RT info:eu-repo/semantics/article T1 Use of a pH-sensitive polymer in a microextraction and preconcentration method directly combined with high-performance liquid chromatography A1 González-Martín, Raúl A1 Pacheco-Fernández, Idaira A1 Maiti, Binoy A1 Ayala, Juan H. A1 Afonso Perera, Ana María A1 Díaz Díaz, David A1 Pino, Verónica K1 pH-sensitive polymer K1 Hydrogel K1 Microextraction K1 Liquid chromatography K1 Polycyclic aromatic hydrocarbons K1 Urine K1 polímeros sensibles al pH K1 hidrogel K1 microextracción K1 cromatografía líquida K1 hidrocarburos aromáticos policíclicos K1 orina AB A pH-sensitive polymer based on the poly(styrene- alt -maleic anhydride) co-polymer serves as basis to develop a microextraction method (pH-HGME) in direct combination with high-performance liquid chromatography (HPLC) and fluorescence detection (FD) for the determination of seven organic com- pounds, including three polycyclic aromatic hydrocarbons (PAHs), three monohydroxylated PAHs and one alkylphenol, in urine. The method bases on the structural modification of the pH-sensitive polymer in the aqueous sample at a high pH value, followed by the formation and insolubilization of a hydrogel contain- ing the preconcentrated analytes by decreasing the pH, and the direct injection of the hydrogel-rich phase in the HPLC-FD system. The optimization of the main variables permitted the selection of low amounts of aqueous sample (10 mL), which was mixed with 10 mg of co-polymer also present in a low volume (150 μL) of concentrated NaOH. The method further requires the addition of 200 μL of concentrated HCl, 3 min of stirring, and 15 min of centrifugation. This pH-HGME-HPLC-FD method presented low limits of detection, ranging from 0.001 μg L −1 to 0.09 μg L −1 in ultrapure water, average relative recoveries of 96.9% for the concentration level of 0.60 μg L −1 , and enrichment factors between 1.50 and 17.7. The pro- posed method also exhibited high precision, with intermediate relative standard deviations lower than 16% for a concentration level of 0.60 μg L −1 . The developed pH-HGME-HPLC-FD method performed ade- quately when analyzing two human urine samples provided by a non-smoker male and a smoker female, respectively. One of the target analytes (2-hydroxynaphthalene) was quantified in both samples using the standard addition method, with a predicted concentration of 7.3 ±0.4 μg L −1 in the non-smoker male urine and 19.3 ±0.6 μg L −1 in the smoker female urine. PB Elsevier YR 2020 FD 2020 LK http://riull.ull.es/xmlui/handle/915/21432 UL http://riull.ull.es/xmlui/handle/915/21432 LA en NO Agencia Canaria de Investigación, Innovación y Sociedad de la Información DS Repositorio institucional de la Universidad de La Laguna RD 27-nov-2024