Results of the preliminary study into the use of the diazepam MISPE for the detection of benzodiazepines in post-mortem hair samples has shown that it can be applied successfully for this purpose. The MISPE is selective for diazepam metabolites and other benzodiazepine analogues. The MISPE method appears to be significantly more streamlined than the SPE method, providing a simpler and more time efficient procedure. MISPE demonstrated higher percentage extraction recoveries for six out of nine analytes whereas SPE achieved lower limit of detection (LOD) values for six out of nine analytes. Diazepam was the most frequently detected, followed by its metabolite nordiazepam. In general, benzodiazepine levels were in the ranges reported in previous literature. Nordiazepam was always detected at a higher concentration then diazepam, a finding that is consistent with other studies. Oxazepam was detected only in two samples. A possible reason for this little detection rate may be that oxazepam has a relatively short half-life compared to nordiazepam, and is a polar compound which may not incorporate readily into hair, and could be present at low levels as a diazepam metabolite, rather than as the parent drug. Temazepam levels have not been reported widely in hair. The levels detected in this study were within a relatively narrow concentration range of 0.16-0.24 ng/mg. Nitrazepam levels detected in one sample by MISPE and SPE were higher than reported in another study. The hair samples selected for testing were from drug-related deaths where a positive benzodiazepine blood result was obtained. Tables, figures, references