Development of certified reference material of 1-(5-fluoropentyl)-N-(2-phenylpropan-2-yl)-1H-pyrrolo[2,3-b]pyridine-3-carboxamide (5F-CUMYL-P7AICA) to establish metrological traceability with mass balance and quantitative nuclear magnetic resonance spectroscopy

1-(5-Fluoropentyl)-N-(2-phenylpropan-2-yl)-1 H -pyrrolo[2,3- b ]pyridine-3-carboxamide (5F-CUMYL-P7AICA) represents a novel class of synthetic cannabinoids (SCs), constituting one of the most rapidly evolving groups of new psychoactive substances (NPS) that have been widely abused in recent years. However, precise qualitative analysis and accurate quantification pose significant challenges due to the lack of reference materials (RM) available for forensic drug prohibition and sentencing judges. Consequently, RM or certified reference materials (CRM) are essential for ensuring exact measurements and traceability of results in chemical analyses. The pure 5F-CUMYL-P7AICA candidate was autonomously synthesized through a two-step reaction process and subsequently purified via two-column chromatography. Two quantitative analytical methods were employed during the assessment of the pure 5F-CUMYL-P7AICA: quantitative nuclear magnetic resonance spectroscopy of hydrogen ( 1 H qNMR) method and mass balance (MB) method. For the 1 H qNMR, the mass fraction value reached 99.86% which could be traced back to the internal standard (benzoic acid). For the MB methods, the mass fraction value was 99.90% while the structurally related impurities of the candidate (0.05%), inorganic impurities (0.000006%), water (0.05%), and volatile organic solvent (0, or not detected) have been subtracted. Finally, the certified value was assigned to 99.9%, with an expanded uncertainty of 0.3% ( k  = 2). Furthermore, the application of CRM would be finished in our subsequent work, and we anticipate that this high-purity CRM could play an essential role in the field of forensic science and sentencing judgement.