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Research Article

Received: 19 January 2016 Revised: 24 June 2016 Accepted article published: 6 July 2016 Published online in Wiley Online Library: 1 August 2016

(wileyonlinelibrary.com) DOI 10.1002/jsfa.7883

Influence of olive ripening degree and crusher


typology on chemical and sensory
characteristics of Correggiolo virgin olive oil
Lucia Morrone,a Sabrina Pupillo,b Luisa Neri,a Giampaolo Bertazza,a
Massimiliano Maglia and Annalisa Rotondia*

Abstract
BACKGROUND: In this study, two types of crusher, hammer and blade, were used to produce olive oils from cv. Correggiolo
olives at four stages of ripeness, to analyse the effect of these two factors on oil quality indices (free acidity, peroxide value,
UV absorption), on phenolic compounds content and sensory profiles. Differences in chemical and sensory data were analysed
by two-way ANOVA.

RESULTS: Ripeness exerted a stronger influence than the crushing equipment on quality indices, phenolic content and
sensory evaluation; moreover the statistical significance of interaction between the factors considered suggests that they are
intertwined. Differences in the texture of olive pastes obtained by squashing and crushing were clearly evident at the first stage
of ripeness via observation with a scanning electron microscope. The stronger mechanical action of the hammer crusher also
produced smaller pit fragments compared to the blade crusher, as shown by particle size analysis of the kernels fragments.

CONCLUSION: Knowledge about the interaction between ripening and crushing will allow olive oil producers to pursue a product
of the quality most suitable for a particular type of consumer. For example, bitterness and pungency, characters recently
connected with health effects because sensory markers of extra virgin olive oil (EVOO) polyphenols, do not have a great sensory
appeal for most consumers; however, there is a niche of gourmet estimators interested in these peculiar flavours and ready
to pay a premium price for them. The producer will be able to customise the EVOO by modulating its chemical and sensory
characteristics, especially the phenolic fraction, thus addressing the needs of consumers with different tastes.
© 2016 Society of Chemical Industry

Supporting information may be found in the online version of this article.

Keywords: extra virgin olive oil; ripeness; typologies of crushers; storage; SEM

INTRODUCTION and the production of oils characterised by a lower level of bitter-


Extra virgin olive oil (EVOO) is obtained from olives only by ness and thus less interesting from an health point of view even
mechanical or other physical means. It is one of the few vegetable if appreciated by consumers. In order to overcome the disadvan-
oils that can be consumed without refining, and has an important tages of the stone mill, different types of crusher have been devel-
economic relevance. EVOO consumption in the world is increasing oped, such as the hammer crusher, blade crusher and toothed disc
thanks to its nutritional value1 and its peculiar aroma, both due to crusher. All these typologies can be part of a continuous process,
minor components such as phenolic and volatiles compounds.2,3 while the energy released in the crushing chamber is different for
These classes of compounds originate during the extraction pro- each crusher, resulting in a different increase of the olive paste
cess pointing out how extraction is crucial for the EVOO quality.4,5 temperature.8
The olive processing consists of several technological steps such Several studies in last few years compared different typologies
as crushing, kneading, malaxing, filtration and packaging, with of olive crushers; some of them9 – 11 studied the changes in EVOO
each step able to affect the final quality of the product. Crushing
and malaxation are the most important steps and influence both
yield and quality of the oil extracted.6 In fact, during these steps the ∗ Correspondence to: A Rotondi, Institute of Biometeorology – National
biogeneration and transformation of phenolic compounds starts Research Council, Via Gobetti 101, 40129 Bologna, Italy.
and is carried out by the enzymes 𝛽-glucosidase and esterase, and E-mail: a.rotondi@ibimet.cnr.it
oxidative enzymes such as polyphenol oxidase, peroxidase and
a Institute of Biometeorology, National Research Council, Via Gobetti 101, 40129
lipooxygenase.7
Bologna, Italy
The stone mill was the first crusher used to obtain olive oil;
this typology of crusher is still used nowadays but it has some b Department of Food Science, University of Parma, Parco Area delle Scienze,
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disadvantages such as the low working capacity, the yield rate 59/a, 43124, Parma, Italy

J Sci Food Agric 2017; 97: 1443–1450 www.soci.org © 2016 Society of Chemical Industry
www.soci.org L Morrone et al.

produced by the use of the stone mill crusher and hammer crusher; an Edwards S150B sputter coater (Sussex, UK), and the processed
others6,8 compared the hammer crusher to the disc crusher; Prez- samples were observed with a field emission scanning microscope
iuso et al.12 compared the blade crusher to the stone mill while (LEO 1530; Zeiss, Oberkochen, Germany) operated at an accelera-
other authors13,14 focused on the effects of the hammer crusher tion voltage of 5 kV. A total of 80 observations were carried out for
with respect to the blade crusher. However, to our knowledge no each crushing system.
study has been focused so far on the interactions between the
two variables crushing and olive ripeness. The different degree Pit particles size analysis
of ripeness affects significantly the chemical characteristics of A volume of 80 mL of olive paste for each sample was collected
EVOO,15 – 17 and the impact of the fruit ripening stage on the oil after crushing for particle size analysis of kernels fragments that
chemical composition is greater than the impact ascribable to the was performed by the computerised image analysis system Leica
fruit variety itself.18 In addition, the chemical changes occurring in Application Suite (Leica, Hamburg, Germany). Parameters of area,
oils during storage are influenced by the initial chemical compo- length and width for each kernel fragment were recorded for
sition of the oil19 and by the oxidative process involving phenols each extraction batch. Seven hundred fragments of kernels were
that occurs normally in the oils and could be accelerated by the subjected to image analysis for every kind of crushing system.
processing steps.20
The aim of this work was to compare olive oils produced using
Analytical indices
two crushing systems at four different stage of olive ripeness in
Free acidity, peroxide value, and UV-spectrophotometric indices
order to better understand the mutual influence of those two fac-
(K 232 , K 270 ,) were evaluated according to the official methods
tors on the chemical and sensory properties of EVOO. Furthermore,
described in Regulation EEC 2568/9123 and following amend-
the chemical and sensory analyses were repeated 6 months after
ments of the Commission of the European Union. All parameters
crushing to check the evolution of EVOO chemical and sensory
were calculated in triplicate for each sample.
characteristics during storage.

Analysis of the phenolic fraction


MATERIALS AND METHODS The phenolic fraction was extracted in triplicate according to Pirisi
Plant material et al.24 with some modifications: 8 g of oil sample were added
The research was carried out on olive plants of the cultivar Cor- to 4 mL of n-hexane and 8 mL of a methanol/water (60:40, v:v)
reggiolo cultivated in an experimental field in the Emilia Romagna solution; after vigorous shaking, the hydro-alcoholic phase was
Region, Italy. The olive drupes were manually harvested from eight collected and the extraction was repeated twice. The combined
20-year-old trees at four different stages of ripeness, starting on 18 extracts were evaporated to dryness, suspended in 1 mL of a
October 2013 and ending on 12 December 2013. Considering that methanol/water (50:50, v:v) solution and filtered through a 0.2 μm
the optimal ripening index for the Correggiolo cultivar is included RC (Whatman Inc., Clifton, NJ, USA); the samples were then sub-
in the range 2–2.5 of the Jaén index,21 as stated by Rotondi and jected to spectroscopic determination of total phenols, analysis of
Magli,22 the harvesting dates were designed in order to obtain an free radical scavenging activity and chromatographic analysis by
early, two medium and one late stage of ripeness. HPLC-DAD.
The total phenol content of the hydro-alcoholic extracts was
determined by the Folin–Ciocalteu spectrophotometric method
Olive processing and storage of the oils at 750 nm (Jasco Spectrophometer V-500; Jasco, Tokyo, Japan), and
For drupes crushing, a low scale mill (Olio Mio Baby 50; Toscana the results were expressed as mg gallic acid kg−1 oil.25
Enologica Mori, Firenze, Italy) with the possibility to be equipped The HPLC analyses of phenolic fraction was carried out using a
with both a hammer and a blade crusher, and characterised HPLC system equipped with pump LC-10 AD VP (Shimadzu, Kyoto,
by an horizontal kneader and two phase decanters, was used. Japan), a degasser Gastorr 154 (Flom, Tokyo, Japan), a low pres-
Both hammer and blade crushers have three crushing members, sure gradient unit FCV-10Alvp (Shimadzu, Kyoto, Japan), column
the grid that contained the crushing chamber had holes with a oven CTO-10A (Shimadzu, Kyoto, Japan), a rheodyne injector with
diameter of 5 mm and the angular velocity for both the crushers a 20 𝜇L loop and diode-array UV–visible detector (DAD) UV 6000
was set at 2800 rpm. (ThermoQuest, San Josè, CA, USA). Analytes were separated on a
The temperature (24 ∘ C) and time of malaxation (20 min), the Kinetex 5 μ C18 150 × 4.6 mm (Phenomenex, Torrance, CA, USA)
speed of the decanter (4200 rpm) and the flux of water in the column and revealed at wavelengths of 280 nm and 330 nm. The
separator (0.8 L h−1 ) were standardised in order to minimise the mobile phase flow rate was 1 mL min−1 and the gradient elu-
variability due to the extraction procedures. Oils samples were tion used was in accordance with Rotondi et al.17 The quantifica-
filtered through cotton filters, poured in dark glass bottles and tion of the oleuropein and ligstroside derivatives was performed
stored in a temperature controlled cupboard set at 15 ± 1 ∘ C. using oleouropein glucoside calibration curve; hydroxytyrosol was
quantified using tyrosol calibration curve while tyrosol, luteolin
Scanning electron microscopy and apigenin were quantified using the calibration curves of their
A sample of olive paste (20 mL) was taken at the exit of the relative analytical standard.
crusher chamber for each of the eight batches; olive paste sam-
ples were fixed in glutaraldehyde in 0.1 mmol L−1 phosphate buffer Sensory analysis
(pH 7.2), completely dehydrated through submersions in a series Sensory analysis was performed by the panel of Agency for Agro-
of increasing concentration of ethanol solutions, and finally dehy- food Section Services of Marche region (ASSAM), a fully-trained
drated in carbon dioxide using a CPD processor (CPD 030; Balz- analytical taste panel recognised by the International Olive Oil
ers, Schalksmühlen, Germany). All dried specimens were mounted Council (IOC) of Madrid, Spain, and by the Italian Ministry for Agri-
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on stubs using double-sided sticky tape and coated with gold in culture, Food, and Forestry Policy. Since the main objective of

wileyonlinelibrary.com/jsfa © 2016 Society of Chemical Industry J Sci Food Agric 2017; 97: 1443–1450
Hammer vs. blade crusher at four olive ripeness stages www.soci.org

the sensory UE method 2568/91 and following revision (EC Reg.


796/02) is to give a commercial classification of the oils, a panel
test was established for the present study using a standard profile
sheet (IOC/T20)26 modified by IBIMET-CNR,27 which allows a more
complete description of the organoleptic properties of the sam-
pled oils to be obtained, including secondary positive flavours.

Statistical analysis
Data were processed using SAS software 9.3 (SAS Institute Inc.,
Cary, NC, USA). The significant differences in pit particle size as well
as in the ripening stages between the two types of crushers under
study were tested by the analysis of variance (ANOVA) followed
by a Tukey’s Honestly Significant Difference (HSD) test. Chemical
and sensory data were analysed using statistical procedure based
on the analysis of variance by a complete factorial design in
order to examine treatment interdependencies (crusher system
and ripeness).

RESULTS AND DISCUSSION


Scanning electron microscopy and pit particle size analysis
The scanning electron microscopy (SEM) observations of the olive
paste samples obtained from fruits at the first stage of ripeness and
processed with the blade crusher revealed a good preservation
of the cellular structures, indeed the cellular lumes are easily
recognisable (Fig. 1a). Contrarily, in the olive paste processed
with the hammer crusher it was not possible to recognise a
structural organisation of tissues, since the cells are squashed and
Figure 1. SEM micrograph of olive paste treated with blade crusher (A) and
collapsed (Fig. 1b). These noteworthy differences in olive paste hammer crusher (B) at the first stage of ripeness.
processed with the two crushing systems were detectable only
at the first stage of ripeness, while no differences were found in
samples collected at the following stages, probably due to the Chemical characteristics of the oils
action of the pectolytic enzymes that start to degrade the middle The analytical indices of extra virgin olive oils produced in this
lamella, causing a loss of consistency of the olive fruit during study are listed in Table 1. Very similar values both of free acidity
the ripening process. In contrast with our findings Veillet et al.,11 and peroxide number were recorded for the two types of crusher,
comparing via SEM olive paste samples milled using stone mill as reported in other works.13,14 An increasing trend in free acid-
and hammer crusher, observed a very good conservation of the ity was observed as the olive ripening proceeded, even if the val-
cellular structures in samples processed by a hammer crusher ues stayed within the legal limits of 0.8% oleic acid, while no clear
compared to samples crushed by stone mill, where a destruction trend was found for the peroxide value (POV), in agreement with
of the intercellular structures for the flattening action of the stone other studies.17 POV is an indicator of the primary oxidation with
mill was observed. The structural differences we observed may be a legal limit for EVOO of 20 mEq O2 kg−1 of oil. An ANOVA pro-
imputable to the more violent action of the hammer compared to cedure by complete factorial design was carried out in order to
the blades. evaluate the interdependencies of the factors (1) crusher typology
The results of the granulometric analysis of kernel fragments and (2) ripening index on the EVOO chemical parameters. Table 1
derived from the two different crushing systems are shown in shows that all parameters, except K 232 and K 270 , are affected almost
Fig. 2. Since no significant differences were found in area, length exclusively by ripeness. K 232 and K 270 are indexes primarily used to
and width of kernel fragments collected at the four stages of detect frauds, with the legal limits for EVOO of 2.5 for K 232 and 0.2
ripeness the samples were all considered replicas so the resulting for K 270 . K 232 is also used as an indicator of olive oil primary oxida-
differences are imputable only to the type of crusher used. The tion during maturation28 and its variability, expressed as percent-
hammer crusher exerted a more violent action causing the pit age of the total sum of the squares, is 61% due to ripeness and 35%
to rupture in smaller fragments than in the case of the blade due to the type of crusher used, while K 270 , indicative of secondary
crusher, at all ripening stages. In fact the mean value of pit area oxidation, is influenced mostly (85%) by the type of crusher. No
obtained with the use of hammer crusher was 0.12 cm2 compared interaction between the two factors have been underlined, thus
to the mean pit area of 0.28 cm2 observed in samples milled by the changes of those spectrophotometric constants during mat-
the blade crusher. The length and width of pit fragments produced uration are independent from the type of crusher. The values of
by the hammer crusher were also statistically smaller than the the analytical indices recorded after 6 months of oils storage (T 6 )
ones of fragments obtained by the blade crusher. These results were on the whole higher than the values recorded before stor-
are in agreement with those obtained by Caponio and colleagues6 age (Table 1). In particular, the variability of free acidity parame-
who related the violence of the crusher, measured by the energy ter for extraction system raised from 0.98% in oils analysed before
developed during the step of pressing, to the size of the kernel storage (T 0 ) to 27.56% in oils analysed after 6 months of storage
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fragments. (T 6 ) (Table 1). This increase in the incidence of the crushing factor,

J Sci Food Agric 2017; 97: 1443–1450 © 2016 Society of Chemical Industry wileyonlinelibrary.com/jsfa
www.soci.org L Morrone et al.

Figure 2. Box plots of area (cm2 ), length (cm) and width (cm) of the pit fragments obtained by milling olive fruits with the use of two types of crusher,
blade and hammer. The line within the box marks indicates the median, and the symbol ⧫ indicates the mean; the box plot outliers are designated by •.

albeit lower than the incidence of maturation factor, is due to the increased during storage due to the interaction between the two
greater increase in free acidity values during oil storage (from T 0 ANOVA factors, meaning that during storage the weight of the
to T 6 ) observed in oils obtained by hammer crusher compared to interaction between type of crusher and olive ripening degree
free acidity in oil produced with blade crusher. Moreover the gap became stronger (Table 1).
between the values of free acidity grows as the ripening proceeds The results from the HPLC analysis of phenolic compounds of
(from 3% at RI to 34% at RIV). The fatty acid fraction was affected the Correggiolo oils produced at four different stages of ripen-
almost exclusively by the ripeness factor (Table S1, in the support- ing with two different types of crusher are listed in Table 2. At
ing material). T 0 the hydroxytyrosol content is higher in the oils produced with
The total phenolic content measured at T 0 shows a clear decreas- the hammers crusher at all the dates but at the fourth stage
ing trend during maturation (Table 1), as reported in literature;15,17 of ripeness (RIV) the difference is very marked, almost 3.5 times
in fact, by analysis of variance, in the case of total phenolic content, higher, making the trend of the hydroxytyrosol content a parabolic
the degree of ripening accounted for 86.8% of variation; the fac- curve. This particular trend suggested an increase of the hydrolytic
tor of crushing and the interaction between factors accounted for events at the expense of secoiridoids emphasised by ripeness
only 9% and 4% respectively (Table 1). Nevertheless, it is interest- in the oil milled with the hammer crusher; indeed, even if the
ing to underline the increasing difference in the phenolic content maturation parameter was responsible for the greatest percent-
between the two types of crusher; at the first two dates of collec- age of variability, it is interesting to underline that the interaction
tion (RI and RII) the oils produced with the hammer crusher is 8% between the factors ripeness and crusher typology was highly sig-
and 6% respectively richer in phenols than the oils produced with nificant (P < 0.001) (Table 2). The analysis at T 6 confirmed overall
the blade crusher, the oil produced with the hammer crusher at the the trend recorded at T 0 but for both crusher typologies there was
third date (RIII) is 20% richer and finally at the last date of ripening an increase in the hydroxytyrosol content (Table 2) due to the lysis
(RIV) is 57% richer than the oil produced with the blade crusher. of the oleuropein derivatives, since hydroxytyrosol is the phenol
These results show the existence of an interaction between the characterised by the highest antioxidant activity in olive oil.31 At
ripening degree factor and the crushing factor, as also results from T 0 the content in tyrosol was characterised by the same trend of
the complete factorial analysis (Table 1). Di Giovacchino et al.29 the content in hydroxytyrosol. At the firsts two dates (RI and RII)
suggested that the higher content in phenolic substances of oils the tyrosol content was very similar between the hammer and the
obtained from ‘violent’ crushers is due to complete rupture of the blade crusher, while from the third date (RIII) the gap between
pulp, moreover Preziuso et al.12 suggested a role of the pieces of the two crushers increased up to 54% (Table 2). During oil storage
stone in a quick attainment of the equilibrium of the concentra- the tyrosol content remained essentially constant, in accordance
tions of the phenolic substances in the aqueous and in the oily with Lozano-Sánchez et al.32 The oils produced using the hammer
phase; our results are in agreement with those reported by these crusher was always richer in secoiridoid compounds than the ones
authors. produced with the blade crusher and, as for the phenol alcohols,
After 6 months of storage the total phenols content increased as the maturation proceeds, the difference in secoiridoids con-
due to the lysis of complex phenols leading to the release of tent became greater, demonstrating the interaction between the
low molecular weight phenols, in agreement to Boselli and crushing and ripening index factors; this interaction explained the
colleagues.30 The increase in the phenol content after storage in 12.69% of the variability by ANOVA procedure (P > 0.01) (Table 2).
the oil produced with the blade crusher was remarkably higher, The presence of secoiridoids in olive oil is due to the activity of
especially at the first stage of ripening when an increase of 22% in several enzymes such as esterases and glucosidases activating dur-
total phenols content was recorded in the oil produced with the ing the tissues physical damage, thus the enzymatic activity is
blade crusher, compared to an increase of 3% in the oil produced crucial for the olive oil quality3 and probably influenced by the
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with the hammer crusher. The variance for total phenolic content crushing parameters. Moreover other studies,33,34 found that the

wileyonlinelibrary.com/jsfa © 2016 Society of Chemical Industry J Sci Food Agric 2017; 97: 1443–1450
Table 1. Analytical characteristics of Correggiolo oils and treatment interdependences of factorial design

J Sci Food Agric 2017; 97: 1443–1450


T0 T6
Parameter Free aciditya POV b K 232 K 270 TPc Free aciditya POVb K 232 K 270 TPc

RI
Blade 0.27 ± 0.01b 7.54 ± 0.15c 2.14 ± 0.07a, b 0.20 ± 0.01c 689.8 ± 11.0b 0.34 ± 0.03b, c 10.46 ± 0.79c,d 2.43 ± 0.21a 0.29 ± 0.09a 845.1 ± 32.3a
Hammer 0.28 ± 0.01a, b 8.47 ± 0.22b 2.26 ± 0.03a 0.27 ± 0.01a 746.1 ± 0.01a 0.35 ± 0.02a, b 11.43 ± 0.18b,c,d 2.32 ± 0.05a – c 0.28 ± 0.04a 770.1 ± 82.9a
RII
Hammer vs. blade crusher at four olive ripeness stages

Blade 0.22 ± 0.01c 9.98 ± 0.32a 2.00 ± 0.03c,d,e 0.17 ± 0.01c,d 395.8 ± 0.01f 0.26 ± 0.02c 15.71 ± 0.49a 2.32 ± 0.09a – c 0.23 ± 0.03a 422.5 ± 4.0c,d
Hammer 0.22 ± 0.01c 10.20 ± 0.41a 2.11 ± 0.05b, c 0.23 ± 0.01b 418.6 ± 0.01e,f 0.31 ± 0.01b, c 12.89 ± 0.75b 2.25 ± 0.11a – c 0.23 ± 0.05a 428.1 ± 28.1b,c,d
RIII
Blade 0.22 ± 0.01c 6.46 ± 0.26d 1.89 ± 0.04e 0.16 ± 0.01d 426.1 ± 0.01e 0.27 ± 0.03b, c 9.64 ± 0.62d 2.00 ± 0.04c 0.19 ± 0.01a 444.1 ± 19.1b,c,d
Hammer 0.23 ± 0.01c 7.22 ± 0.41c,d 2.09 ± 0.07b, c 0.24 ± 0.01a, b 501.03 ± 0.01c 0.31 ± 0.01b, c 9.54 ± 0.53d 2.37 ± 0.21a, b 0.30 ± 0.06a 526.7 ± 51.7b, c
RIV
Blade 0.30 ± 0.01a 8.47 ± 0.22b 1.93 ± 0.04d,e 0.18 ± 0.02c,d 306.5 ± 0.02g 0.32 ± 0.02b, c 11.82 ± 0.70b, c 2.07 ± 0.03b, c 0.19 ± 0.01a 365.3 ± 11.9d
Hammer 0.30 ± 0.01a 7.47 ± 0.25c 2.04 ± 0.02b,c,d 0.25 ± 0.01a, b 481.9 ± 0.01d 0.43 ± 0.06a 10.61 ± 1.30c,d 2.00 ± 0.02c 0.19 ± 0.01a 535.2 ± 21.8b
Ripeness 97.91%*** 89.89%*** 61.58%*** 13.40%*** 86.82%*** 58.99%*** 82.04%*** 62.71%*** 61.86%* 90.26%***
Crusher system 0.98%NS 0.82%NS 35.64%*** 85.72%*** 9.09%*** 27.56%*** 4.32%* 0.83%NS 6.18%NS 1.97%**

© 2016 Society of Chemical Industry


Ripeness × crusher system 1.11%NS 9.29%*** 2.78%NS 0.88%NS 4.09%*** 13.45%* 13.64%** 36.46%* 31.96%NS 7.77%***

RI, RII, RIII and RIV, stage of ripeness; T0 and T6 , different storage time; POV, peroxide values; TP, total phenols.
The values reported are means of three independent determinations ± standard deviation.
a g oleic acid in 100 g of oil;
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b mEq O kg−1 of oil;


2
c mg of gallic acid kg−1 .
Different letters in the same row indicate significant difference at 5%; factorial variability is expressed as percentage of the total sum of the squares; *, **, *** and NS significant F-values; the
* P < 0.05, ** P < 0.01 or *** P < 0.001 levels, NS, not significant.

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Table 2. Phenolic profiles of Correggiolo oils and treatment interdependences of factorial design
∑ ∑ ∑
Storage time Parameter OHTY1 TY DOA2 Luteolin Apigenin Phenol alcohols Secoiridoids Flavones

T0 RI
Blade 5.86 ± 0.30b 11.10 ± 0.32a 296.96 ± 48.63b 5.85 ± 0.37a 4.54 ± 0.42b 16.96 ± 0.55b 482.86 ± 56.05a,b 14.63 ± 0.99a
Hammer 7.89 ± 0.26a 11.80 ± 0.24a 301.10 ± 25.52a,b 5.59 ± 0.58a 5.12 ± 0.78a,b 19.69 ± 0.34a 531.11 ± 25.74a 14.01 ± 1.66a

wileyonlinelibrary.com/jsfa
RII
Blade 2.35 ± 0.83c 4.25 ± 0.93c 149.43 ± 6.77d,e 6.70 ± 0.70a 9.33 ± 2.22a,b 6.60 ± 1.74c 273.43 ± 12.36d,e 22.65 ± 4.1a
Hammer 2.63 ± 0.47c 4.32 ± 0.68c 174.17 ± 29.83c,d 7.73 ± 2.55a 10.31 ± 4.57a 6.95 ± 1.14c 293.65 ± 53.73c,d,e 23.80 ± 9.51a
RIII
Blade 1.05 ± 0.18d 2.76 ± 0.15d 216.85 ± 17.28c,d 7.92 ± 0.67a 6.24 ± 0.84a,b 3.81 ± 0.33d 361.58 ± 23.18c,d 20.80 ± 2.2a
Hammer 2.74 ± 0.21c 5.23 ± 0.14c 374.93 ± 15.95a 7.40 ± 0.76a 5.33 ± 0.52a,b 7.98 ± 0.32c 537.14± 21.12 a 18.21 ± 1.86a
RIV
Blade 1.51 ± 0.04c,d 5.44 ± 0.67c 85.38 ± 24.47e 4.63 ± 0.38a 5.13 ± 0.19a,b 4.63 ± 4.03c 211.72 ± 26.29e 9.24 ± 8.00a
Hammer 6.78 ± 0.46a,b 8.41 ± 0.53b 227.14 ± 19.55b,c 7.94 ± 1.61a 6.37±1.53a,b 15.19 ± 0.98b 387.26 ± 32.88b,c 18.93 ± 3.37a
Ripeness 67.71%*** 91.28%*** 61.49%*** 44.69%NS 94.74%** 73.84%*** 64.94%*** 69.47%*
Crusher system 19.55%*** 5.19%*** 21.92%*** 12.17%NS 1.01%NS 15.17%*** 22.37%*** 4.30%NS
Ripeness × crusher system 12.74%*** 3.53%*** 16.59%*** 43.14%NS 4.25%NS 10.99%*** 12.69%** 26.23%NS
T6 RI
Blade 7.59 ± 0.51b 10.17 ± 0.42a 181.80 ± 10.70b 6.54 ± 0.43b 0.75 ± 0.08b 17.75 ± 0.32a 279.05 ± 15.53a,b 8.26 ± 0.14b
Hammer 9.39 ± 1.84a,b 10.27 ± 1.69a 129.18 ± 21.82c,d,e 5.82 ± 0.26b 0.81 ± 0.13a,b 19.66 ± 3.53a 240.72 ± 23.99a,b,c 7.74 ± 0.46b
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RII
Blade 3.51 ± 0.08c,d 3.34 ± 0.07b,c 105.17 ± 3.15e 6.88 ± 0.56a,b 0.74 ± 0.07b 6.85 ± 0.12b 123.63 ± 83.81d 7.66 ± 2.28b
Hammer 4.55 ± 0.24c 4.41 ± 0.38b,c 107.67 ± 6.79d,e 5.66 ± 1.54b 0.85 ± 0.41a,b 8.96 ± 0.61b 131.96 ± 70.02c,d 7.66 ± 1.14b
RIII

© 2016 Society of Chemical Industry


Blade 2.51 ± 0.38d 2.82 ± 0.31c 140.98 ± 15.36c,d 6.9 ± 0.28a,b 0.81 ± 0.11a,b 5.33 ± 0.68b 209.61 ± 16.82b,c,d 9.31 ± 0.53a,b
Hammer 3.49 ± 0.28c,d 4.13 ± 0.26b,c 254.61 ± 17.38a 8.18 ± 1.08a,b 1.06 ± 0.28a,b 7.62 ± 0.52b 336.88 ± 23.38a 11.16 ± 1.72a,b
RIV
Blade 2.55 ± 0.22c,d 5.20 ± 0.14b 40.41 ± 1.97f 6.41 ± 1.00b 1.22 ± 0.20a,b 7.76 ± 0.35b 105.76 ± 1.62d 9.37 ± 1.47a,b
Hammer 10.34 ± 0.35a 9.42 ± 0.45a 152.49 ± 4.70b,c 9.27 ± 1.30a 1.46 ± 0.41a 19.75 ± 0.80a 251.11 ± 5.41a,b 12.37 ± 2.04a
Ripeness 52.34%*** 85.26%*** 42.68%* 47.65%*** 85.78%** 73.78%*** 59.45%*** 70.76%**
Crusher system 24.8%*** 7.99%*** 5.87%NS 14.95%*** 11.44%NS 10.02%*** 15.36%** 10.79%NS
Ripeness × crusher system 22.86%*** 6.76%*** 51.45%** 37.4%*** 2.78%NS 16.2%*** 25.2%** 18.45%NS

RI, RII, RIII and RIV, stage of ripeness, T 0 and T 6 , different storage time, OHTY, hydroxytyrosol, TY, tyrosol, DOA, decarboxymethyl oleuropein aglycon.
The values reported are means of three independent determinations ± standard deviation.
1 Expressed as mg kg−1 oil of tyrosol, 2 expressed as mg kg−1 oil of oleuropein, the others compounds are expressed as mg kg−1 of relative standard.
Different letters in the same row indicate significant difference at 5%, factorial variability is expressed as percentage of the total sum of the squares, *, **,*** and NS significant F-values, the
* P < 0.05, ** P < 0.01 or *** P < 0.001 levels, NS, not significant.

J Sci Food Agric 2017; 97: 1443–1450


L Morrone et al.
Hammer vs. blade crusher at four olive ripeness stages www.soci.org

Figure 3. Sensory profiles of the oils at four stage of ripeness (RI, RII, RIII and RIV) after production (T 0 ) and after 6 months of storage (T 6 ). Hammer crusher
– – ; blade crusher - - -; OFO, olive fruity (olfactory); OO, other olfactory scents; OF, olive fruity; B, bitterness; P, pungency; G, grass scent; OS, other scents.

enzymatic activity was highest at the start of black stage olive


Table 3. Treatment interdependences of factorial design
maturation, to then subsequently decrease. After 6 months of oil
storage an overall decrease in secoiridoids content was observed Storage Crusher Ripeness ×
at all the ripening stages. The differences in the secoiridoids con- time Characteristic Ripeness system crusher system
tent observed in the oils produced using the two different crushing
systems followed the T 0 trend (Table 2). It is important to under- T0 Bitterness 80.70%*** 2.10%NS 17.20%NS
line the decrease of the incidence of the ripeness factor observed Pungency 70.68%*** 1.80%NS 27.60%*
in storage oils (T 6 ), moreover the interaction between ripeness Olive fruity 48.80%NS 0.60%NS 50.60%*
and crushing system increased, explaining 25.20% of the variabil- T6 Bitterness 71.80%** 9.00%NS 19.20%NS
ity (Table 2). The analyses of the flavonic fraction did not show Pungency 48.60%NS 4.90%NS 46.50%NS
any significant difference in luteolin neither due to ripeness nor to Olive fruity 46.80%NS 1.10%NS 52.20%NS
crushing system, while a slightly decreasing trend was recorded Variability expressed as percentage of the total sum of the squares for
for apigenin which was highest at RII. The luteolin content was sensory attributes perceived in oils.
not affected by storage, in agreement with other authors,30,32 con- *, **, *** and NS significant F-values; the
* P < 0.05, ** P < 0.01 or *** P < 0.001 levels, NS, not significant.
versely a reduction in the apigenin content was recorded after 6
months of storage, while the same authors reported the stability
of the two flavones during storage.
CONCLUSION
Sensory characteristics of the oils The results obtained in this study indicate the greater influence of
The sensory profiles of the Correggiolo oils were characterised ripeness than the type of crusher used on quality indices, phenolic
by average levels of olive fruity, bitterness and pungency (Fig. 3); content and sensory attributes. However, the significance of the
these sensory profiles were in agreement with the profile reported synergic interaction between ripeness and crushing factors on
in the database of the Italian monovarietal olive oils (http://www the chemical and sensory characteristics of virgin olive oils has
.olimonovarietali.it), describing Correggiolo oil as an oil with an been demonstrated. A different evolution of the characteristics of
average level of olive fruity, bitterness and pungency, and with the oils milled using different crushers was not recorded by the
notes of fresh almond, artichoke and grass. At T 0 the effect of analyses carried out six months after production. Nevertheless,
ripeness on the characters bitterness and pungency was statisti- the rise in the variability percentage ascribable to type of crusher
cally significant; in detail their trends decreased as ripening pro- and its interaction with ripeness lead us to conclude that the
gressed (Table 3 and Fig. 3), in agreement with other reports.16,17,35 influence of the crushing equipment comes to light slowly as the
The olive fruity intensities did not differ among the four ripen- storage proceeds.
ing stages, possibly because oils of Correggiolo cv. need to be In this study it was possible to observe, at a microscopic scale,
milled from over-ripe fruits to have a lower olive fruity intensity22 the different mechanical action of the two crushing systems:
(Table 3). No influence of the crusher typologies on sensory the squashing action of the hammer crusher and the tissues
attributes was observed at both T 0 and T 6 . However, statistical tearing of the blade crusher. These differences were clearer
analysis revealed an interaction between the two factors ripen- at the first harvesting date, with fruits still at an early matura-
ing and type of crusher on the pungency and olive fruity charac- tion phase. Moreover, the different mechanical action of the
ters, and the crushing effect is less influential than the fruit stage two types of crusher produces differences in size pit fragments
of ripeness. At T 6 the factors interaction is no longer significant; translating into different oil yields and transfer of phenolic
this underlines the stability of olive fruity and pungency attributes substances.
during storage and their independency from the studied factors. It is an important achievement to have the choice to produce oils
On the contrary, the development of the bitterness attribute dur- characterised by different levels of antioxidants considering the
ing storage is statistically significantly different, discriminating oils different conditions of raw material (olive with different ripeness
from different ripeness stages, while bitterness is independent index) in relation to different types of crushers. In fact, producing
1449

from the crushing equipment. oils with different nutritional properties and tastes can satisfy the

J Sci Food Agric 2017; 97: 1443–1450 © 2016 Society of Chemical Industry wileyonlinelibrary.com/jsfa
www.soci.org L Morrone et al.

demand of traditional consumers, interested in sweet character, attributes and phenolic compounds of Picudo olive oils. Food Res
and the emerging demand of a niche of consumers interested in Int 54:1860–1867 (2013).
17 Rotondi A, Bendini A, Cerretani L, Mari M, Lercker G and Gallina Toschi
products with a high beneficial health impact on degenerative T, Effect of olive ripening degree on the oxidative stability and
diseases and different types of cancer, thus rich in total phenols organoleptic properties of cv. Nostrana di Brisighella extra virgin
and characterised by high bitterness and pungency intensities.36,37 olive oil. J Agric Food Chem 54:3649–3654 (2004).
18 Sánchez Casas J, De Miguel Gordillo C, Osorio Bueno E, Expósito JM,
Gallardo González L and Martínez Cano M, Calidad sensorial de
aceites de oliva virgen procedentes de variedades de aceitunas
ACKNOWLEDGEMENTS producidas en Extremadura. Grasas Aceites 57:313–318 (2006).
This work was supported by IPA Adriatic Cross-border Cooperation 19 Bendini A, Cerretani L, Salvador MD, Fregapane G and Lercker G,
project ‘AOGPRPSL – The Adriatic Olive Grove: risk prevention, sus- Stability of the sensory quality of virgin olive oil during storage: an
tainability, learning’ funded by the European Union. The authors overview. Ital J Food Sci 21:389–406 (2009).
20 Fiori F, Di Lecce G, Boselli E, Pieralisi G and Frega NG, Effects of olive
thank Matteo Mari and Mafalda Govoni for their technical assis- paste fast preheating on the quality of extra virgin olive oil during
tance, Franco Corticelli for the SEM observations and Stefano Cerni storage. Food Sci Technol-Leb 58:511–518 (2014).
and the Province of Rimini. 21 Uceda M and Hermoso M, La calidad del aceite de oliva, in El Cultivo
Del Olivo, ed. by Barranco D, Fernandez-Escobar R and Rallo L. Mundi
Prensa, Madrid, pp. 589–614 (2001).
22 Rotondi A and Magli M, Ripening of olives var. Correggiolo: Modifica-
SUPPORTING INFORMATION tion of oxidative stability of oils during fruit ripening and oil storage.
Supporting information may be found in the online version of this J Food Agric Environ 2:193–199 (2004).
article. 23 European Commission, Regulation EEC 2568/91 on the characteristics
of olive oil and olive pomace and their analytical methods. Off J Eur
Commission L248:6–36 (1991).
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