On-line renewable solid-phase extraction hyphenated to liquid chromatography for the determination of UV filters using bead injection and multisyringe-lab-on-valve approach

• Type: Article in International Scientific Journal
• Date: 2010

Authors

Hugo M Oliveira (Author) Other; Marcela A Segundo (Author) FFUP; Jose L F C Lima (Author) FFUP; Manuel Miro (Author) Other; Victor Cerda (Author) Other

Journal

Title: Journal of Chromatography A

Vol. 1217 No. 43

Pages: 3575-3582

ISSN: 0021-9673

Publisher: Elsevier

Indexing

ISI Web of Knowledge - 32 Citations

Scopus - 39 Citations

Scientific classification

FOS: Natural sciences > Chemical sciences

CORDIS: Health sciences

Other information

Authenticus ID: P-003-6MZ

DOI: 10.1016/j.chroma.2010.03.035

Resumo (PT): 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 C18 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 μg L−1 for 9 mL sample volume. Linear calibration was attained up to 160 μg L−1 for homosalate and up to 35 μg 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 9 min. 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. <br> <br> Keywords: UV filters; Automation; On-line solid-phase extraction; Lab-on-valve; Bead injection <br> <a target="_blank" href="http://www.sciencedirect.com/science?_ob=ArticleURL&_udi=B6TG8-4YPT1RD-2&_user=2460038&_coverDate=05%2F28%2F2010&_rdoc=4&_fmt=high&_orig=browse&_srch=doc-info(%23toc%235248%232010%23987829977%231947685%23FLA%23display%23Volume)&_cdi=5248&_sort=d&_docanchor=&_ct=10&_acct=C000057398&_version=1&_urlVersion=0&_userid=2460038&md5=1d07f0c05a3e0e01ff4d1f764b551f6e "> Texto integral </a> <br> <br>

Abstract (EN): 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.

Language: English

Type (Professor's evaluation): Scientific

No. of pages: 8