Development and application of a novel method for high‐throughput determination of PCDD/Fs and PCBs in sediments

Abstract

A selective pressurized liquid extraction technique was developed for the simultaneous extraction of polychlorinated dibenzo-p-dioxins/dibenzofurans (PCDD/Fs) and dioxin-like polychlorinated biphenyls (dl-PCBs) from contaminated sediments. The final method incorporated cleanup adsorbents (Florisil, alumina, and silica) into the extraction cell in a 1:1 ratio of matrix to individual adsorbent (w/w). Sulfur, a common interference found in sediments, was successfully removed by placing activated copper in the extraction bottle prior to extraction. No additional postextraction cleanup was required, and sample throughput was reduced to 2.5 h per sample. Target analytes were quantified using high-resolution gas chromatography/electron-capture negative ionization mass spectrometry and verified by high-resolution gas chromatography/high-resolution mass spectrometry. Though mean analyte recoveries (n = 3) of PCDD/Fs and dl-PCBs were 84 ± 5.8% and 70 ± 8.4%, respectively, mean surrogate recoveries for all PCDD/Fs using this novel method were greatly improved compared with US Environmental Protection Agency (USEPA) method 1613 (∼25-155%) and USEPA method 8290a (40-135%). After development, the method was used to examine surficial sediment samples from the San Jacinto River waste pits, a Superfund site in Houston, Texas, USA. In all samples, PCDD/Fs and dl-PCBs were detected, and the contaminant concentrations ranged over 5 orders of magnitude.

Pressurized liquid extraction of organic contaminants in environmental and food samples

“…It can be also placed in the collection bottle after PLE extraction with good results, as demonstrated by Aguilar et al [1]. This novel method, schematized in Fig.3 In-cell clean-up was also reported, for the detection of five benzotriazols (light stabilizers) in indoor areas [48].…”

“…PLE has been mostly applied to extract persistent organic pollutants in environmental samples [1,16,23]. In most cases, hexane and dichloromethane were used, because they are able to provide quantitative recoveries of the analytes.…”

“…Use of PLE has increased since its acceptance as an official US Environmental Protection Agency (USEPA) method for persistent organic pollutants in many environmental solid samples [1]. This approach is already a routine technique for trace analysis of organic contaminants, utilized in many laboratories due to its easy manipulation, short extraction time, low sample amount requirements and good performance.…”

“…Accelerated solvent extraction cell with cleanup adsorbents for finalized SPLE of polychlorinated dibenzo-p-dioxins/dibenzofurans and dioxin-like polychlorinated biphenyls from sediments (Reproduced from[1] with permission of SETAC press) Representative time frame of overlaid full scan total ion chromatograms using GC-MS EI from five individually examined adsorbents at a 10:1 adsorbent to gray whale cerumen mass ratio. Florisil ® was finally chosen to reduce bulk matrix interferences (Reproduced from[51] with permission of Elsevier).…”

Contaminated Aquatic Sediments

“…A selective pressurized liquid extraction technique was developed for the simultaneous extraction of polychlorinated dibenzo-p-dioxins/dibenzofurans (PCDD/Fs) and dioxin-like polychlorinated biphenyls (dl-PCBs) from contaminated sediments (Aguilar et al, 2014).…”