title: On-line flow injection molecularly imprinted solid phase extraction for the preconcentration and determination of 1-hydroxypyrene in urine samples.
abstract: New analytical strategies tend to automation of sample pre-treatment and flow analysis techniques provided a number of enhanced analytical methods allowing high throughput. Flow techniques are usually faster, more robust and more flexible than their batch equivalents. In addition, flow methods use less sample and reagent amounts and reduce analytical costs and waste. A flow injection solid-phase extraction pre-concentration system using a molecularly imprinted polymer (MIP) packed micro-column was developed for the determination of 1-hydroxypyrene in human urine with fluorescence detection. The pre-concentration of 1-hydroxypyrene on the MIP was carried out based on the specific retention of analyte by on-line introducing the sample into the micro-column system. Methanol and dichloromethane mixture was used to elute the retained analyte for fluorometric analysis. Important influencing factors were studied in detail, in batch and in flow (MISPE procedure optimisation, sample and eluent volumes, flow rate, dimensions of MIP micro-column and amounts of packing material, etc). To the best of our knowledge, this is the first on-line flow injection molecularly imprinted solid phase extraction for the pre-concentration and determination of hydroxylate PAH metabolite in urine samples. The optimised method was successfully applied to the determination of 1-Hydroxypyrene in spiked urine samples, with recoveries in the range of 74-85% and RSD<4.6%. Under optimum experimental conditions, the linearity concentration range used was 10-400μgL-1, R2>0.996. We obtained limit of detection and quantification of 3.1μgL-1and 10.5μgL-1, respectively.
authors.affiliation: Department of Analytical Sciences, Faculty of Sciences. National University of Distance Education (UNED), 28040 Madrid, Spain.
authors.forename: Montserrat
authors.initials: M
authors.lastname: Serrano
authors.affiliation: Department of Analytical Sciences, Faculty of Sciences. National University of Distance Education (UNED), 28040 Madrid, Spain.
authors.forename: Mónica
authors.initials: M
authors.lastname: Bartolomé
authors.affiliation: Department of Analytical Sciences, Faculty of Sciences. National University of Distance Education (UNED), 28040 Madrid, Spain.
authors.forename: Juan Carlos
authors.initials: JC
authors.lastname: Bravo
authors.affiliation: Department of Analytical Sciences, Faculty of Sciences. National University of Distance Education (UNED), 28040 Madrid, Spain.
authors.forename: Gema
authors.initials: G
authors.lastname: Paniagua
authors.affiliation: Department of Chemical and Energy Technology, Chemical and Environmental Technology, Mechanical Technology and Analytical Chemistry, King Juan Carlos University (URJC), 28933 Móstoles, Spain.
authors.forename: Judith
authors.initials: J
authors.lastname: Gañan
authors.affiliation: Department of Analytical Sciences, Faculty of Sciences. National University of Distance Education (UNED), 28040 Madrid, Spain. Electronic address: agallego@ccia.uned.es.
authors.forename: Alejandrina
authors.initials: A
authors.lastname: Gallego-Picó
authors.affiliation: Department of Analytical Sciences, Faculty of Sciences. National University of Distance Education (UNED), 28040 Madrid, Spain.
authors.forename: Rosa María
authors.initials: RM
authors.lastname: Garcinuño
mesh_terms: D017022:Flow Injection Analysis; D006801:Humans; D007231:Infant, Newborn; D054802:Molecular Imprinting / Q000379:methods*; D011108:Polymers / Q000138:chemical synthesis; D011721:Pyrenes / Q000302:isolation & purification* / Q000652:urine*; D052616:Solid Phase Extraction / Q000379:methods*; D012997:Solvents / Q000737:chemistry
chemical_list: D011108:Polymers; D011721:Pyrenes; D012997:Solvents; C033146:1-hydroxypyrene
keywords: 1-Hydroxypyrene; Flow injection analysis; Human urine; Molecularly imprinted polymer; On-line solid-phase extraction