Professional Documents
Culture Documents
Food Chemistry: P. Reboredo-Rodríguez, C. González-Barreiro, B. Cancho-Grande, J. Simal-Gándara
Food Chemistry: P. Reboredo-Rodríguez, C. González-Barreiro, B. Cancho-Grande, J. Simal-Gándara
Food Chemistry
journal homepage: www.elsevier.com/locate/foodchem
a r t i c l e i n f o a b s t r a c t
Article history: The influence of olive paste preparation conditions on the standard quality parameters, as well as volatile
Received 11 January 2014 profiles of extra virgin olive oils (EVOOs) from Morisca and Manzanilla de Sevilla cultivars produced in an
Received in revised form 21 February 2014 emerging olive growing area in north-western Spain and processed in an oil mill plant were investigated.
Accepted 24 February 2014
For this purpose, two malaxation temperatures (20/30 °C), and two malaxation times (30/90 min)
Available online 6 March 2014
selected in accordance with the customs of the area producers were tested. The volatile profile of the oils
underwent a substantial change in terms of odorant series when different malaxation parameters were
Keywords:
applied.
Extra-virgin olive oil
Malaxation
Ó 2014 Elsevier Ltd. All rights reserved.
Volatile compounds
Odour activity value (OAV)
Odorant series
http://dx.doi.org/10.1016/j.foodchem.2014.02.140
0308-8146/Ó 2014 Elsevier Ltd. All rights reserved.
P. Reboredo-Rodríguez et al. / Food Chemistry 158 (2014) 534–545 535
Table 1
Standard quality indices (free acidity; peroxide value; UV absorption characteristic, K270, K232, DK; waxes, trilinolein and DECN), fatty acids, sterols and triterpenic dialcohols
composition of the studied EVOOs.
Parameter 20 °C 30 °C
A. Morisca+Verdial de Badajoz (90:10%) 30 min 90 min 30 min 90 min
Acidity (%) 0.45 ± 0.01a 0.37 ± 0.01b 0.42 ± 0.00ab 0.52 ± 0.02c
Peroxides (meq. O2/kg oil)* 6.11–9.11 5.90–9.38 6.66–8.79 7.48–14.70
K232 1.68 ± 0.19a 1.69 ± 0.31a 1.71 ± 0.22a 1.86 ± 0.39a
K270 0.16 ± 0.03a 0.19 ± 0.01a 0.15 ± 0.01a 0.20 ± 0.01a
DK 0.0021 ± 0.0000a 0.0054 ± 0.0047ab 0.0022 ± 0.0001a 0.0130 ± 0.0000b
Waxes (mg/kg) 44.1 ± 1.6a 49.6 ± 4.9a 50.7 ± 6.2a 54.0 ± 0.0a
Trilinolein (%) 0.33 ± 0.12a 0.40 ± 0.04a 0.40 ± 0.06a 0.33 ± 0.07a
DECN 0.17 ± 0.02a 0.14 ± 0.01a 0.16 ± 0.05a 0.10 ± 0.13a
Fatty acid composition by GC (% m/m methyl esters)
Myristic C14:0 0.013 ± 0.002a 0.009 ± 0.001a 0.010 ± 0.001a 0.011 ± 0.001a
Palmitic C16:0 12.88 ± 0.00a 12.76 ± 0.19a 12.88 ± 0.23a 12.98 ± 0.08a
Palmitoleic C16:1 0.92 ± 0.02ab 0.88 ± 0.01a 0.94 ± 0.01ab 0.96 ± 0.01b
Margaric C17:0 0.061 ± 0.001a 0.056 ± 0.006a 0.067 ± 0.004a 0.064 ± 0.005a
Margaroleic C17:1 0.098 ± 0.003a 0.088 ± 0.004a 0.097 ± 0.005a 0.101 ± 0.001a
Stearic C18:0 3.04 ± 0.13a 2.97 ± 0.04a 2.99 ± 0.04a 2.98 ± 0.00a
Oleic C18:1 67.99 ± 0.31a 68.14 ± 0.25a 67.74 ± 0.28a 67.92 ± 0.04a
Linoleic C18:2 13.10 ± 0.07a 13.24 ± 0.02ab 13.41 ± 0.01b 13.16 ± 0.06a
Linolenic C18:3 0.91 ± 0.04a 0.92 ± 0.01a 0.91 ± 0.01a 0.89 ± 0.01a
Arachidic C20:0 0.48 ± 0.03a 0.48 ± 0.00a 0.49 ± 0.01a 0.46 ± 0.00a
Eicosenoic C20:1 0.29 ± 0.01a 0.28 ± 0.01a 0.28 ± 0.00a 0.28 ± 0.00a
Behenic C22:0 0.17 ± 0.02a 0.15 ± 0.00a 0.15 ± 0.00a 0.15 ± 0.01a
Lignoceric C24:0 0.063 ± 0.010a 0.053 ± 0.010a 0.068 ± 0.004a 0.059 ± 0.001a
trans oleics 0.015 ± 0.007a Traces 0.020 ± 0.000a 0.011 ± 0.000a
trans L+Ln 0.025 ± 0.007a 0.020 ± 0.000a 0.027 ± 0.004a 0.020 ± 0.000a
Sterols by GC relative amount (%)
Cholesterol 0.053 ± 0.010a 0.061 ± 0.027a 0.069 ± 0.001a 0.062 ± 0.002a
Brassicasterol Traces Traces Traces Traces
Campesterol 2.33 ± 0.01a 2.39 ± 0.02b 2.35 ± 0.01ab 2.32 ± 0.01a
Stigmasterol 1.14 ± 0.01a 1.02 ± 0.01b 1.12 ± 0.01a 1.33 ± 0.03c
Apparent b-Sitosterol 95.60 ± 0.31a 95.64 ± 0.20a 95.46 ± 0.24a 95.46 ± 0.23a
D7-Stigmastenol 0.12 ± 0.05a 0.15 ± 0.01b 0.18 ± 0.08a 0.10 ± 0.00c
Total sterols (lg/g) 1600.0 ± 34.0a 1342.6 ± 146.6a 1616.1 ± 55.1a 1596.5 ± 40.3a
Erythrodiol+Uvaol 3.29 ± 0.08a 3.13 ± 0.01a 3.48 ± 0.16a 3.63 ± 0.19a
Parameter 30 °C
B. Manzanilla de Sevilla+Unknown (95:5%) 30 min 90 min
Acidity (%) 0.25 ± 0.01a 0.28 ± 0.05a
Peroxides (meq. O2/kg oil)* 2.24–5.23 1.94–4.35
K232 1.45 ± 0.11a 1.38 ± 0.13a
K270 0.12 ± 0.03a 0.13 ± 0.01a
DK 0.0036 ± 0.0002a 0.0034 ± 0.0001a
Waxes (mg/kg) 34.5 ± 3.5a 42.9 ± 4.5a
Trilinolein (%) 0.07 ± 0.01a 0.11 ± 0.01a
DECN 0.06 ± 0.03a 0.13 ± 0.06a
Fatty acid composition by GC (% m/m methyl esters)
Myristic C14:0 0.014 ± 0.002a 0.011 ± 0.001a
Palmitic C16:0 10.80 ± 0.15a 11.15 ± 0.05a
Palmitoleic C16:1 0.86 ± 0.01a 0.87 ± 0.01a
Margaric C17:0 0.180 ± 0.057a 0.210 ± 0.014a
Margaroleic C17:1 0.280 ± 0.141a 0.285 ± 0.134a
Stearic C18:0 3.23 ± 0.08a 3.05 ± 0.08a
Oleic C18:1 78.80 ± 0.00a 77.66 ± 0.03b
Linoleic C18:2 4.11 ± 0.08a 4.96 ± 0.06b
Linolenic C18:3 0.80 ± 0.06a 0.81 ± 0.01a
Arachidic C20:0 0.43 ± 0.15a 0.43 ± 0.12a
Eicosenoic C20:1 0.30 ± 0.01a 0.33 ± 0.01a
Behenic C22:0 0.14 ± 0.04a 0.14 ± 0.01a
Lignoceric C24:0 0.072 ± 0.005a 0.116 ± 0.062a
trans oleics 0.023 ± 0.003a 0.022 ± 0.013a
trans L + Ln Traces Traces
Sterols by GC relative amount (%)
Cholesterol 0.050 ± 0.013a 0.068 ± 0.025a
Brassicasterol Traces Traces
Campesterol 2.30 ± 0.01a 2.61 ± 0.01b
Stigmasterol 0.54 ± 0.02a 0.62 ± 0.00b
Apparent b-Sitosterol 96.52 ± 0.08a 96.06 ± 0.09b
D7-Stigmastenol 0.12 ± 0.01a 0.15 ± 0.01a
Total sterols (lg/g) 1443.3 ± 54.2a 1503.4 ± 133.5a
Erythrodiol+Uvaol 2.02 ± 0.02a 2.00 ± 0.00a
Values are mean ± standard deviation (n = 2). Different letters within rows indicate statistical differences as per ANOVA (p < 0.05) and Tukey’s HSD test.
*
Peroxide values were determined three months apart.
P. Reboredo-Rodríguez et al. / Food Chemistry 158 (2014) 534–545 537
Table 2
Concentrations of volatile compounds of the studied EVOOs.
Table 2 (continued)
Values are mean ± standard deviation (n = 4). Different letters within rows indicate statistical differences as per ANOVA (p < 0.05) and Tukey’s HSD test. n.f.: not found.
of volatile compound in oil sample/odour threshold) of each com- category (acidity 6 0.8°; peroxide index 6 20 meq O2/kg;
pound assigned to this series. According to its aroma descriptors, a K270 6 0.22; K232 6 2.5; DK 6 0.01; Waxes 6 250 mg/kg; Trilino-
volatile compound can be included in one or several odorant series. lein < 0.5%; DECN 6 0.2).
The odour descriptors of C6 and C5 compounds that contribute There was an increase, in some cases significant, when either
to the sensory properties of EVOOs were taken from literature the malaxation temperature and/or time was risen (Table 1a, b)
(Angerosa, Mostallino, Basti, & Vito, 2000; Kalua et al., 2007; Tura, such it was observed in the case of Cornicabra variety (Inarejos-
Failla, Bassi, Pedò, & Serraiocco, 2008); and grouped in 9 different García et al., 2009). Ranalli, Contento, Schiavone, and Simone
odorant series: grass, leaf, wood, bitter-like, sweet-like, pungent- (2001) attributed this behaviour to the increase in activity of the
like (or rasping), olive fruit, apple and banana. Some compounds lipase enzymes (responsible for the increase of free acidity) and
were included in two or more odorant series. to an intensification of the primary oxidation processes (responsi-
ble for the increase of the K232 and peroxide index values) and the
2.4. Statistical analysis secondary oxidation processes (responsible for the increase of the
K270 and carbonyl index values) when malaxation temperature
Analysis of variance (ANOVA) was carried out using the rises.
statistical package Statgraphics Centurion XV for windows Version The fatty acid levels, as well as being in accordance with the limits
15.2.06 (Statistical Graphics Corp., Herndon, Va, USA). Tukey’s HSD mentioned in the EU Regulation for ‘extra virgin’ category (European
test was used as a single-step multiple comparison method in con- Union Commission, 1991, 2003), were not significantly influenced
junction with ANOVA to identify significantly different means. by both malaxation parameters (time and temperature) for both
Partial least squares (PLS) regression was implemented by using oil varieties (Morisca and Manzanilla de Sevilla) (Table 1a, b).
the statistical package Unscrambler v. 9.1 for Windows (CAMO Concerning sterols and the sum of erythrodiol and uvaol, ex-
Software, Oslo, Norway). pressed as sum of percentage of total sterols, it should be noted
that for both cultivars, Morisca and Manzanilla de Sevilla, no signif-
icant differences in total sterol composition and erythrodiol+uvaol
3. Results and discussion of oil samples were detected (Table 1a, b). Nevertheless, a trend is
observed by evaluating the effect of malaxation temperature in
3.1. Quality indices, fatty acid, sterol and triterpene dialcohols Morisca oils, higher contents of total sterols and triterpene dialco-
composition of EVOOs extracted at different malaxation conditions hols were observed when olive paste was malaxed at the highest
temperature (30 vs. 20 °C) (Table 1a). According to Allouche et al.
It is of great importance to deepen in the effect of the malaxa- (2010), this rise could be explained by the fact that higher temper-
tion conditions on the quality of the VOO produced in order to atures decrease the oil viscosity, thus the extraction of these com-
strike an appropriate balance between the economic turnover pounds from the olive paste is favoured.
and the quality of the commercial product (Inarejos-García et al.,
2009).
The analysed quality indices of the olive oil samples in the differ- 3.2. Effect of malaxation process on the volatile profile of EVOOs
ent malaxation conditions studied met the standards of the Euro-
pean Community for the classification as ‘extra virgin’ category Three branches of volatile C6 metabolites are generated from
(European Union Commission, 1991, 2011). All the oils from Morisca linolenic acid (LnA) and linoleic acid (LA) through the lipoxygenase
and Manzanilla de Sevilla analysed showed values below the upper (LOX) pathway. LOX transforms LnA and LA into their correspond-
limits established by EU Regulations for the extra virgin olive oil ing 9- and 13-hydroperoxides, in a ratio ranging between 65:35
P. Reboredo-Rodríguez et al. / Food Chemistry 158 (2014) 534–545 539
(a) C6 compounds 20 ºC
9000
8000 30 ºC
7000 20 ºC
6000
30 ºC
5000
ng/g oil
4000 20 ºC 30 ºC
3000
2000
1000
0
30 min 90 min 30 min 90 min 30 min 90 min 30 min 90 min 30 min 90 min 30 min 90 min
LnA compounds LA compounds Total compounds
2000 20 ºC
30 ºC
1500
20 ºC
ng/g oil
20 ºC 30 ºC
1000
500
0
30 min 90 min 30 min 90 min 30 min 90 min 30 min 90 min 30 min 90 min 30 min 90 min
LnA compounds LA compounds Total compounds
Fig. 1. (a) Sum of C6 volatile compounds in Morisca:Verdial de Badajoz (90:10%) oils at different malaxation process conditions: Temperature: 20/30 °C; Time: 30/90 min. (b)
Sum of C5 volatile compounds in Morisca:Verdial de Badajoz (90:10%) oils at different malaxation process conditions: Temperature: 20/30 °C; Time: 30/90 min. (c) Sum of C6
volatile compounds in Manzanilla de Sevilla:Unknown (95:5%) oils at different malaxation process conditions: Temperature: 30 °C; Time: 30/90 min. (d) Sum of C5 volatile
compounds in Manzanilla de Sevilla:Unknown (95:5%) oils at different malaxation process conditions: Temperature: 30 °C; Time: 30/90 min. Volatile content of C6/LnA
aldehydes is trans-2-hexen-1-al. Volatile contents of C6/LnA alcohols are the sum of: cis-2-hexen-1-ol, trans-2-hexen-1-ol, cis-3-hexen-1-ol and trans-3-hexen-1-ol. Volatile
contents of C6/LnA esters are the sum of: cis-3-hexenyl acetate and trans-2-hexenyl acetate. Volatile content of C6/LA aldehydes is hexanal. Volatile content of C6/LA alcohols
is hexanol. Volatile content of C6/LA esters is hexyl acetate. Volatile content of C5/LnA aldehydes is trans-2-pentenal. Volatile contents of C5/LnA alcohols are the sum of: 1-
penten-3-ol, cis-2-penten-1-ol and trans-2-penten-1-ol. A volatile content of C5/LnA ketones is 1-penten-3-one. Volatile content of C5/LA aldehydes is pentanal. Volatile
content of C5/LA alcohols is 1-pentanol. Volatile content of C5/LA ketones is 3-pentanone.
and 55:45, respectively. Only the 13-hydroperoxides, from both 3.2.1. Effect of malaxation time
LnA (13-HPOT) and LA (13-HPOD), are cleaved by hydroperoxide In our oils, an opposite behaviour for the most abundant C6 alde-
lyase (FAHL) into C12 oxo-acids, cis-3-hexenal and hexanal, as hydes, trans-2-hexenal and hexanal, is observed taking account the
the enzyme has a high substrate specificity. Enzymatic transforma- effect of time: in Morisca oils C6 aldehydes decreased in concentra-
tion of the two aldehydes mediated by isomerases (IR), alcohol tion with increasing times of olive paste kneading, such decreases
dehydrogenases (ADH) and alcohol acetyl transferases (AAT) yields were statistically significant (p < 0.05) at 30 °C (Table 2a, Fig. 1a).
the corresponding C6 esters and C6 alcohols. An additional branch In the case of Manzanilla de Sevilla oils, the trend differed com-
of short-chain green volatiles, including oxygenated C5 com- pletely (Table 2b, Fig. 1c) and was in good agreement with other
pounds, is biosynthesised through another LOX pathway. In this varieties such as the Italian Coratina and Frantoio (Angerosa et al.,
case, 13-HPOT undergoes a b-scission yielding pentene dimers 2001), Leccino, Dritta and Caroleo (Ranalli et al., 2003), the Spanish
and pentenols through the alkoxyl radical. The subsequent oxida- Cornicabra (Gómez-Rico, Inarejos-García, Salvador, & Fregapane,
tion of pentenols catalysed by an alcohol dehydrogenase yields 2009) and the Tunisian Chemlali and Chetoui (Youssef et al.,
C5 carbonyl compounds (Ranalli, Pollastri, Contento, Iannucci, & 2013). With these results, it is clear that the behaviour of enzymes
Lucera, 2003). pattern during malaxation is linked to the variety.
540 P. Reboredo-Rodríguez et al. / Food Chemistry 158 (2014) 534–545
C6 compounds
18000 (c)
Total compounds
16000
14000
10000
8000
6000
4000
2000
0
30 min 90 min 30 min 90 min 30 min 90 min
C5 compounds
3000 (d)
Total compounds
2500
2000
LnA compounds LA compounds
ng/ g oil
1500
1000
500
0
30 min 90 min 30 min 90 min 30 min 90 min
Fig. 1 (continued)
The content of C6 alcohols also experienced an increase with especially cis-2-penten-1-ol, was higher at prolonged malaxation
lengthy times for both varieties except trans-2-hexen-1-ol at low times (Table 2b).
temperatures (20 °C) for Morisca oils (Table 2a, b, Fig. 1a, c). In general terms, the total concentration of C6 volatiles in-
A considerable decrease was detected for C6 esters at 30 °C in creased with extended times of olive paste kneading for both stud-
both cultivars, especially for cis-3-hexenyl acetate (Table 2a, b, ied oils regardless of temperature (Fig. 1a, c). For C5 volatiles, this
Fig. 1a, c). Ranalli et al. (2003) attributed this behaviour to a pro- behaviour was maintained in the case of Manzanilla de Sevilla oils
gressive inactivation of AAT. (Fig. 1d) but not in the case of Morisca oils (Fig. 1b): C5 compounds
The concentrations of individually C5 compounds were influ- tended to decrease at high times.
enced differently by time adopted during the malaxation for both
varieties: for Morisca oils, ketones were the compounds that expe- 3.2.2. Effect of malaxation temperature
rienced the most significant changes, only at 30 °C. Thus, the con- Changes in malaxation temperature (at 20 and 30 °C) were eval-
centrations of 1-penten-3-one diminished drastically while the uated only with one cultivar (Morisca). According to Salas and
amount of 3-pentanone increased (Table 2a). Nevertheless, the Sánchez (1999) the malaxation temperature generally causes a
concentration of ketones in Manzanilla de Sevilla oils rarely varied; decrease of levels of volatile compounds from LOX pathways, as
on the other hand, the amount of LnA-alcohols in these oils, a consequence of proved inactivation of hydroperoxide lyases. This
P. Reboredo-Rodríguez et al. / Food Chemistry 158 (2014) 534–545 541
Fig. 2. (a) One-dimension PLS-2: scores plot for Morisca:Verdial de Badajoz (90:10%) oils extracted at 20/30 °C for 30/90 min (x), together with loadings plot of X-variables for
the 18 volatile descriptors (y) and loadings plot of Y-variables for the 9 aroma descriptors (z). One principal component accounted for 86% and 78% of the variance in X and Y
data, respectively. (b) One-dimension PLS-2: scores plot for Manzanilla de Sevilla:Unknown (95:5%) oils extracted at 30 °C for 30/90 min (x), together with loadings plot of X-
variables for the 18 volatile descriptors (y) and loadings plot of Y-variables for the 9 aroma descriptors (z). One principal component accounted for 97% of the variance in both
X and Y data, respectively.
Fig. 2 (continued)
trend was evidenced by other authors as well (Angerosa et al., from LnA (trans-2-hexenal, cis-3-hexen-1-ol, cis-3-hexenyl ace-
2001; Gómez-Rico et al., 2009; Kalua, Bedgood, Bishop, & Prenzler, tate, respectively) and LA (hexanal, 1-hexanol and hexyl acetate,
2006; Ranalli et al., 2001). respectively) decreased. Only an increase in C6/LnA-alcohols was
With prolonged times (90 min) most C6-compounds under- observed, the amount of trans-2-hexen-1-ol was higher at tested
went statistically significant variations when temperature is in- extreme temperatures and times: 30 °C and 90 min (Table 2a,
creased. In this sense, C6-aldehydes, alcohols and esters coming Fig. 1a).
542 P. Reboredo-Rodríguez et al. / Food Chemistry 158 (2014) 534–545
Fig. 2 (continued)
Fig. 2 (continued)
Nevertheless, interactions between malaxation time and observed at 30 °C, when time was set to 90 min C5/LnA compounds
temperature were observed for C5-compounds: the behaviour diminished and C5/LA compounds increased slightly (Fig. 1b).
of the majority compounds at short times (30 min) was opposite Angerosa et al. (2001) found the same trend for Coratina oils, with
to high times (90 min) when temperature was changed the exception of 1-penten-3-one, although these authors assessed
(Table 2a). only C5/LnA compounds. In a previous paper, the same authors
In conclusion, the total concentration of C6 volatiles decreased (Morales, Angerosa, & Aparicio, 1999) highlighted that the
with high temperatures regardless of paste kneading time production of 1-penten-3-one increased with temperature regard-
(Fig. 1a). For C5 volatiles, when malaxation time was set to less malaxation time, suggesting this volatile is produced through
30 min an increase in the total amount of C5 compounds was an oxidation process.
P. Reboredo-Rodríguez et al. / Food Chemistry 158 (2014) 534–545 543
Fig. 2 (continued)
Fig. 2 (continued)
3.3. One-dimension partial least squares regression (PLS2) between Two PLS2 modelling (one for Morisca and another for Manzanil-
volatile compounds and odorant series la de Sevilla oils) between two data matrices (both volatile com-
pounds and odorant series) were performed providing in both
To estimate quantitatively the overall oil aroma, a method cases one-factor or 1D model. The models were evaluated by cross
based in the addition of OAVs was employed. This procedure validation via the root mean square error for predictions (RMSEP),
makes it possible to relate quantitative information obtained by which was calculated to be lower than 10 in both cases. In general,
chemical analysis to sensory perception, providing a tentative aro- there were found significant positive and negative correlations
ma profile (Sánchez-Palomo E & Alonso-Villegas R, 2010). (r = |0.7–1.0|) amongst many of the data of both matrices.
544 P. Reboredo-Rodríguez et al. / Food Chemistry 158 (2014) 534–545
Connecting 18 volatile compounds with 9 aromatic series in The sensory profile of oils from Morisca obtained at 30 °C and
Morisca oils extracted at different malaxation conditions (20 or 90 min changed with respect to shorter times, thus olive and
30 °C for 30 or 90 min) resulted in two different groups of oils. banana fruits were the characteristic aromatic series instead.
The other two groups of oils were remaining together in the middle For Manzanilla de Sevilla the sensory profile changed to apple,
of both extreme groups (Fig. 2a(x)). The findings obtained can be sweet-like, bitter-like and leaf notes.
summarised as follows:
1. According to the scores figure (Fig. 2a(x)), the upper half only Acknowledgements
included the Morisca oils extracted at 30 °C for 30 min, while
the lower half mainly included the Morisca oils extracted at This work was funded by EU FEDER, and also under contracts
30 °C for longer times (90 min). However, along the middle 09TAL045E (Xunta de Galicia and Aceites Abril S.L.) and 2009/
baseline of 0 were placed the non-differentiated groups of 060 (Xunta de Galicia). The authors are grateful to Aceites Abril
Morisca oils extracted at 20 °C for both 30 and 90 min. S. L., and especially indebted to J. M. Pérez-Canal and F. Osorio-
2. According to the X- and Y-loadings figures (Fig. 2a(y), Fig. 2a(z)), Rodríguez.
for the highest values of PC1, Morisca/30 °C/30 min oils
were mainly associated to the following volatile compounds:
1-penten-3-one, trans-2-hexenal and cis-3-hexenyl acetate, References
and to the odorant series: bitter-like, pungent-like, leaf, apple
AAO-Agencia para el aceite de oliva (2013). Available at: http://aplicaciones.
and grass. For the lowest values of PC1, Morisca/30 °C/90 min
magrama.es/pwAgenciaAO/OlivarEspanol.aao?opcion_seleccionada=2100&control
oils were mainly associated to the volatiles trans-2-hexen-1- _acceso=S&idioma=ESP. Accessed 11 June 2013
ol, 1-hexanol and 3-pentanone, and to the odorant series olive Allouche, Y., Jiménez, A., Uceda, M., Paz Aguilera, M., Gaforio, J. J., & Beltrán, G.
and banana fruits. Morisca/20 °C/30 or 90 min oils were more (2010). Influence of olive paste preparation conditions on virgin olive oil
triterpenic compounds at laboratory-scale. Food Chemistry, 119(2), 765–769.
similar to Morisca/30 °C/90 min oils. Angerosa, F., Mostallino, R., Basti, C., & Vito, R. (2000). Virgin olive oil odour notes:
Their relationships with volatile compounds from the lipoxygenase pathway
A clear separation of two groups of Manzanilla de Sevilla oils and secoiridoid compounds. Food Chemistry, 68(3), 283–287.
Angerosa, F., Mostallino, R., Basti, C., & Vito, R. (2001). Influence of malaxation
was obtained (Fig. 2b) by linking 18 volatile compounds with 9 temperature and time on the quality of virgin olive oils. Food Chemistry, 72(1),
aromatic series: 19–28.
Aparicio, R., & Harwood, J. (2003). Manual del aceite de oliva (1st ed.). Madrid: AMV
1. According to scores figure (Fig. 2b(x)), the upper half only Ediciones, Mundi-prensa.
Boselli, E., Di Lecce, G., Strabbioli, R., Pieralisi, G., & Frega, N. G. (2009). Are virgin
included Manzanilla de Sevilla oils extracted at 30 °C for olive oils obtained below 27 °C better than those produced at higher
30 min, while the lower half mainly included Manzanilla de temperatures? LWT – Food Science and Technology, 42(3), 748–757.
Sevilla oils extracted at the same temperature for longer times Clodoveo, M. L. (2012). Malaxation: Influence on virgin olive oil quality. Past,
present and future – An overview. Trends in Food Science and Technology, 25(1),
(90 min). 13–23.
2. According to the X- and Y-loadings figures (Fig. 2b(y), Fig. 2b(z)) European Union Commission (1991). The characteristics of olive oil and olive-
for the highest values of PC1, Manzanilla de Sevilla/30 °C/30 min residue oil and on the relevant methods of analysis. Official Journal of the
European Communities. Regulation EEC/2568/91. § L 248.
oils were mainly associated to the volatiles cis-3-hexenyl acetate,
European Union Commission (2003). The characteristics of olive oil and olive-
hexyl acetate and pentanal, and to the odorant series banana, residue oil and on the relevant methods of analysis. Official Journal of the
olive, grass and wood. For the lowest values of PC1, Manzanilla European Communities. Regulation EC/1989/2003. § L 295.
European Union Commission (2007). The characteristics of olive oil and olive-
de Sevilla/30 °C/90 min oils were mainly associated to the vola-
residue oil and on the relevant methods of analysis. Official Journal of the
tiles trans-2-hexen-1-ol, trans-2-hexenal and hexanal, and to European Communities. Regulation EC/702/2007. § L 161.
the aromatic series apple, sweet-like, bitter-like and leaf. European Union Commission (2011). The characteristics of olive oil and olive-
residue oil and on the relevant methods of analysis. Official Journal of the
European Communities. Regulation EC/61/2011. § L 23.
4. Conclusions European Union Commission (2012). Marketing standards for olive oil. Official
Journal of the European Union. Implementing Regulation (EU) N° 29/2012. § L
The results obtained in this work shows that it is possible to 12.
Gómez-Rico, A., Inarejos-García, A. M., Salvador, M. D., & Fregapane, G. (2009). Effect
modulate the volatile fraction of an oil in accordance with malax- of malaxation conditions on phenol and volatile profiles in olive paste and the
ation temperature ranging from 20 to 30 °C and above all malaxa- corresponding virgin olive oils (Olea europaea L. Cv. Cornicabra). Journal of
tion time ranging from 30 min to 90 min. Agricultural and Food Chemistry, 57(9), 3587–3595.
Inarejos-García, A. M., Gómez-Rico, A., Salvador, M. D., & Fregapane, G. (2009).
The total concentration of C6 volatiles increased with extended Influence of malaxation conditions on virgin olive oil yield, overall quality and
times of olive paste kneading for both oils regardless of tempera- composition. European Food Research and Technology, 228(4), 671–677.
ture. For C5 volatiles, this behaviour was maintained in the case IOOC-International Olive Oil Council (1984). Document No 6.
Kalua, C. M., Allen, M. S., Bedgood, D. R., Jr., Bishop, A. G., Prenzler, P. D., & Robards,
of Manzanilla de Sevilla oils but not in the case of Morisca oils. Con-
K. (2007). Olive oil volatile compounds, flavour development and quality: A
cerning temperature conditions, the total concentration of Morisca critical review. Food Chemistry, 100(1), 273–286.
C6 volatiles decreased with 30 °C regardless of paste kneading time. Kalua, C. M., Bedgood, D. R., Jr., Bishop, A. G., & Prenzler, P. D. (2006). Changes in
volatile and phenolic compounds with malaxation time and temperature during
Nevertheless, for C5 volatiles, when malaxation time was set to
virgin olive oil production. Journal of Agricultural and Food Chemistry, 54(20),
30 min an increase in the total amount of C5 compounds was ob- 7641–7651.
served, and when time was set to 90 min C5/LnA compounds Morales, M. T., Angerosa, F., & Aparicio, R. (1999). Effect of the extraction conditions
diminished and C5/LA compounds increased slightly. of virgin olive oil on the lipoxygenase cascade: Chemical and sensory
implications. Grasas y Aceites, 50(2), 114–121.
A clear difference was found between oils processed at 30 °C/ Peinado, R. A., Mauricio, J. C., & Moreno, J. (2006). Aromatic series in sherry wines
30 min and 30 °C/90 min for both varieties in terms of odorant with gluconic acid subjected to different biological aging conditions by
series: Saccharomyces cerevisiae var. capensis. Food Chemistry, 94(2), 232–239.
Ranalli, A., Contento, S., Schiavone, C., & Simone, N. (2001). Malaxing temperature
affects volatile and phenol composition as well as other analytical features of
The oils from Morisca obtained at 30 °C and 30 min were char- virgin olive oil. European Journal of Lipid Science and Technology, 103(4),
acterised mainly by bitter-like, pungent-like, leaf, apple and 228–238.
Ranalli, A., Pollastri, L., Contento, S., Iannucci, E., & Lucera, L. (2003). Effect of olive
grass odorant series, while for Manzanilla de Sevilla oils, fruity paste kneading process time on the overall quality of virgin olive oil. European
(banana, olive), grass and wood notes predominated. Journal of Lipid Science and Technology, 105(2), 57–67.
P. Reboredo-Rodríguez et al. / Food Chemistry 158 (2014) 534–545 545
Reboredo-Rodríguez, P., González-Barreiro, C., Cancho-Grande, B., & Simal-Gándara, wines from the La Mancha region by odour activity values. Flavour and
J. (2012). Dynamic headspace/GC-MS to control the aroma fingerprint of extra- Fragrance Journal, 25(6), 456–462.
virgin olive oil from the same and different olive varieties. Food Control, 25(2), Stefanoudaki, E., Koutsaftakis, A., & Harwood, J. L. (2011). Influence of malaxation
684–695. conditions on characteristic qualities of olive oil. Food Chemistry, 127(4),
Reboredo-Rodríguez, P., González-Barreiro, C., Cancho-Grande, B., & Simal-Gándara, 1481–1486.
J. (2013a). Concentrations of aroma compounds and odor activity values of Taticchi, A., Esposto, S., Veneziani, G., Urbani, S., Selvaggini, R., & Servili, M. (2013).
odorant series in different olive cultivars and their oils. Journal of Agricultural The influence of the malaxation temperature on the activity of
and Food Chemistry, 61(22), 5252–5259. polyphenoloxidase and peroxidase and on the phenolic composition of virgin
Reboredo-Rodríguez, P., González-Barreiro, C., Cancho-Grande, B., & Simal-Gándara, olive oil. Food Chemistry, 136(2), 975–983.
J. (2013b). Effects of sedimentation plus racking process in the extra virgin olive Tura, D., Failla, O., Bassi, D., Pedò, S., & Serraiocco, A. (2008). Cultivar influence on
oil aroma fingerprint obtained by DHS-TD/GC-MS. Food and Bioprocess virgin olive (Olea europea L.) oil flavor based on aromatic compounds and
Technology, 6(5), 1290–1301. sensorial profile. Scientia Horticulturae, 118(2), 39–148.
Salas, J. J., & Sánchez, J. (1999). The decrease of virgin olive oil flavor produced by Youssef, O., Mokhtar, G., Abdelly, C., Mohamed, S. N., Mokhtar, Z., & Guido, F. (2013).
high malaxation temperature is due to inactivation of hydroperoxide. Journal of Changes in volatile compounds and oil quality with malaxation time of Tunisian
Agricultural and Food Chemistry, 47(3), 809–812. cultivars of Olea europea. International Journal of Food Science and Technology,
Sánchez-Palomo, E., Gómez García-Carpintero, E., Alonso-Villegas, R., & González- 48(1), 74–81.
Viñas, M. A. (2010). Characterization of aroma compounds of Verdejo white