A Low Solvent Extraction and Zero DCM Sample Cleanup for POPs Analysis

Jun 01, 2017
By FMS
Volume 35, Issue 6

Persistent organic pollutants (POPs) such as polychlorinated dibenzo-pdioxins (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 cleanup, and analysis is needed for many laboratories processing samples for POPs. In addition to processing times, solvent use is an important consideration as the cost of sample clean up involving large amounts of solvents can be very high.


Table I: PCDD/F and co-planary PCBs 13C recoveries across cleanup - fish oil and fatty acid used as such, no extraction

A newly developed automated sample extraction and cleanup system, which allows for rapid extraction of the sample (time approximately one hour) and fast cleanup (30 min). Solvent consumption is limited to 110–200 mL depending on lipid content and no dichloromethane is used during the cleanup step. The fully automated system allows for sample turnaround times of only a few hours and same day analysis and results.


Table II: mono- and di-ortho PCBs 13C recoveries across cleanup - fish oil and fatty acid used as such, no extraction

Instrumentation

  • FMS, Inc. PLE®/Low Solvent (LS) EP110™
  • FMS, Inc. SuperVap® Concentrator
  • HRMS®

Consumables

  • FMS, Inc. High Capacity Acid-Base-Neutral Silica column
  • FMS, Inc. Mini Acid-Base-Neutral Silica column
  • FMS, Inc. Mini Basic Alumina column

Pressurized Liquid Extraction

  • Sample placed in extraction cell
  • Capped with disposable Teflon end caps
  • Heated with 50% Dichloromethane/50% Hexane for 20 min at 120 °C and 1500 psi
  • Nitrogen flush to transfer analytes and extract direct to the SuperVap 250 mL collection tubes

SuperVap Concentration

  • Temperature: 45 °C

EconoPrep Cleanup

  • Silica -carbon - alumina columns are used
  • Uses only hexane and toluene for 5-step program
  • Load sample in hexane
  • Elute silica column with hexane
  • Elute carbon in reverse (upward) direction with toluene (collect PCDD/F and co-planary PCBs)
  • Elute alumina in reverse direction with toluene (collect mono-ortho and di-ortho PCBs)

Conclusions

The integrated PLE/Low Solvent Zero DCM EconoPrep generates clean extracts in less than 2 h and generates consistent, reproducible recoveries for a number of matrices. It is a green option that cuts electrical costs. The system uses only a total volume of 110–200 mL of hexane and toluene. It uses zero dichloromethane for the cleanup step.

FMS, Inc.
580 Pleasant Street, Watertown, MA 02472
tel. (617) 393-2396, fax (617) 393-0194, [email protected]
Website: www.fms-inc.com

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