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HPLC-MS determination of pharmaceuticals in wastewaters

In recent years, the occurrence and the fate of pharmaceutically active compounds in the environment (water, soil, sediments and sludges) has been recognized as one of the prevailing problems in ecological risk assessment and chemistry. [1] Theirs low concentrations normally present (low ng/L) in environment, the complexity of environmental matrices and the diverse physico-chemical properties make their determination difficult. It is very important and is quite necessary to have highly sensitive, selective methods for monitoring pharmaceuticals in the environment. [2] Liquid chromatography coupled to mass spectrometry especially multidimensional mass spectrometry (LC-MSn) provides a powerful alternative, combining rapidity, specificity and sensitivity. [3] The aim of this work was to develop a SPE-HPLC-ESI(+)-MS analytical method for determination pharmaceuticals in wastewater. Investigated pharmaceuticals, which belong different classes of antimicrobials, are sulfonamides (sulfaguanidine, sulfadiazine, sulfamethazine and sulfametoxazole), a sulfonamide synergist from diaminopyrimidine class (trimethoprim), fluoroquinolones (ciprofloxacin, enrofloxacin and norfloxacin), a diphenylsulfide (febantel), a hexahydropyrazine (praziquantel), an anesthetic (procaine) and macrolide (roxithromycin). HPLC-ESI(+)-MS separation was examined on Varian ProStar instrument with gradient elution of mobile phase (0.1% formic acid in water and 0.1% formic acid in acetonitrile) on polar embeded C18 Synergy Fusion column (4 μm, 150 x 2.0 mm (Phenomenex)). The pharmaceuticals were extracted from water using Strata-X SPE-cartridges. Developed SPE-HPLC-MS method was validated for linearity, precision, repeatability, limit of detection (LOD), limit of quantification (LOQ) and recovery to confirm method suitability for determination these pharmaceuticals in wastewaters. Optimized and validated method has been applied to determination of selected pharmaceuticals in pharmaceutical industry wastewater. References [1] V. Andreu, C. Blasco, Y. Pico, Analytical strategies to determine quinolone residues in food and the environment, Trends Anal. Chem. 26 (2007) 534-556. [2] F. Hernández, J. V. Sancho, M. Ibáñez, C. Guerrero, Antibiotic residue determination in environmental waters by LC-MS, Trends Anal. Chem. 26 (2007) 466-485. [3] A. Gentili, LC-MS methods for analyzing anti-inflammatory drugs in animal-food products, Trends Anal. Chem. 26 (2007) 595-608.

pharmaceuticals; HPLC-MS; SPE; validation; wastewater

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