Low cost methodology for estrogens monitoring in water samples using dispersive liquid-liquid microextraction and HPLC with fluorescence detection.
A new low cost methodology for estrogens' analysis in water samples was developed in this work. Based on dispersive liquid-liquid microextraction followed by high-performance liquid chromatography with fluorescence detection, the developed method is fast, cheap, easy-to-use, uses low volumes of organic solvents and has the possibility of a large number of samples to be extracted in parallel. Under optimum conditions (sample volume: 8 mL; extraction solvent: 200 μL of chlorobenzene; dispersive solvent: 2000 μL of acetone), the enrichment factor and extraction recoveries were 145 and 72% for 17β-estradiol (E2) and 178 and 89% for 17α-ethinylestradiol (EE2), respectively. Limits of detection of 2.0 ng L(-1) for E2 and 6.5 ng L(-1) for EE2 were achieved, allowing the detection and quantification of these compounds in surface and waste water samples with concentrations from 12 to 32 ng L(-1) for E2 and from 11 to 18 ng L(-1) for EE2. Also, recovery tests were performed to evaluate possible matrix effects. Recoveries between 98% and 106% were obtained using humic acids (HA) to simulate the effect of organic matter, and between 86% and 120% in real water samples.
CESAM & Department of Chemistry, University of Aveiro, Campus de Santiago, 3810-193 Aveiro, Portugal; Department of Complementary Sciences, Superior School of Health Technology of Coimbra, Rua 5 de Outubro S. Martinho do Bispo Apartado 7006, 3040-854 Coimbra, Portugal.
Diana L D
DL
Lima
Carla Patrícia
CP
Silva
Marta
M
Otero
Valdemar I
VI
Esteves
D000096:Acetone; D002722:Chlorobenzenes; D002851:Chromatography, High Pressure Liquid; D004784:Environmental Monitoring / Q000191:economics* / Q000379:methods; D004958:Estradiol / Q000032:analysis*; D004997:Ethinyl Estradiol / Q000032:analysis*; D005453:Fluorescence; D005618:Fresh Water / Q000737:chemistry*; D006801:Humans; D057230:Limit of Detection; D059627:Liquid Phase Microextraction; D012997:Solvents; D062065:Wastewater / Q000737:chemistry*; D014874:Water Pollutants, Chemical / Q000032:analysis*
D000096:Acetone; D002722:Chlorobenzenes; D004958:Estradiol; D004997:Ethinyl Estradiol; D012997:Solvents; D062065:Wastewater; D014874:Water Pollutants, Chemical; C031294:chlorobenzene
Dispersive liquid–liquid microextraction; Estrogens; Fluorescence detection; High-performance liquid chromatography; Water