Determination of barbiturates by solid-phase microextraction (SPME) and ion trap gas chromatography–mass spectrometry

Abstract

Solid-phase microextraction (SPME) in conjunction with quadrupole ion trap GC–MS was applied to the determination of a series of barbiturates. A 65 μm Carbowax–divinylbenzene (DVB) SPME fiber was used to successfully extract a series of eight barbiturates from aqueous solution. Absorption kinetics and distribution coefficients for the 65 μm Carbowax–DVB SPME fiber were determined for the compounds. In addition the method was evaluated with respect to linearity, limit of detection, precision, desorption time, and the effect of salt. Limits of detection reached 1 ng/ml for the barbiturates. Linearity was established for the barbiturates over a concentration range of 10–1000 ng/ml, with coefficients of correlation 0.99. Overall, the precision of the method fell between 2.2%–6.5%, depending on the barbiturate. SPME was applied to the identification and quantitation of the barbiturates in a urine matrix. The method was validated by analyzing a reference standard pentobarbital-spiked urine sample. Both standard addition and internal standard with [2H5]-pentobarbital techniques were evaluated, with recoveries found to be 93% and 104%, respectively. SPME was then used to rapidly screen a urine specimen tested positive for barbiturates, and butalbital was detected and quantified.