Method Validation of Automated Workflows for Persistent Organic Pollutants (POPs) Analysis in Environmental and Food Matrices

New Organic Monitoring Techniques
Poster Presentation

Prepared by T. Hall, R. Addink
Fluid Management Systems, 900 Technology Park Dr, Billerica, Massachusetts, 01821, United States

Contact Information: [email protected]; 617-393-2396


Persistent organic pollutants (POPs) such as polychlorinated dibenzo-p-dioxins (PCDDs), furans (PCDFs) and biphenyls (PCBs) continue to attract interest around the world due to strict regulations in force in many countries. Rapid extraction, sample clean up, and analysis are therefore needed for many laboratories processing samples for POPs.

This study presents the automation of the complete workflow of PCDD/F and PCB extraction, cleanup, and concentration/evaporation. Automated Pressurized Liquid Extraction (PLE) and Semi Automated Sample column cleanup (using a vacuum pump to do all of the column chromatography steps) have been combined with automated sample concentration while extraction and cleanup are going on. State-of-the-art Triple Quadrupole GC/MS/MS analysis assures rapid and sensitive analysis. The work presented here followed US EPA methods 1613B (PCDD/Fs) and 1668C (PCBs).

The workflows with the automated systems are very time efficient, making same-day results possible.

A full validation of methods was run with demonstration of capability, method detection limits, 13C isotope dilution standards recoveries and various matrices.

Demonstration of capability yielded excellent recoveries of native spikes between 90-110% and RSDs < 6%. MDL studies showed values for the various dioxins and PCBs between 1-4 ppt. Recoveries of 13C isotope dilution standards were between 75-105% with RSDs < 10%.

Extraction, clean up and analysis by properly trained personnel can be carried out in one day, resulting in low turnaround times, with excellent results.