title: Synthesis of a molecularly imprinted polymer for the isolation of 1-hydroxypyrene in human urine.
abstract: In the last decades, the assessment of polycyclic aromatic hydrocarbons' exposure has generated great interest and 1-hydroxypyrene (1-OHP) has been commonly used as a biological indicator of exposure to PAHs in many studies in environmental and occupational health. In this research, a molecularly imprinted polymer (MIP) was synthesised by precipitation polymerisation using 1-OHP as template, methacrylic acid (MAA) as functional monomer, ethylene glycol dimethacrylate (EGDMA) as cross-linker, and acetonitrile as porogen. MIP was used as solid-phase extraction (SPE) material for sample pretreatment and isolation of 1-OHP and posterior detection in a reversed-phase HPLC-FLD. Various parameters including washing solvent, elution solvent and volume affecting the extraction efficiency of the polymer have been evaluated to achieve the isolation of 1-OHP from urine samples and to reduce non-specific interactions. Cross-selectivity was studied in the presence of other structural analogues of the 1-OHP as hydroxyphenantrene isomers. The method was validated over a concentration range of 0.15-2.00 µg L(-1), R(2)>0.998. Recovery values were in the range of 78-90% and RSD <6.7%. The limits of detection and quantification were 0.05 µg L(-1) and 0.17 µg L(-1), respectively. In our knowledge, it is the first time that this methodology is applied for analysing urinary hydroxypyrene and it has been demonstrated that this specific MISPE-HPLC-FLD method offers a fast and simple alternative to determine 1-OHP in human urine samples.
authors.affiliation: Department of Analytical Sciences, Faculty of Sciences, National University of Distance Education (UNED), E-28040 Madrid, Spain.
authors.forename: M
authors.initials: M
authors.lastname: Serrano
authors.affiliation: Department of Analytical Sciences, Faculty of Sciences, National University of Distance Education (UNED), E-28040 Madrid, Spain.
authors.forename: M
authors.initials: M
authors.lastname: Bartolomé
authors.affiliation: Department of Analytical Sciences, Faculty of Sciences, National University of Distance Education (UNED), E-28040 Madrid, Spain. Electronic address: agallego@ccia.uned.es.
authors.forename: A
authors.initials: A
authors.lastname: Gallego-Picó
authors.affiliation: Department of Analytical Sciences, Faculty of Sciences, National University of Distance Education (UNED), E-28040 Madrid, Spain.
authors.forename: R M
authors.initials: RM
authors.lastname: Garcinuño
authors.affiliation: Department of Analytical Sciences, Faculty of Sciences, National University of Distance Education (UNED), E-28040 Madrid, Spain.
authors.forename: J C
authors.initials: JC
authors.lastname: Bravo
authors.affiliation: Department of Analytical Sciences, Faculty of Sciences, National University of Distance Education (UNED), E-28040 Madrid, Spain.
authors.forename: P
authors.initials: P
authors.lastname: Fernández
mesh_terms: D000097:Acetonitriles / Q000737:chemistry; D006801:Humans; D007231:Infant, Newborn; D008689:Methacrylates / Q000737:chemistry; D054802:Molecular Imprinting; D058105:Polymerization; D011108:Polymers / Q000138:chemical synthesis* / Q000737:chemistry; D011721:Pyrenes / Q000737:chemistry / Q000302:isolation & purification* / Q000652:urine*; D052616:Solid Phase Extraction / Q000379:methods*
chemical_list: D000097:Acetonitriles; D008689:Methacrylates; D011108:Polymers; D011721:Pyrenes; C008384:methacrylic acid; C004919:ethylene dimethacrylate; C033146:1-hydroxypyrene; C032159:acetonitrile
keywords: 1-Hydroxypyrene; HPLC-FLD; MISPE; Urine