and liquid chromatography (LC) with UV detection was developed to determine bisphenol A, octylphenol, and nonylphenol at trace levels in water. The on-line coupled SPE procedure automatically enables an approximately 300-fold preconcentration of analytes, which can be further enhanced by an increase in applied sample volume. By using C18 cartridges, recoveries of >90% were obtained for all the analytes. A validation procedure was carried out with a groundwater sample to ensure the quality of the results; performance criteria such as detection limits (LODs), quantitation limits (LOQs), linearity, and precision were evaluated. LODs and LOQs in the range of 0.17-0.36 and 0.35-1.88 microg/L, respectively, were found; for all the analytes, linearity was established over 2 orders of magnitude (r2 >0.997, n = 54). The intraday repeatability values expressed as relative standard deviations were <5.3%; a nested analysis of variance was performed to verify the influence of 3 different factors, i.e., different days, extraction procedure, and LC replicate injection, on data precision.