Nitrazolam has been used as an example compound to demonstrate the microscale synthesis of reference materials utilizing polymer‐supported reagents. Nitrazolam is a designer benzodiazepine, There is growing evidence suggesting that such compounds have the potential to cause severe adverse events. Information about tolerability in humans is scarce but typically. Variability of the active ingredient in tablet formulations can also be of a concern. The unavailability of reference standards can impact on the ability to identify these compounds. The present study was triggered when samples of clonazolam were received in powdered and tablet form at a time when reference material for this drug was commercially unavailable.