Solid Phase Extraction Purification of Saliva Samples for Antipsychotic Drug Quantitation

Abstract

Saliva is far less popular as a diagnostic material than blood. This has resulted in a lack of procedures for the sampling and handling of saliva, e.g., effective ways to purify endogenous compounds from saliva to enable a simultaneous determination of xenobiotics such as neuroleptics. Therefore, the aim of this study was to develop an analytical procedure to purify saliva samples so that it is then possible to simultaneously determine five neuroleptics (aripiprazole, clozapine, olanzapine, quetiapine and risperidone) and the antiepileptic drug carbamazepine, and their respective metabolites (dehydroaripiprazole, N-desmethylclozapine, N-demethylolanzapine, norquetiapine, 9-OH-risperidone and carbamazepine-10,11-epoxide). A study of three types of solid-phase extraction (SPE) columns showed that the purest eluates were obtained using columns containing ion exchange sorbent. The sorbents were first washed with water then with a mixture of water and methanol (1:1), and the adsorbed residue was eluted with a 5% ammonia solution in methanol. Saliva samples for SPE were diluted with 2% formic acid and a mixture of methanol and water (1:1). This procedure was developed to purify a saliva sample spiked with a mixture of neuroleptics and carbamazepine, and their respective metabolites. A chromatographic analysis confirmed the isolation of all compounds, indicating that this procedure can be used in further development and validation for a method designed to monitor the levels of neuroleptic drugs in saliva and to monitor their uptake by patients.