Screening of citalopram, fluoxetine and their metabolites in human urine samples by gas chromatography-mass spectrometry. A global robustness/ruggedness study.

ABSTRACT

Capillary gas chromatography with mass spectrometry detection in SIM mode (GC-MS-SIM) has been used for the analysis of citalopram (CIT), fluoxetine (FLX), and all of their metabolites in urine samples. The instrumental parameters affecting GC separation and MS-SIM detection were investigated. A validation procedure was performed on urine matrix and a simultaneous robustness/ruggedness evaluation is also presented in this paper. An optimized solid-phase extraction (SPE) has been applied, reaching in this way to limits of detection (LODs) between 0.7 ng L(-1) (CIT) and 33.6 microg L(-1) (CIT-PA). A pharmacokinetic screening in clinical urine samples has been also carried out.