Novel method for extraction and quantitation of 6PPD-Q in solid matrices using ultrasonic-assisted extraction (UAE)...

This study presents a UAE-LC-MS/MS method for the extraction and quantitation of 6PPD-Q in stormwater sediment matrices. The final method uses ultrasonic-assisted extraction with a hexane:ethyl acetate solvent system and LC-MS/MS instrumental analysis with matrix-matched calibration, and demonstrated acceptable sensitivity, selectivity, and reproducibility. This study addressed challenges specific to sediment matrix, a lack of commercially available reference material, and co-extracted chromatographic interferences. Matrix effects were reduced through optimized extraction parameters, rather than post-extraction cleanup procedures. A total of 28 sediment samples were analyzed using LC-MS/MS to evaluate 6PPD-Q concentrations, resulting in values ranging from 11.4 ng/g to 691 ng/g, with a mean value of 171 ng/g. The method achieved a method detection limit of 1.1 ng/g and limit of quantitation of 5 ng/g using a 250 mg sample size. The mean recovery rate of 6PPD-Q in laboratory control samples was 80.1% (range: 74.8% - 82.3%).•Extract sediment sample with hexane:ethyl acetate mix and dry.•Reconstitute with acetonitrile.•Analyze using LC-MS/MS.