Determination of pharmaceuticals of various therapeutic classes by solid-phase extraction and liquid chromatography–tandem mass spectrometry analysis in hospital effluent wastewaters

• Published in: Journal of Chromatography A 2006-05, Vol.1114 (2), p.224-233
• Main Authors: GOMEZ, M. José, PETROVIC, Mira, FERNANDEZ-ALBA, Amadeo R, BARCELO, Damia
• Format: Article
• Language: English
• Subjects: Adrenergic beta-Antagonists - analysis; Analytical chemistry; Anti-Bacterial Agents - analysis; Anti-Inflammatory Agents - analysis; Anticonvulsants - analysis; Antidepressive Agents - analysis; Applied sciences; Chemistry; Chromatographic methods and physical methods associated with chromatography; Chromatography, Liquid - methods; Exact sciences and technology; Hospital Bed Capacity, under 100; Hospital wastewaters; Liquid chromatography–tandem mass spectrometry; Medical Waste Disposal; Narcotics - analysis; Other chromatographic methods; Other wastewaters; Pharmaceutical Preparations - analysis; Pharmaceuticals; Pollution; Spectrometry, Mass, Electrospray Ionization - methods; Wastewaters; Water Pollutants, Chemical - analysis; Water treatment and pollution
• ISSN: 0021-9673
• DOI: 10.1016/j.chroma.2006.02.038

A multi-residue analytical method has been developed and validated for determining a selection of 16 pharmaceuticals: the anti-epileptic carbamazepine, seven analgesic/anti-inflammatory drugs (mefenamic acid, indomethacine, ibuprofen, naproxen, diclofenac, ketorolac and acetaminophen), the analgesic opiate codeine, two antidepressants (fluoxetine and paroxetine), β-blockers (atenolol and propranolol), antibiotic (trimethoprim, metronidazole, and erythromycin) and the anti-ulcer ranitidine in hospital effluent wastewaters. The method allows simultaneous extraction of the pharmaceuticals compounds by solid-phase extraction (SPE) using the Waters Oasis HLB at pH 7. The analytes were then identified and quantitatively determined by liquid chromatography–tandem mass spectrometry (LC–MS–MS) using multiple reaction monitoring (MRM). Recoveries of the pharmaceuticals were higher than 75%, with the exception of ranitidine (45%) and the overall variability of the method was below 9%. The instrumental detection limit (IDL) varied between 2 and 31 pg injected, the method detection limit (LOD) was between 7 and 47 ng/L in spiked hospital effluent. The precision of the method, calculated as relative standard deviation (RSD), ranged from 0.3 to 4.9%. A detail study off matrix effect is included in this work, regarding to signal suppression in these effluent wastewaters from a hospital complex samples. The developed analytical method was applied for preliminary data results in effluent wastewaters from a hospital.