Abstract
BackgroundKhat (Catha edulis Forsk) is an evergreen shrub of the Celastraceae family. It is widely cultivated in Yemen and East Africa, where its fresh leaves are habitually chewed for their momentary pleasures and stimulation as amphetamine-like effects. The main psychostimulant constituents of khat are the phenylpropylamino alkaloids: cathinone, cathine and norephedrine.ResultsIn this study, simple procedures based on preparative HPLC and salting-out assisted liquid–liquid extraction (SALLE) based methods were developed respectively for large scale isolation and the extraction of psychoactive phenylpropylamino alkaloids; cathinone, cathine and norephedrine, from khat (Catha edulis Forsk) chewing leaves, a stimulant and drug of abuse plant. The three khat alkaloids were directly isolated from the crude oxalate salt by preparative HPLC–DAD method with purity > 98%. In addition, a modified (SALLE) method has been developed and evaluated for the extraction efficiency of psychoactive phenylpropylamino alkaloids from khat (Catha edulis Forsk) chewing leaves. An in situ two steps extraction protocol was followed without dispersive SPE clean up. The method involves extraction of the samples with 1% HAc and QuEChERS salt (1.0 g of CH3COONa and 6.0 g of MgSO4) followed by subsequent in situ liquid–liquid partitioning by adding ethyl acetate and NaOH solution. The optimized method allowed recoveries of 80–86% for the three alkaloids from khat sample with relative standard deviation (RSD) values less than 15% and limits of detection (0.85–1.9 μg/mL).ConclusionThe method was found to be simple, cost-effective and provides cleaner chromatogram with good selectivity and reproducibility. The SALLE based protocol provided as good results as the conventional extraction method (ultrasonic assisted extraction followed by solid phase extraction, UAE–SPE) and hence the method can be applicable in forensic and biomedical sectors.
Highlights
Khat (Catha edulis Forsk) is an evergreen shrub of the Celastraceae family
The aim of the present work was to optimize preparative high performance liquid chromatography (HPLC) method for the simultaneous isolation of the three khat alkaloids from khat extract; and to modify and develop the conventional salting-out assisted liquid–liquid extrac‐ tion (SALLE) extraction protocol for the analysis of psychoactive phenylpropylamino alkaloids from khat (Catha edulis Forsk) chewing leaves
Isolation of the three khat alkaloids from the oxalate salt of crude extract Originally the concentrated aqueous extract was supposed to be used for the preparative HPLC–DAD isolation protocol
Summary
Khat (Catha edulis Forsk) is an evergreen shrub of the Celastraceae family. It is widely cultivated in Yemen and East Africa, where its fresh leaves are habitually chewed for their momentary pleasures and stimulation as amphetamine-like effects. The main psychostimulant constituents of khat are the phenylpropylamino alkaloids: cathinone, cathine and norephedrine. Khat (Catha edulis Forsk) is an evergreen shrub of the Celastraceae family. It is widely cultivated in Yemen and East Africa, where its fresh leaves are habitually chewed for their momentary pleasures and stimulation as amphetamine-like effects. The main psychostimulant constituents/compounds of khat are the phenylpropylamino alkaloids: (−)-cathinone [(S)-α-aminopropiophenone], (+)-cathine [(1S) (2S)-norpseudoephedrine], and (–)-norephedrine [(1R) (2S)-norephedrine] (Fig. 1). There are more than 200 identified compounds in khat leaves, the phenylpropylamino alkaloids are primarily considered to be the addictive and reinforcing agents responsible for continued chewing behavior [5, 6]
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