title: Development and validation of a rapid method for the determination of tetracycline in activated sludge by SPE clean-up and HPLC-UV detection.
abstract: The aim of this study was to develop and validate a rapid analytical method for tetracycline (TC) determination in activated sludge. The analytical method developed is applicable on activated sludge containing a volatile suspended solid concentration below 10 g l(-1), which nearly includes all wastewater treatment plants and the major proportion of membrane bioreactors. The analytical method included two steps: sample clean-up followed by high-performance liquid chromatography (HPLC) with ultraviolet (UV) detection analysis. Prior to the analysis, TC was extracted from the matrix by a mixture of EDTA and McIlvaine buffer. Sample clean-up was carried out by solid phase extraction (SPE) with strong anion exchange (SAX) cartridges. SAX cartridges retained organic matters interfering with TC. Analysis was performed by HPLC-UV with a gradient elution. The method was validated as the R2 value was 0.9991 for the calibration curve. Recoveries were between 92% (+/- 6%) and 103% (+/- 9%). The limit of detection (LOD) and the limit of quantification (LOQ) were 0.1 mg l(-1) and 0.5 mg l(-1), respectively. Accuracy was not entirely satisfactory, but should be related to the complexity of the matrix, which is a hindrance to the precision of the method. The method was also validated on industrial samples.
authors.affiliation: Ecole Nationale Supérieure de Chimie de Rennes, Université de Rennes 1, Rennes, France.
authors.forename: Nolwenn
authors.initials: N
authors.lastname: Prado
authors.forename: Emilie
authors.initials: E
authors.lastname: Renault
authors.forename: Juan
authors.initials: J
authors.lastname: Ochoa
authors.forename: Abdeltif
authors.initials: A
authors.lastname: Amrane
mesh_terms: D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D012015:Reference Standards; D012722:Sewage / Q000737:chemistry*; D013056:Spectrophotometry, Ultraviolet / Q000379:methods*; D013752:Tetracycline / Q000032:analysis*
chemical_list: D012722:Sewage; D013752:Tetracycline