Journal
JOURNAL OF CHROMATOGRAPHY A
Volume 1217, Issue 22, Pages 3575-3582Publisher
ELSEVIER SCIENCE BV
DOI: 10.1016/j.chroma.2010.03.035
Keywords
UV filters; Automation; On-line solid-phase extraction; Lab-on-valve; Bead injection
Funding
- FCT [PTDC/AAC-AMB/104882/2008]
- Spanish Ministry of Education and Science [CTQ2007-64331]
- Integrated Action [E-48/09, HP2008-0045]
- Fundacao para a Ciencia e Tecnologia (FCT)
- FSE (III Quadro Comunitario) [SFRH/BD/22494/2005]
- Fundação para a Ciência e a Tecnologia [SFRH/BD/22494/2005] Funding Source: FCT
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For the first time, an automatic sample pre-treatment/detection method is proposed for the multiclass determination of UV filters (namely, benzophenone-3, ethylhexylmetoxycinnamate, butylmethoxydibenzoylmethane and homosalate) in environmental samples. The new methodology comprises in-line solid-phase extraction (SPE) of the target analytes by exploiting the bead injection (BI) concept in a mesofluidic lab-on-valve (LOV) format, with subsequent determination by liquid chromatography (LC). The proposed microanalytical system, using a multisyringe burette as propulsion unit, automatically performed the overall SPE steps, including the renewal of the sorbent in each analytical cycle to prevent sample cross-contamination and the post-extraction adjustment of the eluate composition to prevent chromatographic band broadening effects. In order to expedite the LC separation, a C-18 monolithic column was applied and an accelerated isocratic elution was carried out by using a cationic surfactant as mobile phase additive. The LOV-BI-LC method was proven reliable for handling and analysis of complex matrices, e.g., spiked swimming pool water and seawater, with limits of detection ranging between 0.45 and 3.2 mu g L-1 for 9 mL sample volume. Linear calibration was attained up to 160 mu g L-1 for homosalate and up to 35 mu g L-1 for the other target analytes, with good reproducibility (RSD < 13%, for 5 different SPE columns). The hyphenated scheme is able to process a given sample simultaneously and within the same time frame than the chromatographic separation/determination of the formerly pre-treated sample, providing concentration values every 9min. Hence, the sample throughput was enhanced up to 33 times when compared with previously reported off-line SPE methods. A drastic reduction in reagent consumption and effluent production was also attained, contributing to the development of an environment-friendly analyzer. (C) 2010 Elsevier B.V. All rights reserved.
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