Heating on the Volatile Composition and Sensory Aspects of Extra-Virgin
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566 HEATING ON THE VNUNES,OLATILE C. A. et al. COMPOSITION AND SENSORY ASPECTS OF EXTRA-VIRGIN OLIVE OIL Aquecimento na composição volátil e aspectos sensoriais do azeite de oliva extra virgem Cleiton Antônio Nunes1, Vanessa Rios de Souza2, Síntia Carla Corrêa2, Marília de Cássia da Costa e Silva2, Sabrina Carvalho Bastos2, Ana Carla Marques Pinheiro2 ABSTRACT The main ways by which extra-virgin olive oil is consumed include direct application on salads or as an ingredient in sauces, but it is also been used by some for cooking, including frying and baking. However, it has been reported that under heat stress, some nonglyceridic components of olive oil are degraded. So, the effect of heating (at 50, 100, 150, and 200 °C for 2 h) on the volatile composition and sensory aspects of extra-virgin olive oil were evaluated. Heating altered the volatile composition of extra-virgin olive oil, mainly at higher temperatures (above 150 °C). The main modifications were related to the formation of large amounts of oxidized compounds, particularly large chain aldehydes. Sensory aspects were also altered when the oil was heated to higher temperatures, which might have occurred because of color alterations and mainly changes in the volatile composition of the oil. Index terms: Vegetable oil, sensory analysis, chemical composition. RESUMO Os principais meios de consumo do azeite de oliva extravirgem incluem a aplicação direta em saladas ou como ingrediente em molhos, mas ele também tem sido usado para cozinhar, seja em frituras ou cozimentos. No entanto, sob estresse térmico, alguns componentes não-glicerídicos do azeite podem ser degradados. Assim, o efeito do aquecimento (a 50, 100, 150 e 200 °C por 2 h) sobre os componentes voláteis e aspectos sensoriais do azeite de oliva extravirgem foram avaliados. Os resultados indicaram que o aquecimento alterou a composição volátil do azeite extra virgem, principalmente em temperaturas mais elevadas (acima de 150 °C). As principais modificações foram relacionadas à formação de compostos oxidados, sobretudo aldeídos de cadeia longa. Os aspectos sensoriais também sofreram alterações quando o azeite foi aquecido a temperaturas elevadas (acima de 150 °C), o que pode ter sido influenciado por alterações de cor e pelas da composição volátil do produto. Termos para indexação: Óleo vegetal, análise sensorial, composição química. (Received in january 30, 2013 and approved in september 6, 2013) INTRODUCTION some pathologies, particularly cardiovascular diseases (MESA et al., 2006). Therefore, the consumption of extra- Extra-virgin olive oil is a product appreciated for its virgin olive oil has been increasing and research has been flavor, which is distinguished from that of other vegetable encouraged aimed at improving the production (DUTRA oils, and is used in various culinary practices worldwide. et al., 2004; OLIVEIRA et al., 2009; OLIVEIRA et al., 2010). Extra-virgin olive oil is obtained from the first cold pressing Although the main ways by which extra-virgin olive of olives, which produces a special volatile compound oil is consumed include direct application on salads or as composition that provides its much-appreciated an ingredient in sauces, it is also been used by some for characteristics of taste and aroma (OLIVEIRA et al., 2008). cooking, including frying and baking. However, it has been Since no refining process is employed, extra-virgin reported that under heat stress, some nonglyceridic olive oil contains a number of nonglyceridic constituents, components of olive oil are degraded, such as chlorophylls, which are believed to account for its beneficial health carotenoids (AVADI; GRATI-KAMOUN; ATTIA, 2009), effects due to their considerable antioxidant activity tocopherols (ALLOUCHE et al., 2007), and especially (VISIOLI et al., 2006). In addition, extra-virgin olive oil has phenolic compounds (CERRETANI et al., 2009; BENDINI been reported to have anticancer, anti-inflammatory, and et al., 2009; VALLI et al., 2010; ). In addition, parameters antiatherogenic activities (BERGER; JONAS; ABUMWEIS, related to the hydrolytic and oxidative states of the oil also 2004). Furthermore, its high monounsaturated fatty acid are altered under heat stress (CERRETANI et al., 2009; composition has been associated with the prevention of BENDINI et al., 2009). 1Universidade Federal de Lavras/UFLA – Departamento de Ciência dos Alimentos/DCA – Cx. P. 3037 – 37200-000 – Lavras – MG – Brasil – [email protected] 2Universidade Federal de Lavras/UFLA – Departamento de Ciência dos Alimentos/DCA – Lavras – MG – Brasil Ciênc. agrotec., Lavras, v. 37, n. 6, p. 566-572, nov./dez., 2013 Heating on the volatile composition... 567 Triglycerides can also degrade under thermal stress, were repeated in quadruplicate. The more capable (those thus affecting the quality of the oil. Studies on soybean oil with better repeatability and discriminative ability) testers and soybean oil-based fats showed that volatile were selected for the experiments. compounds (SNYDER; KING, 1994) and sensory The 10 selected trained testers were then asked to characteristics (BREWER et al., 1999) were altered after discriminate samples of extra-virgin olive oil heated at 50 intense heating. The main alterations in volatile °C, 100 °C, 150 °C, and 200 °C from a unheated control composition are the formation of oxidized compounds, based on flavor and overall aspects using the scale particularly specific aldehydes, which were negatively described above. The evaluations were carried out in correlated with sensory aspects. triplicate. The results were expressed as the means of the This work evaluates the effect of heating on the difference from the control given by the testers. volatile composition and sensory aspects of extra-virgin Experiments were conducted in a closed cabin with olive oil. Samples of extra-virgin olive oil were heated at 50 white illumination. The samples (5 mL of extra-virgin olive °C, 100 °C, 150 °C, and 200 °C for 2 h. oil) were labeled with 3 random digits on a white surface. MATERIAL AND METHODS Color analysis Sample preparation Color parameters of the extra-virgin olive oil samples were measured in triplicate using a Minolta CR- Samples of extra-virgin olive oil were obtained from 400 colorimeter based on the CIE-L*a*b* color system. a local market in Lavras, Minas Gerais, Brazil. The samples (from the same mark and lot) were sold in 500 mL amber Volatile compound analysis glass bottles. No test has been carried out to attest the A headspace was created by heating 5 mL of extra- authenticity of product. virgin olive oil at 40 °C for 15 min in a 10.0 mL glass flask. For the heat treatments, 250 mL samples of extra- The compounds in the vapor phase were extracted by solid virgin olive oil were put in 1,000 mL beakers and heated in phase microextraction using a PDMS/DVD fiber. After 15 a temperature-controlled electric furnace (Layr model Jady) min, the fiber was injected in a gas chromatograph/mass for 2 h. The samples were heated at 50 °C, 100 °C, 150 °C, spectrometer (GCMS-QP2010 plus; Shimadzu, Kyoto, and 200 °C. An unheated reference sample also was Japan). The injection was made in splitless mode with prepared. After the heat treatment, the samples were helium as carrier gas at a flow rate of 1.0 mL min-1. The protected from light until analysis (after 24 h). injector temperature was 220 °C. A fused-silica capillary Sensory analysis column (5% phenyl-95% polydimethylsiloxane, 30 m × 0.25 mm, 0.25 m) was employed for separation of the The effect of heating on the sensory aspects of compounds. The oven temperature was programmed from extra-virgin olive oil was evaluated by a difference from 35 °C (for 2 min) to 250 °C at a rate of 5 °C min-1, and was the control test. This test was used to determine if there then maintained at 250 °C for 1 min. The mass spectrometer was, in fact, a difference between the test samples and the was used with electron ionization (70 eV) and a mass scan control, and if there was a difference, its size was also range from 40 to 600 Da. The temperatures of the ion source measured (MEILGAARD; CIVILLE; CARR, 2007; and the GC-MS interface were 200 °C and 230 °C, LAWLESS; HEYMANN, 2010). respectively. Compounds were identified by comparing First, a training test was given to regular consumers their mass spectra with GC/MS spectral libraries (Wiley 8 of extra-virgin olive oil. This type of tester was used in order and FFNSC 1.2 libraries). A comparison of relative retention to reproduce the effect of heating on the perception of index (obtained using a series of n-alkanes under the same common consumers of extra-virgin olive oil. So, expert olive operational conditions) with references from databases oil tasters were not employed. For the experiments, the (ADAMS, 2007; EL-SAYED, 2012; ACREE; ARN, 2012) was testers were asked to discriminate 3 samples (100% olive oil, also used for compound identification. The relative and 80% and 60% olive oil blended with soybean oil) from a abundance of the compounds was expressed as the relative control (100% olive oil) based on flavor and overall aspects chromatographic peak area (normalized area, %). using the following scale: 0 - no difference, 1 - very small Statistical analysis difference, 2 - small difference, 3 - small/moderate difference, 4 - moderate difference, 5 - moderate/large difference, 6 - The data from the sensory tests were analyzed by large difference, and 7 - very large difference. The experiments Dunnett’s test at the 5% significance level. The data from Ciênc. agrotec., Lavras, v. 37, n. 6, p. 566-572, nov./dez., 2013 568 NUNES, C. A. et al. the color characterization were analyzed by Tukey’s test RESULTS AND DISCUSSION at the 5% significance level. All calculations were Volatile compound profile performed using SensoMaker software (PINHEIRO; NUNES; VIETORIS, 2013).