Derivatization of alkaloids for gas chromatography

A new method for the rapid separation of alkaloids, inter alia atropine, has been elaborated, using chromatography on paper that is impregnated with zirconium oxide.57 Cation-exchange h.p.l.c. analysis of tropane alkaloids has been developed,58 followed by post-column derivatization using the fluorimetric ion-pair technique.58,59 Gas chromatography of tropanes has been reviewed.60... 

In recent years several sensitive and specific methods for the simultaneous determination of ephedrine alkaloids in plant material have been published. These include thin-layer chromatography (292,426), gas chromatography (251), straight-phase and reversed-phase high-performance liquid chromatography (253, 255, 302, 355, 427), isotachophoresis (303, 356), and 13C-NMR (304). Resolution of enantiomeric alkaloids by HPLC has been achieved on chiral stationary phases (417, 418) or after derivatization with a chiral agent on an achiral stationary phase (419). Chromatographic separation and analytical detection of... 

Floberg et al. applied glass capillary gas chromatography for the analysis of theophylline and caffeine in plasma. The alkaloids were analyzed as such, or after derivatization. 

Insufficient volatility and thermal stability are the biggest challenges in the application of gas chromatography for the analysis of steroids. The development of gas chromatography (GC) methods for steroids analysis should take in consideration thermal stability, the derivatization step to increase volatility, the stationary phase, and the detector. Several GC methods have been summarized for the analysis of various steroids including anabolic steroids, brassinosteroids, corticoids, estrogen, endocrine-disrupting chemicals, neurosteroids, sterols, steroid saponins, and steroid alkaloids. 

HPLC analysis for pharmaceutical preparations of alkaloids started about 30 years ago. Gas chromatography (GC) is suitable for volatile compoxmds and requires laborious derivatization. Thus, GC is unsuitable to analyze the bisindole alkaloids due to their high boiling point. HPLC can provide better analytical precision and higher sample loading capacity. HPLC methods coupled to UV and MS detection have been applied for the determination of the active compounds in Catharanthus roseus. 

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