Solid-phase micro extraction (SPME) and headspace derivatization of clenbuterol followed by GC-FID and GC-SIMMS quantification

Solid-phase micro extraction (SPME) and on fiber derivatization followed by Gas Chromatography coupled with Flame Ionization Detection (GC-FID) or Selected Ion Monitoring Mass Spectrometry (GC-SIMMS) allows for simple yet sensitive quantification for the hexamethyldisilazane derivative of the beta-agonist denbuterol. Using an 85-mum polyacrylate fiber, the analysis method is optimized with respect to extraction time, derivatization time and temperature, and solution pH. In addition, the use of a rapid temperature ramping injection port allows for optimization of fiber desorption conditions. Under optimal conditions, the limits of detection for the hexamethyldisilazane derivative of denbuterol are 1.1 ppb by FID and 0.20 ppb by SIMMS.