Analysis of organophosphorus flame retardants in environmental and biotic matrices using on-line turbulent flow chromatography-liquid chromatography-tandem mass spectrometry

A fast on-line analytical method based on turbulent flow chromatography (TFC) in combination with tandem mass spectrometry (MS-MS) has been applied for the analysis of fourteen organophosphorus flame retardants (OPFRs) in sediment and fish samples. Applying this technique, time-consuming sample preparation steps were eliminated. The extraction was performed by ultrasound liquid extraction for biota and by pressurized liquid extraction for sediments. After extraction, environmental and biotic extracts were directly injected to the chromatographic system and analytes were concentrated into the cleanup loading column. Thereafter, analytes were transferred into the analytical column for subsequent detection by MS-MS. Analytical parameters showed acceptable recoveries (between 47 and 112% for sediment, and between 47 and 98% for fish) with very low relative standard deviations (always below 8.8% for sediment, and below 16% for fish). Moreover, mLODs and mLOQs are similar or even lower than those reported in other works using off-line methodologies. mLODs ranged between 0.02 and 1.25 ng/g dry weight (dw) and between 0.19 and 19.3 ng/g lipid weight (lw) for sediments and fish samples, respectively. The applicability of the developed methodology was demonstrated by the analysis of real samples, corresponding to river sediments as well as river and marine fish samples. OPFRs were detected in all samples, with values up to 549 ng/g dw, 15.8 ng/g lw and 646 ng/g lw for sediment, marine fish and river fish, respectively.