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A solid-phase extraction and size-exclusion liquid chromatographic method for polyethylene glycol 25 p-aminobenzoic acid determination in urine: validation for urinary excretion studies of users of sunscreens
Authors:Balaguer A  Chisvert A  Salvador A  Herraez M  Diez O
Affiliation:a Departamento de Química Analítica, Universitat de València, 50 Doctor Moliner St., 46100-Burjassot, Valencia, Spain
b Departamento de Química Analítica, Nutrición y Bromatología, Universidad de Alicante, Alicante, Spain
c Departamento de Farmacia y Tecnología Farmacéutica, Universitat de València, Valencia, Spain
Abstract:No previous publications about percutaneous absorption of polyethylene glycol 25 p-aminobenzoic acid (PEG-25 PABA) have been found in the literature and the expected levels to be found in human urine after sunscreens use are unknown. The method proposed here is suitable to determine PEG-25 PABA in the urine of sunscreens users in order to carry out studies on body accumulation/excretion. It is based on solid-phase extraction (SPE) with size-exclusion liquid chromatography determination. Solid-phase extraction allows the analyte to be retained and subsequently eluted for a clean-up, using a silica-based cartridge. The size-exclusion liquid chromatography of the eluted allows the rest of matrix interferences to be avoided. Fluorescence intensity was measured at λem = 350 nm (λexc = 300 nm). The sensitivity of the proposed method is in the order of 450 ± 5 mL ng−1 and the detection limit (3 Sy/x/b) in the measured solutions is in the order of 13 ng mL−1, that is 2.6 ng mL−1 in urine samples. The method enables PEG-25 PABA to be determined in both, spiked and unspiked human urine samples. Results obtained for spiked human urine samples (11-100 ng mL−1) demonstrated the accuracy of the method. The mean relative standard deviation of the results was in the order of 3-10%. Three volunteers applied a sunscreen lotion containing a 8% PEG-25 PABA sunscreen cream and their urinary excretion was controlled from the moment of application until the excreted amounts were no longer detectable.
Keywords:Polyethylene glycol 25 p-aminobenzoic acid   Ultraviolet filter   Sunscreen   Urine   Solid-phase extraction   Size-exclusion liquid chromatography   Fluorescence detection
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