Optimization of solid-phase extraction for a liquid chromatographic–tandem mass spectrometric general unknown screening procedure by means of computational techniques

• Published in: Journal of Chromatography A 2004-11, Vol.1056 (1), p.57-65
• Main Authors: Decaestecker, Tineke N., Lambert, Willy E., Van Peteghem, Carlos H., Deforce, Dieter, Van Bocxlaer, Jan F.
• Format: Article
• Language: English
• Subjects: Analytical chemistry; Chemistry; Chromatographic methods and physical methods associated with chromatography; Chromatography, Liquid - methods; Exact sciences and technology; Experimental design; Forensic Sciences; General unknown screening; Information-dependent acquisition; Mass Spectrometry - methods; Other chromatographic methods; Reproducibility of Results; Screening; Solid-phase extraction
• ISSN: 0021-9673
• DOI: 10.1016/j.chroma.2004.06.010

A solid-phase extraction (SPE) method was optimized to suit the particular demands of an information-dependent acquisition LC–MS–MS procedure for general unknown screening in a forensic toxicology setting. In a first phase, a Plackett–Burman screening design with fold-over was carried out to distinguish the significant factors affecting the extraction procedure. This part eventuated in the determination of only three statistically relevant parameters, requiring consecutive optimization. To that end, in phase II of this study, a rotatable central composite design was applied to define the response surface as a function of the significant parameters and to choose the optimal conditions for the SPE.