Development of a Complete Method validation for the use of Solidphase Extraction with EPA 625.1

Advances in Sample Preparation and Clean-up
Oral Presentation

Presented by T. Hall
Prepared by P. Bassignani, R. Addink, R. Juma
Fluid Management Systems, Inc., 580 Pleaseant Street, Watertown, MA, 02472, United States


Contact Information: pbassignani@fms-inc.com; 617-393-2396


ABSTRACT

With the acceptance of Solid Phase Extraction as a viable alternative to LLE for the analysis of semi-volatile organic compounds in waste water matrices, there is a demand for reliable and proven processes for environmental lab to easily adopt. The need for fully validated protocols and robust standard operating procedures is vital for labs to be able to rapidly incorporate any new methodology with the least amount of overhead.

Using the FMS an automated SPE system, a complete data validation protocol has been developed for EPA 625.1 that can be reference and easily incorporated by testing labs wishing to make the transition from LLE to SPE. The validation protocol compromises the initial start up of IDC and MDL runs, various real world and synthetic matrix verification, PT data for all required analytes, and a complete reference SOP. Runs for full 1 liter samples as well as low sample volume runs for all matrices tested are available, as well as analysis on various Mass Spec platforms.

Specific detail is provided on dealing with real world waste water samples, particularly samples with high amounts of organic particulate matter. Direct comparisons with such matrices between LLE and SPE extracts like emulsion formulation and water separation are also made demonstrating the issues SPE solves with trouble sample matrices.