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Abstract
An efficient and simple method for the determination of furan in baby-food (vegetables and fruits) by solid phase micro-extraction–gas
chromatography–mass spectrometry (SPME–GC–MS) was developed and validated. Experimental design was used to investigate the effects
of temperature and time of extraction. The calculated regression model was used to find the experimental conditions providing the optimal SPME
extraction yield. Validation was carried out in terms of limit of detection (LOD), limit of quantitation (LOQ), linearity, precision and trueness.
LOD and LOQ values in the low ng kg−1 were achieved, whereas linearity was established over two order of magnitude. Good precision was
obtained both in terms of intra-day repeatability and between-day precision on two concentration levels (RSD% lower than 3.6%). Recovery
values of 91.5 ± 6.2% and of 96.1 ± 1.3% (n = 3) were calculated at 75 ng kg−1 and 75 g kg−1 level. Finally, the applicability of the method to the
determination of furan in a number of commercial and home-made baby-food samples was demonstrated.
© 2006 Elsevier B.V. All rights reserved.
Keywords: Furan; Solid phase micro-extraction; Baby-food; Food safety; GC–MS; Method validation
1. Introduction tion and toxicology [3]. In fact, although furan is a well known
heat treatment related by-product and has been detected in many
Food safety is regarded as a widespread priority task. In addi- thermally treated foods [4], only few methods principally based
tion to the actions undertaken by food-related industries, the EU on static headspace techniques have been developed and applied
legislative committees are reviewing current legislation, both for furan determination in food [5–10].
introducing new recommendations aimed to the establishment SPME is an alternative solvent-free sampling technique
of general principles issuing rules to increase quality standards widely used for the analysis of volatile compounds, but nowa-
in food and fixing hazard limits for the EU citizen health [1]. days only a SPME–GC–MS method with the use of a cryofo-
Recently, great attention has been paid to the presence of both cussing unit was recently developed for furan determination in
natural and xenobiotic contaminants in raw and processed foods. heated foodstuffs [11].
Among naturally-occurring substances, great concern is The aim of this work was the development and validation of
addressed to the analysis of furan, this compound being classi- a more simple method for the selective and sensitive analysis of
fied by the International Agency for Research on Cancer (IARC) furan in baby-food, based on SPME–GC–MS.
in the group 2B “as possibly carcinogenic to humans” [2]. The An experimental design was used to study the effects of two
Food and Drug Administration (FDA) is requesting the submis- parameters on the SPME extraction, i.e. temperature of extrac-
sion of data and information regarding the occurrence of furan tion and time of extraction. Data obtained allowed to calculate
in food, as well as sources of exposure, mechanisms of forma- the main and interaction effects of the factors under investiga-
tion, thus indicating the optimised extraction conditions.
The SPME–GC–MS method was then validated under opti-
∗ Corresponding author. Tel.: +39 0521 905433; fax: +39 0521 905556. mised conditions. According to the EURACHEM guidelines,
E-mail address: federica.bianchi@unipr.it (F. Bianchi). in-house validation was carried out in terms of detection
0021-9673/$ – see front matter © 2006 Elsevier B.V. All rights reserved.
doi:10.1016/j.chroma.2005.10.056
F. Bianchi et al. / J. Chromatogr. A 1102 (2006) 268–272 269
limit (LOD), quantitation limit (LOQ), linearity, precision The fiber was conditioned in the injection port of the gas
and trueness. Excellent results in the low ng kg−1 level were chromatograph at 300 ◦ C under helium flow for 1.5 h prior to
obtained for LOD and LOQ, thus proving the potential of the use. Desorption was carried out at the temperature of 230 ◦ C
method for the determination of furan at ultratrace levels in for 3 min. A fiber blank was run between each sample to reduce
baby-food. memory effects.
The method developed was then applied to determine furan
in commercial and home-made baby-food samples. 2.4. GC–MS analysis
In order to obtain the highest furan yield and the absence of 3.3. Method validation
memory effects, fiber selection was performed by testing three
different coatings: The method was validated in terms of detection limit, quanti-
tation limit, linearity, precision and trueness by using the exper-
• Polydimethylsiloxane-divinylbenzene (PDMS-DVB) 65 m; imental setting providing the optimised conditions.
F. Bianchi et al. / J. Chromatogr. A 1102 (2006) 268–272 271
Table 1
Furan content in baby-food samples
Baby-food samples Furan (g/kg)a
The analytical approach was based on the use of SPME cou- [6] http://www.fda.gov/ohrms/dockets/ac/cfsan04.html, accessed 27 Septem-
pled with GC–MS analysis for food safety evaluation purposes. ber 2005.
[7] http://www.cfsan.fda.gov/∼dms/furandat.html, accessed 27 September
The selection of the SPME fiber and the use of an experimen-
2005.
tal design allowed to calculate the optimal sampling conditions. [8] A. Becalski, S. Seaman, J. AOAC 88 (2005) 102.
These conditions were found in correspondence with a tempera- [9] T. Kuballa, S. Stier, N. Stricow, Deutsche Lebensmittel-Rundschau 101
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the determination of the investigated analyte at low ng kg−1 lev- 878.
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a number of commercial and home-made baby-food samples, New York, 1978.
thus revealing differences related to the production technique. [13] A.I. Khuri, J.A. Cornell, Response Surfaces, Marcel Dekker, New York,
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[14] F. Bianchi, M. Careri, C. Corradini, A. Mangia, M. Musci, CAC 1
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