A sustainable approach for the reliable and simultaneous determination of terpenoids and cannabinoids in hemp inflorescences by vacuum assisted headspace solid-phase microextraction

Abstract

• Headspace solid phase microextraction can be adopted for the recovery of terpenoids and cannabinoids from Cannabis sativa inflorescences. • Vacuum conditions in the Cannabis headspace ensure the recovery of cannabinoids with low sampling temperature and time. • The adoption of mild conditions allows to not discriminate volatile and semivolatile fractions. • The adoption of mild conditions decreases the formation of artefacts. • The separation of terpenoid and cannabinoids markers can be obtained in less than 30 min with short narrow bore columns. Cannabis sativa L. is an intriguing plant that has been exploited since ancient times for recreational, medical, textile and food purposes. The plant's most promising bioactive constituents discovered so far belong to the terpenoid and cannabinoid classes. These specialised metabolites are highly concentrated in the plant aerial parts and their chemical characterisation is crucial to guarantee the safe and efficient use of the plant material irrespective of which use it is. This study investigates for the first time the use of vacuum assisted HS-SPME as a sample preparation process in an analytical protocol based on HS-SPME combined to fast GC-MS analysis that aims at comprehensively characterising both the terpenoid and cannabinoid profiles of Cannabis inflorescences in a single step. The results proved that vacuum in the HS should be preferred over atmospheric pressure conditions as it ensures the fast recovery of cannabinoid markers at relatively lower sampling temperatures (i.e., 90°C) that do not discriminate the most volatile fraction nor cause the formation of artefacts when the sampling time is minimised.