Multivariate optimization of headspace trap for furan and furfural simultaneous determination in sponge cake

• Published in: Talanta (Oxford) Vol. 164; pp. 708 - 715
• Main Authors: Cepeda-Vázquez, Mayela, Blumenthal, David, Camel, Valérie, Rega, Barbara
• Format: Journal Article
• Language: English
• Published: Netherlands Elsevier B.V 01.03.2017; Elsevier
• Subjects: Desirability function; Life Sciences; Optimal design of experiments; Random blocks; Response surface; Stable isotope dilution assay; Standard addition method; Standard addition method; HS; dp; DHS; Te; Random blocks; SPME; Response surface; DOE; SLS; LOD; RSD; Optimal design of experiments; RSM; ta; LOQ; ra; GC-MS; O-DOE; REML; ti; cy; SIM; Stable isotope dilution assay; Desirability function; LPME
• ISSN: 0039-9140; 1873-3573
• DOI: 10.1016/j.talanta.2016.10.073

Furan, a possibly carcinogenic compound to humans, and furfural, a naturally occurring volatile contributing to aroma, can be both found in thermally treated foods. These process-induced compounds, formed by close reaction pathways, play an important role as markers of food safety and quality. A method capable of simultaneously quantifying both molecules is thus highly relevant for developing mitigation strategies and preserving the sensory properties of food at the same time. We have developed a unique reliable and sensitive headspace trap (HS trap) extraction method coupled to GC-MS for the simultaneous quantification of furan and furfural in a solid processed food (sponge cake). HS Trap extraction has been optimized using an optimal design of experiments (O-DOE) approach, considering four instrumental and two sample preparation variables, as well as a blocking factor identified during preliminary assays. Multicriteria and multiple response optimization was performed based on a desirability function, yielding the following conditions: thermostatting temperature, 65°C; thermostatting time, 15min; number of pressurization cycles, 4; dry purge time, 0.9min; water / sample amount ratio (dry basis), 16; and total amount (water + sample amount, dry basis), 10g. The performances of the optimized method were also assessed: repeatability (RSD: ≤3.3% for furan and ≤2.6% for furfural), intermediate precision (RSD: 4.0% for furan and 4.3% for furfural), linearity (R2: 0.9957 for furan and 0.9996 for furfural), LOD (0.50ngfuran gsample dry basis−1 and 10.2ngfurfural gsample dry basis−1), LOQ (0.99ngfuran gsample dry basis−1 and 41.1ngfurfural gsample dry basis−1). Matrix effect was observed mainly for furan. Finally, the optimized method was applied to other sponge cakes with different matrix characteristics and levels of analytes. [Display omitted] •An optimized HS trap extraction method was developed using an O-DOE approach.•A tailor-made DOE was created for analytical screening and a blocking factor.•4 instrumental and 2 sample preparation factors were identified and optimized.•Furan and furfural can be accurately quantified in a complex solid food matrix.