Analysis of OSPAR priority pharmaceuticals using high-performance liquid chromatography-electrospray ionisation tandem mass spectrometry

The occurrence and potential adverse effects of pharmaceutical compounds in the aquatic environment have received much scientific interest. Presented are analytical methodologies for the determination of 10 of the pharmaceuticals listed on the Oslo and Paris Commission for the protection of the Marine Environment of the North East Atlantic (OSPAR) hazardous substances website. In addition to these 10 substances, the chemical fluoxetine (Prozac) was also investigated. The performance characteristics of a combined solid phase extraction (SPE) isolation and high-performance liquid chromatography-electrospray ionisation tandem mass spectrometry (HPLC-ESI-MS/MS) procedure have been determined. Extraction efficiencies were obtained for a variety of SPE sorbents, following this initial investigation. Strata-X (Phenomenex, UK) was selected for further development. The extraction method performed satisfactorily for the majority of the 11 compounds analysed, with recoveries of over 60% for most of the compounds and relative standard deviations of between 4 and 13%. The recoveries of chloroquine and closantel were below 50% but the method provides semi-quantitative information regarding the occurrence of these compounds. Separation of the analytes was made using a C18 Luna analytical column (Phenomenex, UK) and mass spectra were obtained using an ion trap mass spectrometer operated in both positive and negative electrospray ionisation modes. Limits of detection for all compounds ranged from 1 to 20 ng/l, making the method suitable for low level environmental analysis. Of the selected surface water and treated sewage effluent samples (n = 6) analysed, chlorpromazine, fluoxetine and miconazole were detected in concentrations ranging from 7 to 34 ng/l. The chemicals determined using this procedure fall into a variety of pharmaceutical classes including antipsychotics and tranquilisers resulting in an analytical method that contains compounds from diverse chemical classes.