engleski

HPLC-FLD determination of pharmaceuticals in wastewaters of pharmecautical industry after precolumn derivatization by fluorescamine

Industries often use surface water as a recipient for effluents after wastewater treatment. In case of human or veterinary pharmaceutical production those wastewaters are usually loaded with high concentracions active pharmaceutical ingredients (API). In order to meet the future environmental quality standards it is important to develop robust and sensitive API multiclass determination methods. A liquid chromatographic method with fluorimetric detection (HPLC-FLD) is proposed for the determination of pharmaceuticals in wastewater samples: sulfonamides (sulfaguanidine, sulfadiazine and sulfadimidine), fluoroquilones (ciprofloxacin, enrofloxacin, norfloxacin) and local anesthetic procaine. the analytes are preconcentrated by solid phase extraction (SPE) using Strata-X cartridges and acetonitrile as eluent. the chromatographic separation on a Synergy Fusion-RP18 80°A, 150 mm x 4, 6 mm, particle size 4 micrometers column with a gradient elution program using mobile phase based on mixtures of solvents 0, 1% acetic acid in water and 0, 1% acetic acid in acetonitrile at a flow rate of 1, 0 mL/min is performed. Fluoroquinolones are highly fluorescent ; sulfonamides and procaine are precolumn derivatized with a fluorescamine solution in acetonitrile (5mg/10mL acetonitrile) and acetic buffer. The highly fluorescent compounds are detected at different lambda(ex)/lambda(em) (nm/nm): sulfonamides and procaine at 405/495 and fluoroquinolones at 277/445. The performance characteristics of the SPE-HPLC-FLD method were established by validation procedure. Selectivity, linearity, limits of detection (LOD) and quantification (LOQ), precision and recovery were studied. The decsribed method is applied to the determination of the investigated pharmnaceuticals in pharmaceutical industry wastewater.

HPLC-FLD; wastewater; derivatization; fluorescamine; veterinary pharmaceuticals

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