An Alternate Testing Protocol to EPA 1613B for PCDD/Fs on an Agilent 8890–7010D GC/MS/MS: Performance Confirmation by Matrix Spikes and NIST SRM 2706New Organic Monitoring Techniques
Poster Presentation
Prepared by A. Cuthbertson, A. Andrianova, J. Ferrer
Agilent Technologies, 2850 Centerville Rd, Wilmington, DE, 19805, United States
Contact Information: [email protected]; 302-332-6928
ABSTRACT
We outline an isotope dilution GC/MS/MS workflow on an Agilent 8890 GC coupled to a 7010E triple quadrupole operating in multiple reaction monitoring mode (MRM) for the determination of the 17 toxic 2,3,7,8 substituted PCDD/F congeners as an alternate approach to EPA Method 1613B (SGS AXYS Method 16130). The method uses a 60 m DB 5 GC column and incorporates an Agilent Reference Compound Introduction Valve (RCIV) to introduce a low, continuous flow of PFTBA, enabling ongoing checks of ionization and transmission analogous to high-resolution mass spectrometry (HRMS) lock mass practices. Calibration, product ion ratio criteria, and instrument readiness checks are aligned with 1613B QA/QC expectations. Method performance was validated through matrix spike/duplicate experiments across representative matrices (e.g., water, solids, tissues) and by analyzing NIST Standard Reference Material (SRM) 2706 (New Jersey Soil) to establish trueness in a soil like matrix. Targets for linearity, sensitivity (relative to 1613B method reporting limits), and precision are informed by previously reported GC/TQ studies with this platform; with final validation with spike recoveries and agreement with SRM certificate or reference values. This work is intended to document a practical, lower complexity alternative to HRMS that can meet 1613B performance requirements when appropriate QA/QC measures are applied. Finally, we have developed a data reporting package that meets 1613B requirements including QA/QC checks (CC, LCS, MSD), and unknown estimated concentrations.
