GC-FID as a primary method for establishing the purity of organic CRMs used for drugs in sport analysis

The National Analytical Reference Laboratory has synthesized and characteri zed 67 anabolic steroid marker metabolites, both unlabelled and deuterated, and 37 key glucuronide and sulfate steroid conjugate pure substance refere nce materials. Work is also in process to establish their full traceability so that they can be issued as certified and primary reference materials. B oth identity and purity have been rigorously characterized using a number o f techniques and a primary method for purity assessment developed, based ga s chromatography combined with flame ionization detection for the parent st eroids and HPLC with evaporative light scattering detection for nonvolatile steroid conjugates. Strategies for establishing traceability and for estim ating measurement uncertainty are reported. The strategies described are co nsidered applicable to a wide range of organic pure substance reference mat erials.