Published:Journal of Chromatographic Science, ISSN 0021-9665 Volume 45, Number 5, May/June 2007, pp.251-255

Simultaneous Determination of Caffeine, Ergotamine, and Metamizol in Solid Pharmaceutical Formulation by HPTLC–UV-FLD with Mass Confirmation by Online HPTLC–ESI-MS

Mario Aranda and Gertrud Morlock
Institute of Food Chemistry, University of Hohenheim, Garbenstrasse 28, 70599 Stuttgart, Germany

A new high-throughput method is developed to quantify caffeine, ergotamine, and metamizol in a solid pharmaceutical formulation. After dissolution, the compounds are separated on silica gel 60 F254 high-performance thin-layer chromatography (HPTLC) plates with ethyl acetate–methanol–ammonia 90:15:1 (v/v/v) as the mobile phase. Detection is performed by UV absorption at 274 nm for caffeine and metamizol, and by fluorescence at 313 /> 340 nm for ergotamine. Calibrations are linear or polynomial with determination coefficients (R2) ≥ 0.9986. Recoveries of the three compounds are between 95% and 102% at three different concentration levels. Repeatability [relative standard deviation (RSD)] of all substances in the matrix is between ± 0.9% and ± 1.7%. Intermediate precision (RSD) of the three compounds range from ± 2.0% to ± 3.1%. Mass confirmation is performed by a single quadrupole mass spectrometry in positive electrospray ionization full scan mode for caffeine and ergotamine and in negative mode for metamizol. The results proved that this method is a simple and reliable alternative for routine analysis.

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