Combined thin layer chromatography/mass spectrometry: An application of252Cf plasma desorption mass spectrometry for drug monitoring

Abstract

The pharmacokinetic analysis is performed in a three-step procedure: sample extraction, sample purification by thin layer chromatography (TLC) and quantitative sample detection by time-of-flight (TOF) mass spectrometry. 252Cf plasma desorption (PD) mass spectrometry utilizing the fission fragment-induced ionization and desorption of non-volatile compounds is suitable as a universal, non-destructive detector in TLC. Here TLC and mass spectrometry are operated in an off-line combination. As an example some pharmacokinetic data for etoposide (VP 16-213) together with calibration data are presented. The new experimental method is discussed in terms of sensitivity and detection limit.

Plasma desorption mass spectrometry: coming of age

“…In addition to their more fundamental studies, the group at Orsay (and the Curie Institute) used the PDMS technique for the analysis of nucleic acids modified by carcinogenic polycyclic hydrocarbons (24). An LC/PDMS system was developed at Marburg (25), where PDMS was also used in conjunction with thinlayer chromatography to investigate the pharmacokinetics of the antitumor drugs etoposide and teniposide (26). The Uppsala group reported the first PDMS mass spectrum of bovine insulin using 127I+2°ions from a tandem ac-celerator (27).…”

Thin-Layer Chromatography/Laser-Induced Acoustic Desorption/Electrospray Ionization Mass Spectrometry

“…Desorption ionization (DI) techniques, such as fast atom bombardment (FAB), secondary ion mass spectrometry (SIMS), laser desorption (LD), and matrix-assisted desorption ionization (MALDI), have been used to characterize nonvolatile or thermally labile compounds directly on TLC plates. [12][13][14][15][16][17] Nevertheless, several problems are still encountered when using these approaches: (1) time and labor consumption, due to the requirement of a high vacuum for the ion source; (2) poor sensitivity for the detection of volatile or semivolatile compounds;…”

Interfaces To Connect Thin-Layer Chromatography with Electrospray Ionization Mass Spectrometry

“…Mass spectrometric methods for detecting compounds directly from intact TLC plates have attracted particular interest because they provide fast and automated analyses . For example, analytes have been volatilized directly inside the ion source using direct electron impact and chemical ionization probes. , Furthermore, desorption/ionization techniques such as fast atom bombardment, plasma desorption, laser desorption, and matrix-assisted laser desorption/ionization (MALDI) also have been used to analyze compounds separated by TLC. − Although desorption/ionization techniques (e.g., MALDI) have been attempted for in situ detection of various types of analytes on TLC plates, previous experiments with direct TLC/MS have been limited to off-line analysis. Additionally, for sensitive desorption/ionization analyses of intact TLC plates, the analytes should be concentrated close to the surface of the TLC gel.…”