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Matrix-assisted laser desorption/ionisation time-of-flight/thin layer chromatography/mass spectrometry—a rapid method for impurity testing

✍ Scribed by Siew Mowthorpe; Malcolm R. Clench; Anna Cricelius; Don S. Richards; Vic Parr; Lee W. Tetler

Publisher
John Wiley and Sons
Year
1999
Tongue
English
Weight
108 KB
Volume
13
Category
Article
ISSN
0951-4198

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✦ Synopsis

Thin layer chromatography/matrix-assisted laser desorption/ionisation mass spectrometry (TLC/MALDI-MS) has been previously used to obtain mass spectra from a variety of compounds, principally peptides. For pharmaceutical compounds, which are often of relatively low molecular weight, it is important that any matrix materials employed do not interfere with the mass spectra obtained. The key step to successful TLC/ MALDI-MS is hence the preparation of the TLC plate prior to mass spectrometry. Crucial to this is the deposition of matrix material into the plate to promote co-crystallisation with the analyte. In this work we have examined the literature methods for plate preparation and developed two new approaches. The first involves brushing the TLC plate with a supersaturated solution of matrix and the second involves electrospraying the TLC plate with a matrix solution. Data are presented from the direct analysis of tetracycline and its impurities. Using the electrospray method the limit of detection for tetracycline is 1 ng from a TLC plate. A commercial MALDI-TOF mass spectrometer has been modified to allow the acquisition of chromatographic data from TLC plates. Chromatograms from replicate spots of 100 and 1 mg of tetracycline are shown.

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