Reference measurement procedure for Δ9-tetrahydrocannabinol in serum
An isotope dilution gas chromatography/mass spectrometry (ID-GC/MS) reference measurement procedure for Δ9-tetrahydrocannabinol (THC) in serum was developed and validated. The method complies with the concept of a ratio primary reference measurement procedure. The uncertainty was determined for two concentrations of THC in serum (1 ng/mL and 2.4 ng/mL). The calculation procedure is based on the Guide to the Expression of Uncertainty in Measurement (GUM). The relative expanded uncertainty was found to be less than 2% for both concentration levels, corresponding to a 95% confidence interval. For the reference method, it was shown that the measurement of THC within the concentration range covered by the current threshold values is very accurate. The method has the potential to provide traceability for the methods used in practical forensics.
GC–FID as a primary method for establishing the purity of organic CRMs used for drugs in sport analysis
Abstract The National Analytical Reference Laboratory has synthesized and characterized 67 anabolic steroid marker metabolites, both unlabelled and deuterated, and 37 key glucuronide and sulfate steroid conjugate pure substance reference materials. Work is also in process to establish their full traceability so that they can be issued as certified and primary reference materials. Both identity and purity have been rigorously characterized using a number of techniques and a primary method for purity assessment developed, based gas chromatography combined with flame ionization detection for the parent steroids and HPLC with evaporative light scattering detection for non-volatile steroid conjugates. Strategies for establishing traceability and for estimating measurement uncertainty are reported. The strategies described are considered applicable to a wide range of organic pure substance reference materials.
Primary methods of measurement and primary standards
The definition and concept of primary method are explained, taking examples from the fields of thermometry and measurements of amount of substance. It is shown that although few methods can be considered strictly primary, small departures from the strict definition can be quantified and useful practical primary methods are thus available. The links between primary methods of measurement, primary standards of measurement and primary reference materials are discussed.