Total Rapid Prep for Same Day Turnaround of POPs Analysis

The Application Notebook

The Application Notebook, The Application Notebook-06-01-2009, Volume 0, Issue 0

Human health not only depends on providing good medical care, but also on the priority given to prevent exposure to environmental and other health risks. Persistent Organic Pollutants (POPs) are organic compounds typically of anthropogenic origin that resist degradation and accumulate in the food chain and are associated with adverse effects on human health and the environment (1). Due to their toxicity to humans, at much lower concentration than other pollutants, it is important to monitor compounds like polychlorinated dioxins/furans PCDD/Fs, DLPCBs, BDEs, and PCNs. More sophisticated requirements are needed for their analysis. In the past, extraction and clean-up of POPs present in fish and biota samples were conducted with procedures such as Soxhlet extraction, acid digestion, and liquid-liquid extraction. The clean-up of these samples was accomplished through chromatographic columns using different types of adsorption media such as silica, alumina, and carbon. These analytical methods used for analysis..

Fluid Management Systems, Inc.

Human health not only depends on providing good medical care, but also on the priority given to prevent exposure to environmental and other health risks. Persistent Organic Pollutants (POPs) are organic compounds typically of anthropogenic origin that resist degradation and accumulate in the food chain and are associated with adverse effects on human health and the environment (1). Due to their toxicity to humans, at much lower concentration than other pollutants, it is important to monitor compounds like polychlorinated dioxins/furans PCDD/Fs, DLPCBs, BDEs, and PCNs. More sophisticated requirements are needed for their analysis. In the past, extraction and clean-up of POPs present in fish and biota samples were conducted with procedures such as Soxhlet extraction, acid digestion, and liquid-liquid extraction. The clean-up of these samples was accomplished through chromatographic columns using different types of adsorption media such as silica, alumina, and carbon. These analytical methods used for analysis not only pose risk through human exposure, but are also typically labor intensive and time consuming, with high costs.

Automated Extraction and Clean-Up

Automated extractions were performed on the FMS PLE system. Six samples are extracted simultaneously. The extracted sample was then concentrated to ~ 1 ml. The extract is diluted to ~35 ml with Hexane to start the clean-up procedure. The clean-up procedure was carried out with the Power-Prep system using pre-packed FMS columns for the fractionation of the target compounds.

Results and Discussion

Method development studies have produced accurate results using real fish samples (see Figure 1). Results are well within the acceptable range for the analytes of interest. Analysis of contaminated natural matrix reference material yielded good recoveries for the method. The method is able to separate the planar compounds – dioxins/furans, nonortho-PCBs, and PCNs into one fraction and non-planar compounds – BDEs and mon-ortho PCBs into another fraction using the FMS columns. All tests carried out during method development studies included Spiked Procedure Blanks (SPBs) for QC purposes. No significant differences were observed between blanks values and the PLE and Power-Prep Systems.

Figure 1

Conclusions

The automated extraction of a sample for PCDDs/PCDFs, DLPCBs, PCNs, and BDEs in fish and biota matrices in one extraction followed by an automated clean-up can save time, solvent, cost, and lower the possibility of any health hazards. The automated extraction is less labor-intensive and can run parallel samples unattended. The overall process for this method between extraction and cleanup has demonstrated the ruggedness, accuracy, repeatability, and a significant increase in productivity for sample extraction/preparation by reducing the time of sample preparation from about 4–5 working days for each target analyte group to 4 working days for all four POPs in single extraction. Also, this method has lower method detection limits than the separate methods, especially for the PCDD/F, DLPCBs, and the PCNs and greater analytical precision and increased surrogate recoveries for BDEs. See the full application note on the FMS website.

Special thanks to Laila Fayez at the Ontario Ministry of the Environment, Laboratory Services Branch, Toronto, ON, M9P3V6 Canada for sharing their work.

Fluid Management Systems, Inc.

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Website: www.fmsenvironmental.com