Interlaboratory Comparison of a Biomimetic Extraction Method Applied to Oil Sands Process-Affected Waters

Biomimetic extraction using solid-phase microextraction is a passive sampling analytical method that can predict the aquatic toxicity of complex petroleum substances. The method provides a nonanimal alternative to traditional bioassays with the potential to reduce both vertebrate and invertebrate aquatic toxicity testing. The technique uses commercially available polydimethylsiloxane-coated fibers that, following nondepletive extraction of water samples, are injected into a gas chromatograph with flame ionization detection. As the predictive nature of the method is operationally defined, it is critical that its application be harmonized with regard to extraction, analysis, and standardization parameters. Results are presented from a round robin program comparing the results from 10 laboratories analyzing four different sample sets of dissolved organics in water. Samples included two incurred oil sands process-affected waters and a cracked gas oil water accommodated fraction. A fourth sample of cracked gas oil blended in an oil sands process-affected water was analyzed to demonstrate the method's ability to differentiate between neutral and ionizable dissolved hydrocarbons. Six of the 10 laboratories applied an automated version of the method using a robotic autosampler where the critical extraction steps are precisely controlled and which permits batch screening of water samples for aquatic toxicity potential. The remaining four laboratories performed the solid-phase microextraction manually. The automated method demonstrated good reproducibility with between-laboratory variability across the six laboratories and four samples yielding a mean relative standard deviation of 14%. The corresponding between-laboratory variability across the four laboratories applying the manual extraction was 53%, demonstrating the importance of precisely controlling the extraction procedure. Environ Toxicol Chem 2022;41:1613-1622. © 2022 The Authors. Environmental Toxicology and Chemistry published by Wiley Periodicals LLC on behalf of SETAC.