Development and Optimization of a HPLC-DAD Method for the Determination of Diverse Pharmaceuticals in Estuarine Surface Waters

This paper describes the development and validation of a simple analytical method using solid-phase extraction followed by a high-performance liquid chromatography with diode array detection (HPLC-DAD) analysis. Target compounds included six pharmaceuticals (carbamazepine, diazepam, fluoxetine, prop...

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Bibliographic Details
Published in:Journal of chromatographic science 2010-03, Vol.48 (3), p.176-182
Main Authors: Madureira, Tânia Vieira, Rocha, Maria João, Cass, Quezia Bezerra, Tiritan, Maria Elizabeth
Format: Article
Language:English
Subjects:
Analysis methods
Analytical chemistry
Applied sciences
Chemistry
Chromatographic methods and physical methods associated with chromatography
Chromatography, High Pressure Liquid - methods
Exact sciences and technology
Limit of Detection
Natural water pollution
Other chromatographic methods
Pharmaceutical Preparations - analysis
Pollution
Rivers - chemistry
Water - analysis
Water Pollutants, Chemical - analysis
Water treatment and pollution
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Summary:This paper describes the development and validation of a simple analytical method using solid-phase extraction followed by a high-performance liquid chromatography with diode array detection (HPLC-DAD) analysis. Target compounds included six pharmaceuticals (carbamazepine, diazepam, fluoxetine, propranolol, sulfamethoxazole, and trimethoprim) and the active metabolite of fenofibrate (fenofibric acid). Briefly, this method consisted of the preconcentration of water samples (2 L) on 500 mg Oasis HLB cartridges and HPLC analysis using a RP-18 analytical column in a gradient mode with a flow rate of 1 mL/min. The validation parameters revealed that this method was highly specific for all assayed compounds (> 99%), and the linearity of the calibration curves always showed a correlation higher than 0.99. The detection limits were in the ng/L level, and recovery rates were > 70% for most of the target compounds. Analysis of samples from polluted areas of the Douro River estuary indicated that propranolol and carbamazepine are present in concentrations ranging from 22.0 to 54.0 ng/L and 21.3 to 32.7 ng/L, respectively. Thus, it is concluded that this method can be successfully applied for screening pharmaceuticals in polluted estuarine areas.
ISSN:0021-9665
1945-239X
DOI:10.1093/chromsci/48.3.176