Detecção e quantificação de fármacos e disruptores endócrinos na urina humana durante o processo de estocagem com vistas ao uso agrícola
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Data
2011-02-28
Autores
Campos, Julia Magalhães Brum
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Universidade Federal do Espírito Santo
Resumo
Human urine contains most of the essential nutrients in agriculture. However, urine is also the route of excretion of unchanged pharmaceuticals and metabolites and endocrine disruptors. This study aimed to evaluate the chromatographic profile of sodium diclofenac, prednisolone, progesterone and sulfamethoxazole in human urine duringthestorage treatment process of human urine with and without acidification, assess the influence of temperature and pH variation during the process of treatment, quantify by HPLC-DAD the analyzed compoundsin acidifiedhuman urine duringthestorage treatment process and determine the method of detection. The method was applied to acidified and non acidified human urine samples,submitted to the storage process for 30 days cycles under different temperatures. It was observed that the employed temperature variation did not alter the chromatographic profile of theanalyzedsamples. The urine that was not submitted to the acidification process showed changesin its chromatographic profile, probably due to the process of urea hydrolysis, and not being, therefore, possible to quantify pharmaceuticals and endocrine disruptors in it. The method for reversed-phase HPLC developed in this study is sensitive, selective and reproducible for the determination of the four pharmaceuticals used in human urine during the storage period. The most appropriate mobile phase for the elution of pharmaceuticals and endocrine disruptors studied (SULFA, PRED, DICLEand PRO) in human urine, with less dispersion of the analyte, was the mobile phase 4 (FM4). At thismobile phasethe elution was performed by gradient, 1.0 mL min-¹ flow and concentration of acetonitrile (ACN) ranging between 10 and 15%, allowing the mobile phase to produce adequate chromatographic strength and selectivity forthe separation of the pharmaceuticals and disruptors studied. The HPLC-DAD method used showed satisfactory linearity (r> 0.99 for all analyzed compounds) and precision (CV <5% for all compounds). The limits of detection (LOD) and quantification (LOQ) values were lower than those used in the process of storage, thereforesuitable for the performed analysis. Thus,the quantification of thesestudiedcompounds was performed only inacidifiedhuman urine. We conclude that the treatment conditions used in this work, that is, urineacidificationand storage temperature,were not sufficient to reduce the concentration of the studied compounds. The initially added concentration was maintained until the end of the experiment, with no decreases.
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Palavras-chave
human urine , agricultural fertilizer , storage , validation , HPLC , urina humana , fertilizante agrícola , estocagem , CLAE , validação
Citação
CAMPOS, Julia Magalhães Brum. Detecção e quantificação de fármacos e disruptores endócrinos na urina humana durante o processo de estocagem com vistas ao uso agrícola. 2011. 107 f. Dissertação (Mestrado em Engenharia Ambiental) - Universidade Federal do Espírito Santo, Centro Tecnológico, Vitória, 2011.