Application of monolithic supports to online extraction and LC-MS analysis of benzodiazepines in whole blood samples.
A column-switching (CS) LC-MS method allowing high-speed determination of benzodiazepines (BZDs) in whole blood is presented. After protein precipitation with ACN followed by evaporation and reconstitution with the loading mobile phase, the online sample clean-up was carried out using a CS device. Two extractive precolumns were evaluated: a conventional restricted access material (RAM) sorbent and a monolithic silica support. Separation was achieved using a Chromolith Performance RP-18e (100 mmx4.6 mm id) monolithic silica column, and detection was performed by atmospheric pressure chemical ionization (APCI) MS. The method with both supports has been fully validated according to an accuracy profile approach. Finally, the monolithic silica column, demonstrating better validation data and a higher robustness than the RAM sorbent, was used for the analysis of several real forensic cases.
Bugey
Aurélie
A
Institute of Forensic Medicine, University of Geneva, Geneva, Switzerland.
Staub
Christian
C
D001569:Benzodiazepines / Q000097:blood*; D002853:Chromatography, Liquid / Q000295:instrumentation / Q000379:methods; D006801:Humans; D016014:Linear Models; D013058:Mass Spectrometry / Q000295:instrumentation / Q000379:methods*; D012016:Reference Values; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D013997:Time Factors
D001569:Benzodiazepines