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Olive oil: a review on the identity and quality of olive oils produced in Brazil

Azeite de oliva: uma revisão sobre a identidade e a qualidade de azeites produzidos no Brasil

Abstract

The sensory quality of olive oils is influenced by the diversity and concentration of volatile and non-volatile compounds that vary according to cultivar, and edaphic, climatic, and cultivation conditions, which allows for establishing the origin of the product. In addition, since this crop has been recently introduced in Brazil, little is known about the performance of cultivars in this region, where investments in this activity have been made. Thus, relevant aspects about the chemical and sensory quality of olive oils are presented and discussed, as well as how these aspects influence the identity of the product.

Index terms
Brazilian olive oil; volatile compounds; chemical composition

Resumo

A qualidade sensorial dos azeites é influenciada pela diversidade e pela concentração de compostos voláteis e não voláteis que variam conforme a cultivar e as condições edafoclimáticas e de cultivo, o que permite estabelecer a procedência do produto. Além disso, por se tratar de uma cultura introduzida recentemente no Brasil, pouco se sabe sobre o desempenho das cultivares nas regiões onde o investimento nessa atividade vem sendo feito. Dessa forma, são apresentados e discutidos, nesta revisão, aspectos relevantes sobre a qualidade química e sensorial dos azeites de oliva e como esses aspectos influenciam a identidade do produto.

Termos para indexação
azeite de oliva brasileiro; compostos voláteis; composição química

Introduction

Extra-virgin olive oil is widely appreciated by consumers as a consequence of its sensory attributes and health benefits (APARICIO et al., 2012 APARICIO, R.; MORALES, M.T.; GARCÍA-GONZÁLEZ, D.L.Towards new analyses of aroma and volatiles to understand sensory perception of olive oil. European Journal of Lipid Science and Technologyy, Weinheimm v.114, n.10, p.1114-1125, 2012. ; BAJOUB; SÁNCHEZ-ORTIZ et al., 2015 BAJOUB, A.; SÁNCHEZ-ORTIZ, A.; OUAZZANI, N.; FERNÁNDEZ-GUTIÉRREZ, A.; BELTRÁN, G.; CARRASCO-PANCORBO, A. First comprehensive characterization of volatile profile of north Moroccan olive oils: a geographic discriminant approach. Food Research International, New York, v.76, p.410-417, 2015. ). According to data from the International Olive Council (IOC), both olive oil production and consumption have grown considerably in areas outside the Mediterranean region, mainly in the United States, Australia, Canada, Chile, Uruguay, Brazil, Japan, and China (IOC, 2020 IOC - International Olive Council. International olive figures. Madrid, 2020. Disponível em:https://www.internationaloliveoil.org/estaticos/view/131-world-olive-oil-figures. Acesso em: 05 mar. 2020.
https://www.internationaloliveoil.org/es...
), and this is due to the fact that it is a food product widely reported as beneficial to health (GUASCH-FERRÉ et al., 2020 GUASCH-FERRÉ, M.; LIU, G.; LI, Y.; SAMPSON, L.; MANSON, J.E.; SALAS-SALVADÓ, J.; MARTÍNEZ-GONZÁLEZ, M.A.; STAMPFER, M.J.; WILLETT, W.C.; SUN, Q. Olive oil consumption and cardiovascular risk in US adults. Journal of the American College of Cardiology, New York, v.75, n.15, p.1729-1739, 2020. ) and a part of different culinary profiles, from the most classic to more recent trends, such as vegetarian and vegan diets (MENAL-PUEY et al., 2019 MENAL-PUEY, S.; MARTÍNEZ-BIARGE, M.; MARQUES-LOPES, I. Developing a food exchange system for meal planning in vegan children and adolescents. Nutrients, Basel, v.11, n.1, p.43, 2019. ).

In Brazil, olive growing occupies about 7,000 hectares, of which 4,500 hectares are cultivated in Rio Grande do Sul and about 2,000 hectares in the “Serra da Mantiqueira” region, which encompasses areas of the states of Minas Gerais, São Paulo, and Rio de Janeiro (KIST et al., 2019 KIST, B.B.; DE CARVALHO, C.; BELING, R.R. Anuário brasileiro das oliveiras. 2.ed. Santa Cruz: Editora Gazeta, 2019. 56 p. ). The cultivation of olive trees (Olea europaea L.) is expanding in Espírito Santo, which currently has 186.5 hectares and expects further investments. In addition, in “Chapada Diamantina” (Bahia), the first 1.6 tons of olives were harvested in 2021, totaling 280 liters of oil (SANTO, 2019 SANTO, G.D.E. O cultivo de oliveiras para a produção de azeite é apresentado na Assembleia Legislativa. 2019. Disponível em: https://www.es.gov.br/Noticia/o-cultivo-e-oliveiras-para-a-producao-de-azeite-e-apresentado-na-assembleia-legislativa. Acesso em: 05 mar. 2021.
https://www.es.gov.br/Noticia/o-cultivo-...
; MINAS, 2021 MINAS, A. Primeiro azeite extravirgem da Chapada Diamantina é produzido com tecnologia Epamig. Belo Horizonte, 2021. Disponível em: http://www.agenciaminas.mg.gov.br/noticia/primeiro-azeite-extravirgem-da-chapada-diamantina-e-produzido-com-tecnologia-epamig. Acesso em: 05 mar. 2021.
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). Rio Grande do Sul accounts for the vast majority of the area planted with olive trees in Brazil and also for the largest olive oil production. In the 2019 harvest, 180 thousand liters of olive oil were produced, 75% more than in the previous year. However, the 2020 harvest was affected by climatic factors, which caused 57% reduction in the total production of olives in many orchards of Rio Grande do Sul (IBRAOLIVA, 2020 IBRAOLIVA - Instituto Brasileiro de Olivicultura. Abertura oficial da colheita da oliva será em Caçapava do Sul. 2020. Disponível em: https://www.ibraoliva.com.br/noticias/detalhe/77/abertura-oficial-da-colheita-da-oliva-sera-em-cacapava-do-sul. Acesso em: 04 mar. 2020.
https://www.ibraoliva.com.br/noticias/de...
).

In addition to the increase in olive oil production and consumption, there is a trend in consumer buying habits, which show greater concern about traceability, authenticity, and quality of olive oils, so that greater value is given to products that are associated with a specific location (geographical indication) and/or special means of production (BAJOUB et al., 2018 BAJOUB, A.; MEDINA-RODRÍGUEZ, S.; CUADROS-RODRÍGUEZ, L.; MONASTERIO, R.P.; VERCAMMEN, J.; FERNÁNDEZ-GUTIÉRREZ, A.; CARRASCO-PANCORBO, A. A metabolic fingerprinting approach based on selected ion flow tube mass spectrometry (SIFT-MS) and chemometrics: A reliable tool for Mediterranean origin-labeled olive oils authentication. Food Research International, New York, v.106, p.233-242, 2018. ). In this context, the aromatic profile of olive oils is of great interest, since numerous volatile organic compounds (VOCs) including aldehydes, alcohols, esters, ketones, terpenes, among others, have been described as indicators of sensory quality (DA SILVA et al., 2012 DA SILVA, M.D.G.; FREITAS, A.M.C.; CABRITA, M.J.; GARCIA, R. Olive oil composition: volatile compounds. In: DIMITRIOS, B. (ed.). Olive oil: constituents, quality, health properties and bioconversions. London: Intech, 2012. p.500. ; BAJOUB; SÁNCHEZORTIZ et al., 2015 BAJOUB, A.; SÁNCHEZ-ORTIZ, A.; OUAZZANI, N.; FERNÁNDEZ-GUTIÉRREZ, A.; BELTRÁN, G.; CARRASCO-PANCORBO, A. First comprehensive characterization of volatile profile of north Moroccan olive oils: a geographic discriminant approach. Food Research International, New York, v.76, p.410-417, 2015. ). In addition to influencing the sensory characteristics of olive oils, VOCs authenticate the geographical origin of this type of product, since the profile and abundance of these compounds may vary depending on the environmental conditions characteristic of each region and cultivar (PROCIDA et al., 2005 PROCIDA, G.; GIOMO, A.; CICHELLI, A.; CONTE, L.S. Study of volatile compounds of defective virgin olive oils and sensory evaluation: a chemometric approach. Journal of the Science of Food and Agriculture, New York, v.85, n.13, p.2175-2183, 2005. ; CAJKA et al., 2010 CAJKA, T.; RIDDELLOVA, K.; KLIMANKOVA, E.; CERNA, M.; PUDIL, F.; HAJSLOVA, J. Traceability of olive oil based on volatiles pattern and multivariate analysis. Food Chemistry, London, v.121, n.1, p.282-289, 2010. ; BAJOUB; SÁNCHEZ-ORTIZ et al., 2015 BAJOUB, A.; SÁNCHEZ-ORTIZ, A.; OUAZZANI, N.; FERNÁNDEZ-GUTIÉRREZ, A.; BELTRÁN, G.; CARRASCO-PANCORBO, A. First comprehensive characterization of volatile profile of north Moroccan olive oils: a geographic discriminant approach. Food Research International, New York, v.76, p.410-417, 2015. ).

In addition to volatile compounds, phenolic compounds also influence the sensory characteristics of olive oils and can be used as quality markers. Phenolic compounds such as elenolic acid, ligstroside aglycone, oleuropein aglycone and acetoxypinoresinol allow discriminating oils from different geographical regions (OUNI et al., 2011 OUNI, Y.; TAAMALLI, A.; GÓMEZ-CARAVACA, A.M.; SEGURA-CARRETERO, A.; FERNÁNDEZ-GUTIÉRREZ, A.; ZARROUK, M. Characterisation and quantification of phenolic compounds of extra-virgin olive oils according to their geographical origin by a rapid and resolutive LC–ESI-TOF MS method. Food Chemistry, London, v.127, n.3, p.1263-1267, 2011. ). On the other hand, the composition of fatty acids seems to be more dependent on the cultivar than on the cultivation conditions or production region (LANTERI et al., 2002 LANTERI, S.; ARMANINO, C.; PERRI, E.; PALOPOLI, A. Study of oils from Calabrian olive cultivars by chemometric methods. Food Chemistry, London, v.76, n.4, p.501-507, 2002. ).

Thus, scientific knowledge about the chemical and sensory quality of Brazilian olive oils is essential, since production is recent and little is known about the quality of Brazilian commercial olive oils. The knowledge about its composition allows producers to strengthen the identity of the regional product and position their products in the market with distinctive signs. As a matter of fact, Brazilian olive oils have received international awards for their outstanding sensory quality. In addition, as it is a recently introduced crop (mid-2003) (KIST et al., 2019 KIST, B.B.; DE CARVALHO, C.; BELING, R.R. Anuário brasileiro das oliveiras. 2.ed. Santa Cruz: Editora Gazeta, 2019. 56 p. ; CAYE et al., 2020 CAYE, A.; RUFFONI, J.; ZIEGLER, D.D.R. Sistema setorial de inovação no agronegócio: uma análise para a produção de azeite de oliva no RS. Estudos Econômicos, São Paulo, v.37, n.75, p.75-105, 2020. ), little is known about the performance of cultivars in this new growing region (outside the Mediterranean region). Within this context, in this review, the relevant aspects about olive growing in Brazil, the production of olive oils and the chemical and sensory quality of olive oils and how these aspects influence the product identity will be presented and discussed.

Olive growing

Olive growing occupies sixth place in the world production of vegetable oils, and the Mediterranean Basin region represents approximately 90% of the world olive oil production. The main producing countries are Spain, Italy, Greece, Tunisia, Turkey, Morocco, and Portugal. However, olive cultivation has been progressively increasing in countries and regions outside the Mediterranean Basin such as Argentina, Australia, Brazil, Canada, Chile, China, Japan, Peru, United States, Uruguay, and West Africa (IOC, 2020 IOC - International Olive Council. International olive figures. Madrid, 2020. Disponível em:https://www.internationaloliveoil.org/estaticos/view/131-world-olive-oil-figures. Acesso em: 05 mar. 2020.
https://www.internationaloliveoil.org/es...
). The expansion and intensification of olive cultivation are associated with the perception that olive oil and table olives are healthy foods (Rallo et al., 2018 RALLO, L.; DÍEZ, C.M.; MORALES-SILLERO, A.; MIHO, H.; PRIEGO-CAPOTE, F.; RALLO, P. Quality of olives: A focus on agricultural preharvest factors. Scientia Horticulturae, Wageningen, v.233, p.491-509, 2018. ) and versatile for use in international food and gastronomy (KOIDIS; BOSKOU, 2006 KOIDIS, A.; BOSKOU, D. The contents of proteins and phospholipids in cloudy (veiled) virgin olive oils. European Journal of Lipid Science and Technology, Weinheim, v.108, n.4, p.323-328, 2006. ).

Following this trend, the area cultivated with olive trees in Brazil is around 7,000 hectares, the largest area (4,500 ha) is located in Rio Grande do Sul and in the Serra da Mantiqueira region (2,000 ha), the latter covering areas of the states of Minas Gerais, São Paulo, and Rio de Janeiro. Olive growing has also been taking place, but in smaller areas, in states such as Espírito Santo, Bahia, Santa Catarina and Paraná, in all cases with prospects for expansion (ROYO, 2010 ROYO, J. Projeto pioneiro inicia cultivo de oliveiras em Santa Catarina. Florianópolis: Epagri, 2010. Disponível em: http://diadecampo.com.br/zpublisher/materias/Materia.asp?id=21249esecao=Pacotes%20Tecnol%F3gicoset=EPAGRI . Acesso em: 05 mar. 2021.
http://diadecampo.com.br/zpublisher/mate...
; DA COSTA, 2019 DA COSTA, E.B. Oliveiras avançam em terras capixabas: na safra 2020/21, a meta é produzir azeite genuinamente capixaba em escala comercial. Vitória: ES Brasil, 2019. 16 p. Disponível em: https://esbrasil.com.br/oliveiras-avancam-em-terras-capixabas/.
https://esbrasil.com.br/oliveiras-avanca...
; FLORIPA, 2019 FLORIPA, T.S. Rancho queimado: empresa é pioneira na produção do azeite de oliva com fins comerciais. Florianópolis, 2019. Disponível em: http://www.tudosobrefloripa.com.br/index.php/desc_noticias/rancho_queimado_empresa_e_pioneira_na_producaeo_do_azeite_de_oliva_com_fins. Acesso em: 05 mar. 2021.
http://www.tudosobrefloripa.com.br/index...
; KIST et al., 2019 KIST, B.B.; DE CARVALHO, C.; BELING, R.R. Anuário brasileiro das oliveiras. 2.ed. Santa Cruz: Editora Gazeta, 2019. 56 p. ; SANTO, 2019 SANTO, G.D.E. O cultivo de oliveiras para a produção de azeite é apresentado na Assembleia Legislativa. 2019. Disponível em: https://www.es.gov.br/Noticia/o-cultivo-e-oliveiras-para-a-producao-de-azeite-e-apresentado-na-assembleia-legislativa. Acesso em: 05 mar. 2021.
https://www.es.gov.br/Noticia/o-cultivo-...
; MINAS, 2021 MINAS, A. Primeiro azeite extravirgem da Chapada Diamantina é produzido com tecnologia Epamig. Belo Horizonte, 2021. Disponível em: http://www.agenciaminas.mg.gov.br/noticia/primeiro-azeite-extravirgem-da-chapada-diamantina-e-produzido-com-tecnologia-epamig. Acesso em: 05 mar. 2021.
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).

In Rio Grande do Sul, the most favorable climatic parameters for fruit ripening are observed in the southern half of the state, with temperatures between 25º C and 35º C, within the temperature range considered ideal for the ripening of olives, although the rainfall index is above levels commonly agreed as optimal for the development of the olive tree (650 mm) (ALBA et al., 2013 ALBA, J.M.F.; FLORES, C.A.; WREGE, M.S. Zoneamento edafoclimático da olivicultura para o Rio Grande do Sul. Brasília: Embrapa Clima Temperado, 2013. 70 p. ). In the mountain areas of Rio Grande do Sul and Santa Catarina, the cold hours accumulated during winter favor the dormancy of olive trees (WREGE et al., 2015 WREGE, M.S.; COUTINHO, E.F.; PANTANO, A.P.; JORGE, R.O. Distribuição potencial de oliveiras no Brasil e no mundo. Revista Brasileira de Fruticultura, Jaboticabal, v.37, n.3, p.656-666, 2015. ). On the other hand, in Paraná although the thermal requirements regarding heat and rainfall are met, the low number of cold hours in most of the state is a limiting factor for olive production (SIMÕES, 2016 SIMÕES, F.R.M.M. Zoneamento agroclimático e as possibilidades para a olivicultura no estado do Paraná. 2016. Monografia (Trabalho de Conclusão de Curso Bacharelado em Geografia) - Universidade Estadual Paulista, Câmpus Experimental de Ourinhos, 2016. ). In the state of Espírito Santo, the “Capixaba” Institute for Research, Technical Assistance and Rural Extension (Incaper) has already identified 150,000 hectares of land suitable for olive cultivation in the mountainous region, with altitude above 900 meters above sea level (DA COSTA, 2019 DA COSTA, E.B. Oliveiras avançam em terras capixabas: na safra 2020/21, a meta é produzir azeite genuinamente capixaba em escala comercial. Vitória: ES Brasil, 2019. 16 p. Disponível em: https://esbrasil.com.br/oliveiras-avancam-em-terras-capixabas/.
https://esbrasil.com.br/oliveiras-avanca...
). The fact that the region of Minas Gerais has higher altitudes favors the cultivation of olive trees in the Serra da Mantiqueira region; however, only the southern regions and a small part of the midwestern region of Minas Gerais have climatic characteristics favorable to the cultivation of olive trees (GARCIA et al., 2018 GARCIA, S.R.; DOS SANTOS, D.F.; MARTINS, F.B.; TORRES, R.R. Aspectos climatológicos associados ao cultivo da oliveira (Olea europaea L.) em Minas Gerais. Revista Brasileira de Climatologia, São Paulo, v.22, p.188-206, 2018. ; MARTINS et al., 2020 MARTINS, F.B.; PEREIRA, R.A.D.A.; TORRES, R.R.; SANTOS, D.F.D. Climate projections of chill hours and implications for olive cultivation in Minas Gerais, Brazil. Pesquisa Agropecuária Brasileira, Brasília, DF, v.55, p.e01852, 2020. ).

In the context of the olive oil business, Brazil is the world’s second largest olive oil importer, only behind the United States, and has production corresponding to less than 2% of its domestic consumption. Thus, investment in the sector is promising and the challenge today is to increase production (AGROLINK, 2020 AGROLINK. Olivicultura pode ser oportunidade. 2020. Disponível em: https://www.agrolink.com.br/noticias/olivicultura-pode-ser-oportunidade_440170.html. Acesso em: 20 out. 2020.
https://www.agrolink.com.br/noticias/oli...
). According to the Brazilian Institute of Olive Growing, the Brazilian olive oil production in 2019 was estimated at 230 thousand liters, approximately 180 thousand liters in RS.

It is important to observe that Brazilian olive trees are young and have not yet reached their peak production, with only 40% of the planted area being currently in production. Currently, Brazil grows cultivars Arbequina, Arbosana, Ascolano 315, Coratina, Frantoio, Grapollo 541, Koroneiki, Manzanilla, and Picual, with ‘Arbequina’ being the predominant one, as it adapts well to the climate and soil of producing regions (KIST et al., 2019 KIST, B.B.; DE CARVALHO, C.; BELING, R.R. Anuário brasileiro das oliveiras. 2.ed. Santa Cruz: Editora Gazeta, 2019. 56 p. ). It is in the context of an emerging and vigorous activity, that the production of olives and olive oils appears on the national scenario. Despite the success it has already reached, there are challenges to be overcome, which demand research, knowledge generation, validation and sharing of knowledge, and promotion of the national product.

The perception of traders, associations and regular consumers of olive oils is that products made in Brazil have high quality (SÁ et al., 2019 SÁ, D.; CAMPOS, R.D.S.; DE FARIA-MACHADO, A. Aceitação de azeites de oliva da Região da Mantiqueira (MG): entendendo consumidor e azeite brasileiros. Rio de Janeiro: Embrapa Agroindústria de Alimentos, 2019. (Documentos INFOTECA-E) ). The construction of the identity of a food product demands, in addition to the production system, a technical-scientific classification in sensory and chemical terms (BAJOUB et al., 2014 BAJOUB, A.; CARRASCO-PANCORBO, A.; MAZA, G.B., FERNÁNDEZ-GUTIÉRREZ, A.; OUAZZANI, N. Contribution to the establishment of a protected designation of origin for Meknès virgin olive oil: A 4-years study of its typicality. Food Research International, New York, v.66, p.332-343, 2014. ).

In addition, food quality certification is an important requirement in the agrifood sector, as it assures the consumer the conformity and authenticity of products and allows establishing a bond of trust and fidelity in the acquisition of products of proven quality. The characterization of an olive oil increases the added value of the product and promotes its commercialization in both domestic and foreign markets (POULIAREKOU et al., 2011 POULIAREKOU, E.; BADEKA, A.; TASIOULA-MARGARI, M.; KONTAKOS, S.; LONGOBARDI, F.; KONTOMINAS, M.G. Characterization and classification of Western Greek olive oils according to cultivar and geographical origin based on volatile compounds. Journal of Chromatography A, Amsterdam, v.1218, n.42, p.7534-7542, 2011. ). Although the commercial production of olive oils in Brazil is still recent, the construction of databases on the composition of the products needs to be carried out in order to support future demands for indication of origin (IO) or designation of origin (DO).

Fruit constituents

The olive tree (Olea europaea L.) is a dicotyledonous angiosperm plant of the Oleaceae family, of arboreal size and native to temperate regions, characterized by two seasons: one cold and wet, in which the plant reaches dormancy, and the other hot and dry, when fruiting occurs.

The olive tree fruit is a drupe spherical or elliptical in shape, varying in size and weight (2 to 20 g) (even on the same tree) and dependent on the cultivar, fruit load, pedoclimatic conditions, and agricultural practices.

Anatomically, olives consist of three parts: skin or peel, called epicarp (1.0-3.0% of the drupe weight), pulp or flesh, also called mesocarp (70-80% of whole fruits), and the stone, called woody endocarp (18-22% of the fruit weight) (BIANCHI, 2003 BIANCHI, G. Lipids and phenols in table olives. European Journal of Lipid Science and Technology, Weinheim, v.105, n.5, p.229-242, 2003. ).

Fruit ripening is accompanied by a change in the epicarp color from green to purple (Figure 1), which is related to a progressive decrease in the content of chlorophylls and carotenoids, followed by increase in the content of anthocyanins as the fruit matures (BIANCHI, 2003 BIANCHI, G. Lipids and phenols in table olives. European Journal of Lipid Science and Technology, Weinheim, v.105, n.5, p.229-242, 2003. ; LANZA e DI SERIO, 2015 LANZA, B.; DI SERIO, M.G. Characterization of olive (Olea europaea L.) fruit epicuticular waxes and epicarp. Scientia Horticulturae, Wageningen, v.191, p.49-56, 2015. ; SERVILI et al., 2016 SERVILI, M.; SORDINI, B.; ESPOSTO, S.; TATICCHI, A.; URBANI, S.; SEBASTIANI, L. Metabolomics of olive fruit: a focus on the secondary metabolites. In: RUGINI, E.; BALDANI, L.; MULEO, R.; SEBASTIANI, L. (ed.). The olive tree genome. Berlin: Springer, 2016. p.123-139. ).

Figure 1
Changes in the olive color during ripening (Source: Filoda, P.F).

The epicarp cells are covered by a cuticle composed of cutin (a polymer almost impermeable to water) and waxes that can be intracuticular or present on the fruit surface and protect internal tissues from mechanical damage and from the attack of fungi and insects. The mesocarp makes up most of the olives and together with the skin, represent the edible portion of olives. Depending on the cultivar and maturation level, its composition is comprised of mainly water (70-75%) and lipids (14-30%) (SERVILI et al., 2016 SERVILI, M.; SORDINI, B.; ESPOSTO, S.; TATICCHI, A.; URBANI, S.; SEBASTIANI, L. Metabolomics of olive fruit: a focus on the secondary metabolites. In: RUGINI, E.; BALDANI, L.; MULEO, R.; SEBASTIANI, L. (ed.). The olive tree genome. Berlin: Springer, 2016. p.123-139. ).

The lipid fraction of olives, located mainly in the mesocarp, includes triglycerides, phospholipids, and waxes. In general, table olives have lower oil contents, since high levels of this fraction tend to impair the consistency and conservation of the processed fruit (BIANCHI, 2003 BIANCHI, G. Lipids and phenols in table olives. European Journal of Lipid Science and Technology, Weinheim, v.105, n.5, p.229-242, 2003. ). Triglyceride content increases with fruit growth and maturation. The fatty acid profile of lipids present in olives is composed of oleic acid (18: 1) as the major fatty acid, followed by palmitic acid (16: 0), linoleic acid (18: 2), palmitoleic acid (16: 1), stearic acid (18: 0), and linolenic acid (18: 3), in addition to other minorities whose abundance does not reach 1% of the total fraction (GÓMEZ-RICO et al., 2009 GÓMEZ-RICO, A.; SALVADOR, M.D.; FREGAPANE, G. Virgin olive oil and olive fruit minor constituents as affected by irrigation management based on SWP and TDF as compared to ETc in medium-density young olive orchards (Olea europaea L. cv. Cornicabra and Morisca). Food Research International, New York, v.42, n.8, p.1067-1076, 2009. ; INGLESE et al., 2011 INGLESE, P.; FAMIANI, F.; GALVANO, F.; SERVILI, M.; ESPOSTO, S.; URBANI, S. Factors affecting extra-virgin olive oil composition. Horticultural Reviews, New York, v.38, p.83, 2011. ; RALLO et al., 2018 RALLO, L.; DÍEZ, C.M.; MORALES-SILLERO, A.; MIHO, H.; PRIEGO-CAPOTE, F.; RALLO, P. Quality of olives: A focus on agricultural preharvest factors. Scientia Horticulturae, Wageningen, v.233, p.491-509, 2018. ). Olives also have organic acids such as oxalic, succinic, malic, and citric acids (1.2- 2.1% of the dry pulp) (SERVILI et al., 2016 SERVILI, M.; SORDINI, B.; ESPOSTO, S.; TATICCHI, A.; URBANI, S.; SEBASTIANI, L. Metabolomics of olive fruit: a focus on the secondary metabolites. In: RUGINI, E.; BALDANI, L.; MULEO, R.; SEBASTIANI, L. (ed.). The olive tree genome. Berlin: Springer, 2016. p.123-139. ).

The sugar content decreases during fruit maturation. The main soluble sugars in olives are glucose, fructose, sucrose, and mannitol, although other sugars, such as galactose, mannose, sorbitol, xylose, and rhamnose are also found as structural and reserve components (DROSSOPOULOS; NIAVIS, 1988 DROSSOPOULOS, J.; NIAVIS, C. Seasonal changes of the metabolites in the leaves, bark and xylem tissues of olive tree (Olea europaea.L) II. Carbohydrates. Annals of Botany, London, v.62, n.3, p.321-327, 1988. ; BIANCHI, 2003 BIANCHI, G. Lipids and phenols in table olives. European Journal of Lipid Science and Technology, Weinheim, v.105, n.5, p.229-242, 2003. ; TAIZ et al., 2017 TAIZ, L.; ZEIGER, E.; MOLLER, I.M.; MURPHY, A. Fisiologia e desenvolvimento vegetal. Porto Alegre: Artmed Editora, 2017. ; RALLO et al., 2018 RALLO, L.; DÍEZ, C.M.; MORALES-SILLERO, A.; MIHO, H.; PRIEGO-CAPOTE, F.; RALLO, P. Quality of olives: A focus on agricultural preharvest factors. Scientia Horticulturae, Wageningen, v.233, p.491-509, 2018. ). Sugars are related to textural properties (important components of the cell wall, polymerized in the form of pectins and cellulose), in addition to being precursors of oil biosynthesis and providing energy for metabolic changes (MARSILIO et al., 2001 MARSILIO, V.; CAMPESTRE, C.; LANZA, B.; DE ANGELIS, M. Sugar and polyol compositions of some European olive fruit varieties (Olea europaea L.) suitable for table olive purposes. Food Chemistry, London, v.72, n.4, p.485-490, 2001. ; RALLO et al., 2018 RALLO, L.; DÍEZ, C.M.; MORALES-SILLERO, A.; MIHO, H.; PRIEGO-CAPOTE, F.; RALLO, P. Quality of olives: A focus on agricultural preharvest factors. Scientia Horticulturae, Wageningen, v.233, p.491-509, 2018. ).

The aspects considered when determining the ideal harvest time include maximization of the fruit size and oil production and quality within a context of efficient orchard management (RALLO et al., 2018 RALLO, L.; DÍEZ, C.M.; MORALES-SILLERO, A.; MIHO, H.; PRIEGO-CAPOTE, F.; RALLO, P. Quality of olives: A focus on agricultural preharvest factors. Scientia Horticulturae, Wageningen, v.233, p.491-509, 2018. ). Usually, late fruit harvest results in oils with lower concentration of phenolic compounds and less pronounced aromatic profile (SALVADOR et al., 2001 SALVADOR, M.; ARANDA, F.; FREGAPANE, G. Influence of fruit ripening on ‘Cornicabra’virgin olive oil quality a study of four successive crop seasons. Food Chemistry, London, v.73, n.1, p.45-53, 2001. ; SERVILI et al., 2015 SERVILI, M.; ESPOSTO, S.; TATICCHI, A.; URBANI, S.; DI MAIO, I.; VENEZIANI, G.; SELVAGGINI, R. New approaches to virgin olive oil quality, technology, and by-products valorization. European Journal of Lipid Science and Technology, Weinheim, v.117, n.11, p.1882-1892, 2015. ).

For example, the contents of the phenolic compound hydroxytyrosol and the volatile organic compound trans- 2-hexenal (responsible for fruity aroma and green notes) in olive oils obtained from more ripe fruits are lower than those obtained from less ripe fruits (BAJOUB; CARRASCO-PANCORBO et al., 2015 BAJOUB, A.; CARRASCO-PANCORBO, A.; OUAZZANI, N.; FERNÁNDEZ-GUTIÉRREZ, A. Potential of LC–MS phenolic profiling combined with multivariate analysis as an approach for the determination of the geographical origin of north Moroccan virgin olive oils. Food Chemistry, London, v.166, p.292-300, 2015. ; ROMERO et al., 2016 ROMERO, N.; SAAVEDRA, J.; TAPIA, F.; SEPÚLVEDA, B.; APARICIO, R.Influence of agroclimatic parameters on phenolic and volatile compounds of Chilean virgin olive oils and characterization based on geographical origin, cultivar and ripening stage. Journal of the Science of Food and Agriculture, New York, v.96, n.2, p.583-592, 2016. ). Therefore, olive growers start harvesting earlier in order to obtain high quality olive oils; however, green olives have characteristics that affect technological and rheological properties, in addition to obtaining low oil yield (AGUILERA et al., 2010 AGUILERA, M.P.; BELTRAN, G.; SANCHEZ-VILLASCLARAS, S.; UCEDA, M.; JIMENEZ, A. Kneading olive paste from unripe ‘Picual’fruits: I. Effect on oil process yield. Journal of Food Engineering, London, v.97, n.4, p.533-538, 2010. ). Thus, the time for harvesting olives influences characteristics of bitterness, pungency, and oxidative stability of olive oils, and consequently the acceptance of the product by consumers (DAG et al., 2011 DAG, A.; KEREM, Z.; YOGEV, N.; ZIPORI, I., LAVEE, S.; BEN-DAVID, E. Influence of time of harvest and maturity index on olive oil yield and quality. Scientia Horticulturae, Wageningen, v.127, n.3, p.358-366, 2011. ).

Olive oil production

Unlike most vegetable oils, olive oil is obtained through mechanical extraction (ANGEROSA et al., 2006 ANGEROSA, F.; CAMPESTRE, C.; GIANSANTE, L. Analysis and authentication. In: BOSKOU, D. Olive oil: chemistry and technology. Champaign: AOAC, 2006. p.113-172. ). Brazilian legislation defines olive oil as the product obtained only from olive tree fruits, excluding oils obtained through solvent extraction or re-esterification processes and/or any mixture of other oils (BRASIL, 2005 BRASIL. Regulamento técnico para óleos vegetais, gorduras vegetais e creme vegetal. Resolução n° 270, de 22 de setembro de 2005. Diário Oficial da União, Brasília, DF, v.184, p.372-373, 2005. ( ). According to Normative Instruction No. 1 of the Ministry of Agriculture, Livestock, and Supply (MAPA), olive oil and olive-pomace oil are categorized according to their identity requirements such as raw material and processes used for obtaining olive oil, and the quality requirements defined in terms of the percentage of free acidity, peroxide indexes, and specific extinction coefficient in the ultraviolet spectrum. Thus, olive oil and olive-pomace oil can be classified into the following groups and types: Virgin olive oil, Olive oil, Refined olive oil, Olive-pomace oil, and Refined olive-pomace oil (BRASIL, 2012 BRASIL. Regulamento técnico dos azeites de oliva e dos óleos de bagaço de oliva. Brasília, DF: Ministério da Agricultura, Pecuária e Abastecimento (MAPA). Diário Oficial da União, Brasília, DF, v.166, p.2-5, 2012. ). Virgin olive oil is further classified into three types: extra virgin, virgin, and lampante, which is dependent on the quality parameters of free acidity, peroxide index, and specific extinction coefficient in the ultraviolet spectrum (BRASIL, 2012 BRASIL. Regulamento técnico dos azeites de oliva e dos óleos de bagaço de oliva. Brasília, DF: Ministério da Agricultura, Pecuária e Abastecimento (MAPA). Diário Oficial da União, Brasília, DF, v.166, p.2-5, 2012. ).

The production of olive oil involves a series of stages ranging from the harvest of olives to oil storage.

In this process, some of the main stages of the industrial process for obtaining the different types of olive oil are illustrated in Figure 2. Dashed arrows indicate stages of mixtures between the oils that may occur during the process to obtain the final product.

Figure 2
Flowchart showing the processes for obtaining olive oil of different categories (Source: Filoda, P.F).

Once harvested, whether using manual or mechanical methods, olives must be placed in ventilated boxes for transport from the field to the oil press. Olives should be processed as quickly as possible, usually within 24 hours after harvest in order to limit oxidation and biochemical changes. Then, olives are selected for quality, rinsed in running water and weighed to be submitted to crushing and malaxation stages (EPAMIG, 2006 EPAMIG. Azeitona e azeite de oliva: tecnologias de produção. Informe Agropecuário, Belo Horizonte, v.27, n.231, p.104, 2006. ; SOUILEM et al., 2017 SOUILEM, S.; EL-ABBASSI, A.; KIAI, H.; HAFIDI, A.; SAYADI, S.; GALANAKIS, C.M. Olive oil production sector: environmental effects and sustainability challenges. In: GALANAKIS, C.M. (ed.). Olive mill waste. Oxford: Academic Press: 2017. p.1-28 ).

The crushing of olives using mechanical hammer crushers is a process used to break the fruit tissues and release the oil contained within the cells. The crushing step is followed by malaxation, an operation that consists of slowly stirring the olive paste obtained to increase the crushing effect, making the paste uniform and breaking the oil/water emulsion, so that oil drops come together to form bigger drops. The malaxation step is carried out in cylindrical mixers (thermomixers), with blades inside that rotate and mix the paste and exert, in a certain way, a scissor effect that cuts the formed paste, considered one of the most crucial stages of the oil extraction process, in which temperature and duration parameters are very influential in the quality and composition of the oil obtained (KAPELLAKIS et al., 2008 KAPELLAKIS, I.E.; TSAGARAKIS, K.P.; CROWTHER, J.C. Olive oil history, production and by-product management. Reviews in Environmental Science and Bio/Technology, Amsterdam, v.7, n.1, p.1-26, 2008. ). At the end of the process, the olive paste derived from the previously mentioned operations, consists of a solid fraction (pomace) and a liquid fraction (oily wort composed of oil and water). The main objective of the remaining stages of the extraction process is the adequate and efficient separation of these phases in order to achieve the greatest possible recovery of the oily phase (BAJOUB, 2016 BAJOUB, A. Virgin olive oil: potential of different omics approaches to authenticate its geographical and botanical origin. 2016. Thesis (Doctor) - Universidad de Granada, Department of Analytical Chemistry, Granada, 2016. ).

For the separation of solid-liquid mixtures, agroindustries commonly use decanter-type centrifuges, where due to the different densities, the high centrifugal forces separate the finely distributed solid particles from the suspension. In this process, a rotating screw conveyor continuously conducts the solid to the discharge. The liquid phase (s) flow (s) along the screw conveyor.

Decanter centrifuges are the most modern and widely used method for phase separation (BAJOUB, 2016 BAJOUB, A. Virgin olive oil: potential of different omics approaches to authenticate its geographical and botanical origin. 2016. Thesis (Doctor) - Universidad de Granada, Department of Analytical Chemistry, Granada, 2016. ).

Two-phase and three-phase decanter systems differ mainly in water requirements during the process.

Thus, when water is added to the paste to facilitate the extraction process, the system is called three-phase, whereas when oil is centrifuged without adding water, the process is described as two-phase. In a continuous threephase system, three products are generated: oil, pomace, and wastewater. However, the oil fraction obtained still contains water droplets in the emulsion and insoluble solids in the dispersion, and therefore must be submitted to a vertical centrifuge where oil separation and cleaning occurs. In this process, large amounts of wastewater are generated. Although the two-phase system provides two final flows (oil and olive pomace), wastewater continues to be eliminated, but together with the solid portion (MORAL; MÉNDEZ, 2006 MORAL, P.S.; MÉNDEZ, M.V.R. Production of pomace olive oil. Grasas y Aceites, Madrid, v.57, n.1, p.47-55, 2006. ).

Filtration is the final stage of olive oil processing, which can be carried out using diatomaceous earth or cellulose to remove suspended solids, as well as moisture before bottling and storage of the final product. Olive oil oxidation, which can start during processing, can be accelerated during the storage stage by exposure to air, heat, light, and metals. Thus, to avoid this problem, olive oil must be stored in dark containers (to prevent exposure to light and oxygen), and kept at about 15-18 ° C (BAJOUB, 2016 BAJOUB, A. Virgin olive oil: potential of different omics approaches to authenticate its geographical and botanical origin. 2016. Thesis (Doctor) - Universidad de Granada, Department of Analytical Chemistry, Granada, 2016. ).

Residues obtained from the olive oil extraction process comprise the aqueous residue, composed of water used during the extraction process, in addition to water contained in fruits and water used to wash them and the solid residue, called pomace, composed of pulp and epicarp, parts of the crushed stone and water. Extraction industries seek to invest in alternatives that enable the use of residues, such as composting and mineral fertilization, herbicide, animal nutrition, use of dry pomace for energy generation, and food applications (MEDEIROS et al., 2016 MEDEIROS, R.M.L.; VILLA, F.; DA SILVA, D.F.; CARDOSO FILHO, L.R. Destinação e reaproveitamento de subprodutos da extração olivícola. Scientia Agraria Paranaensis, Cascavel, v.15, n.2, p.100-108, 2016. ).

Due to the costs of olive oil cultivation, harvesting, and extraction processes, in addition to having higher concentration of antioxidant compounds than other oils and exclusive sensory characteristics, olive oil has high market value among vegetable oils, being frequent target of adulteration. In view of the fact that food adulterations often involve replacing high-cost ingredients with cheaper substitutes, fraud involving olive oil by adding other types of vegetable oils of lesser commercial value and of similar composition becomes a major problem both for the industry and for the health of consumers (FLORES et al., 2006 FLORES, G.; DEL CASTILLO, M.L.R.; HERRAIZ, M.; BLANCH, G.P. Study of the adulteration of olive oil with hazelnut oil by on-line coupled high performance liquid chromatographic and gas chromatographic analysis of filbertone. Food Chemistry, London, v.97, n.4, p.742-749, 2006. ; VLACHOS et al., 2006 VLACHOS, N.; SKOPELITIS, Y.; PSAROUDAKI, M.; KONSTANTINIDOU, V.; CHATZILAZAROU, A.; TEGOU, E. Applications of Fourier transform-infrared spectroscopy to edible oils. Analytica Chimica Acta, Amsterdam, v.573, p.459-465, 2006. ).

Quality parameters

Brazilian legislation has implemented quality and identity criteria for vegetable oils established by the International Olive Council (IOC) and the Codex Alimentarius Commission (BRASIL, 2005 BRASIL. Regulamento técnico para óleos vegetais, gorduras vegetais e creme vegetal. Resolução n° 270, de 22 de setembro de 2005. Diário Oficial da União, Brasília, DF, v.184, p.372-373, 2005. ( ). IOC is an international agency that regulates olive oil by defining quality standards and monitoring authenticity. According to this agency, traditional methods used for detecting adulteration in edible oils include mainly sensory evaluation, chromatography, mass spectrometry, and nuclear magnetic resonance (IOC, 2013 IOC - International Olive Council. Trade standard applying to olive oil and olive-pomace oil. Madrid, 2013. (COI/T.15/NC No 3/Rev.7) ). However, although knowledge about the sensory profile of olive oils is relevant to distinguish the quality of products, Brazilian legislation does not require the performance of sensory analysis.

The quality and authenticity of olive oils can be assessed from parameters of free acidity, peroxide index, and specific extinction coefficients, as well as from the composition of fatty acids, sterols, stigmastadienes, and waxes (BRAZIL, 2012 BRASIL. Regulamento técnico dos azeites de oliva e dos óleos de bagaço de oliva. Brasília, DF: Ministério da Agricultura, Pecuária e Abastecimento (MAPA). Diário Oficial da União, Brasília, DF, v.166, p.2-5, 2012. ). These parameters can be influenced by factors such as maturation, storage, enzymatic action, olive quality, olive oil production system, degree of refining, and purity (BRASIL, 2005 BRASIL. Regulamento técnico para óleos vegetais, gorduras vegetais e creme vegetal. Resolução n° 270, de 22 de setembro de 2005. Diário Oficial da União, Brasília, DF, v.184, p.372-373, 2005. ( ; DA SILVA et al., 2012 DA SILVA, M.D.G.; FREITAS, A.M.C.; CABRITA, M.J.; GARCIA, R. Olive oil composition: volatile compounds. In: DIMITRIOS, B. (ed.). Olive oil: constituents, quality, health properties and bioconversions. London: Intech, 2012. p.500. ).

The acidity of olive oils comes from the action of lipases that hydrolyze triacylglycerols, releasing fatty acids. The peroxide index measures the degree of oil oxidation, which increases as unsaturated and free fatty acids react with oxygen. Extinction coefficients indicate whether the product comes from good quality raw materials and whether the processing conditions were adequate, since this analysis verify the presence of carbonyl compounds (secondary oxidation stage) and conjugated trienes formed during the clarification stage by oxidation and dehydration of epoxides derived from unsaturated fatty acids (ANGEROSA et al., 2006 ANGEROSA, F.; CAMPESTRE, C.; GIANSANTE, L. Analysis and authentication. In: BOSKOU, D. Olive oil: chemistry and technology. Champaign: AOAC, 2006. p.113-172. ; AUEDPIMENTEL et al., 2008 AUED-PIMENTEL, S.; TAKEMOTO, E.; KUMAGAI, E.E.; CANO, C.B. Determinação da diferença entre o valor real e o teórico do triglicerídeo ECN 42 para a detecção de adulteração em azeites de oliva comercializados no Brasil. Química Nova, São Paulo, v.31, n.1, p.31-34, 2008. ).

Olive oil composition

In general, olive oil is basically composed of two fractions: the saponifiable fraction and the unsaponifiable fraction. The saponifiable fraction represents approximately 98% of the total oil weight, which is mainly composed of triacylglycerols (fatty acids esterified in glycerol) and other minor components, such as free fatty acids, phospholipids, waxes, and esters of sterols. The unsaponifiable fraction, which represents approximately 2% of the total oil weight, comprises a complex set of compounds belonging to chemical families such as aliphatic and triterpene alcohols, sterols, hydrocarbons, phenolic compounds, pigments, and volatile components (SERVILI et al., 2004 SERVILI, M.; SELVAGGINI, R.; ESPOSTO, S.; TATICCHI, A.; MONTEDORO, G.; MOROZZI, G. Health and sensory properties of virgin olive oil hydrophilic phenols: agronomic and technological aspects of production that affect their occurrence in the oil. Journal of Chromatography A, Amsterdam, v.1054, n.1-2, p.113-127, 2004. ; DABBOU et al., 2009 DABBOU, S.; ISSAOUI, M.; ESPOSTO, S.; SIFI, S.; TATICCHI, A.; SERVILI, M.; HAMMAMI, M. Cultivar and growing area effects on minor compounds of olive oil from autochthonous and European introduced cultivars in Tunisia. Journal of the Science of Food and Agriculture, New York, v.89, n.8, p.1314-1325, 2009. ). These groups of compounds from the unsaponifiable fraction are essential in the taste and oxidative stability of olive oils and there is evidence of the beneficial health properties provided by some of these olive oil components, including vitamin E, pigments, phytosterols, and phenolic compounds (BAJOUB; CARRASCO-PANCORBO et al., 2015 BAJOUB, A.; CARRASCO-PANCORBO, A.; MAZA, G.B., FERNÁNDEZ-GUTIÉRREZ, A.; OUAZZANI, N. Contribution to the establishment of a protected designation of origin for Meknès virgin olive oil: A 4-years study of its typicality. Food Research International, New York, v.66, p.332-343, 2014. ).

Olive oil is distinguished from other oils due to its high content of monounsaturated fatty acids, with oleic acid (C18: 1 Δ9) being the most abundant, representing 55 to 83% of total fatty acids (AL-BACHIR; SAHLOUL, 2017 AL-BACHIR, M.; SAHLOUL, H. Fatty acid profile of olive oil extracted from irradiated and non-irradiated olive fruits. International Journal of Food Properties, Philadelphia, v.20, n.11, p.2550-2558, 2017. ). Linoleic (C18: 2 Δ9,12) and linolenic (C18: 3 Δ9,12,15) polyunsaturated acids represent 3 to 21% and less than 1%, respectively, of the total olive oil fatty acid composition (BRASIL, 2005 BRASIL. Regulamento técnico para óleos vegetais, gorduras vegetais e creme vegetal. Resolução n° 270, de 22 de setembro de 2005. Diário Oficial da União, Brasília, DF, v.184, p.372-373, 2005. ( ; MAGGIO et al., 2009 MAGGIO, R.M.; KAUFMAN, T.S.; DEL CARLO, M.; CERRETANI, L.; BENDINI, A.; CICHELLI, A.; COMPAGNONE, D. Monitoring of fatty acid composition in virgin olive oil by Fourier transformed infrared spectroscopy coupled with partial least squares. Food Chemistry, London, v.114, n.4, p.1549-1554, 2009. ; DA SILVEIRA et al., 2017 DA SILVEIRA, R.; VÁGULA, J.M.; DE LIMA FIGUEIREDO, I.; CLAUS, T.; GALUCH, M.B.; JUNIOR, O.O.S.; VISENTAINER, J.V. Rapid methodology via mass spectrometry to quantify addition of soybean oil in extra virgin olive oil: A comparison with traditional methods adopted by food industry to identify fraud. Food Research International, New York, v.102, p.43-50, 2017. ). In addition, olive oil is a product that contains considerable amounts of saturated fatty acids in its composition, especially palmitic acid, which can represent up to 20% of the total olive oil fatty acid composition. Table 1 shows the fatty acid composition of extra virgin olive oils, established by IOC and adopted by Brazilian legislation. However, a certain difference between limits for myristic (less than or equal to 0.05) and linoleic (3.5 to 21.0) fatty acids established in Brazil is verified in relation to IOC limits, where the amount of myristic acid must be less or equal to 0.03 and for linoleic acid, the limit is 2.5-21.0.

Table 1
General composition of extra virgin olive oil fatty acids

Olive oil composition can vary depending on cultivar, latitude, agricultural techniques adopted, maturation level of olives at harvest, olive oil extraction system and storage conditions (ROMERO et al., 2016 ROMERO, N.; SAAVEDRA, J.; TAPIA, F.; SEPÚLVEDA, B.; APARICIO, R.Influence of agroclimatic parameters on phenolic and volatile compounds of Chilean virgin olive oils and characterization based on geographical origin, cultivar and ripening stage. Journal of the Science of Food and Agriculture, New York, v.96, n.2, p.583-592, 2016. ).

The authenticity of the product and the distinction of oils from different cultivars and geographical origins can be performed based on the fatty acid profile (YOUSSEF et al., 2011; BAJOUB; CARRASCO-PANCORBO et al., 2015 BAJOUB, A.; CARRASCO-PANCORBO, A.; OUAZZANI, N.; FERNÁNDEZ-GUTIÉRREZ, A. Potential of LC–MS phenolic profiling combined with multivariate analysis as an approach for the determination of the geographical origin of north Moroccan virgin olive oils. Food Chemistry, London, v.166, p.292-300, 2015. ; BORGES et al., 2017 BORGES, T. H., LÓPEZ, L. C., PEREIRA, J. A., CABRERA–VIQUE, C., e SEIQUER, I. Comparative analysis of minor bioactive constituents (CoQ10, tocopherols and phenolic compounds) in Arbequina extra virgin olive oils from Brazil and Spain. Journal of Food Composition and Analysis, v. 63, p. 47-54, 2017. ).

In Brazil, due to the recent olive oil production, little is known about the composition of local products. Studies on the composition of Brazilian olive oils began in 2010, when the physicochemical characteristics of different olive cultivars cultivated in the municipality of Maria da Fé (MG) were evaluated, with the first oils extracted from the region being classified as extra virgin (DE OLIVEIRA et al., 2010 DE OLIVEIRA, A.F.; NETO, J.V.; GONÇALVES, E.D.; VILLA, F.; DA SILVA, L.F.D.O. Parâmetros físico-químicos dos primeiros azeites de oliva brasileiros extraídos em Maria da Fé, Minas Gerais. Scientia Agraria, Curitiba, v.11, n.3, p.255-261, 2010. ). Subsequently, olive oils extracted from cultivars JB1, Ascolano 315, Negroa, 0025 and 0004 cultivated on the Epamig experimental farm, in the municipality of Maria da Fé (MG), were evaluated for characteristics of acidity index, iodine, saponification, peroxides and fatty acid profile. ‘Negroa’ and ‘JB1’ showed the highest productivity and the best acidity, saponification, peroxides and iodine rates. In addition, all cultivars showed fatty acid levels within expected limits (CARDOSO et al., 2010 CARDOSO, L.G.V.; BARCELOS, M.D.F.P.; DE OLIVEIRA, A.F.; PEREIRA, J.D.A.R.; DE ABREU, W.C.; DE ARAUJO PIMENTEL, F.; DE ANGELIS PEREIRA, M.C. Características físico-químicas e perfil de ácidos graxos de azeites obtidos de diferentes variedades de oliveiras introduzidas no Sul de Minas Gerais–Brasil. Semina: Ciências Agrárias, Londrina, v.31, n.1, p.127-135, 2010. ).

Olive oils from ‘Arbequina’ grown in southern Brazil, in the municipalities of Caçapava do Sul and Cachoeira do Sul, were evaluated in terms of physicochemical parameters and fatty acid profile. The results of analyses met the required standards, classifying oils as extra virgin (MELLO; PINHEIRO, 2012 MELLO, L.D.; PINHEIRO, M.F. Aspectos físico-químicos de azeites de oliva e de folhas de oliveira provenientes de cultivares do RS, Brasil. Alimentos e Nutrição, São Paulo, v.23, n.4, p.537-548, 2012. ).

Ballus et al. (2014) BALLUS, C.A.; MEINHART, A.D.; DE SOUZA CAMPOS JR, F.A.; DA SILVA, L.F.D.O.; DE OLIVEIRA, A.F.; GODOY, H.T. A quantitative study on the phenolic compound, tocopherol and fatty acid contents of monovarietal virgin olive oils produced in the southeast region of Brazil. Food Research International, New York, v.62, p.74-83, 2014. evaluated the profile of phenolic compounds, tocopherols and fatty acids from 17 monovarietal olive oils produced at the Maria da Fé (MG) experimental station. Ballus et al. (2015) BALLUS, C.A.; QUIRANTES-PINÉ, R.; BAKHOUCHE, A.; DA SILVA, L.F.D.O.; DE OLIVEIRA, A.F.; COUTINHO, E.F.; GODOY, H.T. Profile of phenolic compounds of Brazilian virgin olive oils by rapid resolution liquid chromatography coupled to electrospray ionisation time-of-flight mass spectrometry (RRLC–ESI-TOF-MS). Food Chemistry, London, v.170, p.366-377, 2015. also evaluated the profile of phenolic compounds of cultivars Arbequina, Grappolo, Koroneiki, and Manzanilha grown in Dom Pedrito and ‘Arbequina’, ‘Coratina’, ‘Frantoio’ and ‘Koroneiki’ grown in Pelotas. In all cases, it was observed that these oils had high quantity and diversity of phenolic compounds.

The production and yield of olive oils from cultivars Arbequina, Arbosana, and Koroneiki in four locations in Santa Catarina were evaluated in order to obtain more information about the production potential of the crop in that region. In general, cultivars showed good fruit productivity and satisfactory olive oil yield, particularly cultivar Koroneiki (DA CROCE et al., 2016 DA CROCE, D.M.; BRUGNARA, E.C.; DE OLIVEIRA, V.P.; DIAS, C.R. Avaliação da produção e do rendimento de azeite das oliveiras ‘Arbequina’,‘Arbosana’e ‘Koroneiki’ em Santa Catarina. Agropecuária Catarinense, Florianópolis, v.29, n.1, p.54-57, 2016. ). In a previous study, the physicochemical characteristics of olive oils produced in experimental units of Santa Catarina were evaluated, and the authors reported that ‘Koroneiki’, ‘Arbequina’, and ‘Arbosana’ were adapted to the local edaphic and climatic conditions and were able to produce high-quality olive oils, according to chemical quality parameters required by IOC (DA CROCE et al., 2012 DA CROCE, D.M.; FLOSS, P.A.; DO ESPÍRITO SANTO, F.R.C.; RETT, H.T.; MATIAS, A.C. Características físico-químicas de azeite de oliva produzido em unidades experimentais de Santa Catarina. Agropecuária Catarinense, Florianópolis, v.25, n.2, p.39-41, 2012. ).

The composition of Brazilian oils was also evaluated by Bruscato et al. (2017) BRUSCATTO, M.H.; ZAMBIAZI, R.C.; CRIZEL-CARDOSO, M.; PIATNICKI, C.M.S.; MENDONÇA, C.R.B.; DUTRA, F.L.G.; COUTINHO, E.F. Caracterização química e estabilidade oxidativa de azeites extraídos de oliveiras do Sul do Brasil. Pesquisa Agropecuária Brasileira, Brasília, DF, v.52, n.12, p.1231-1240, 2017. , who determined the levels of tocopherols, pigments, phenolic compounds, and fatty acids in olive oils produced at the “Embrapa Clima Temperado” (RS) research station. The composition of olive oils from cultivar Arbequina produced in Pelotas- RS and Maria da Fé-MG was also evaluated in order to compare it with that of oils from the same cultivar produced in Spain (BORGES et al., 2017 BORGES, T. H., LÓPEZ, L. C., PEREIRA, J. A., CABRERA–VIQUE, C., e SEIQUER, I. Comparative analysis of minor bioactive constituents (CoQ10, tocopherols and phenolic compounds) in Arbequina extra virgin olive oils from Brazil and Spain. Journal of Food Composition and Analysis, v. 63, p. 47-54, 2017. ). More recently, the volatile profile and organoleptic characteristics of olive oils from cultivars Arbequina, Arbosana, Coratina, Grappolo, and Koroneiki produced in Minas Gerais, São Paulo, and Paraná were evaluated (ZAGO et al., 2019 ZAGO, L.; SQUEO, G.; BERTONCINI, E.I.; DIFONZO, G.; CAPONIO, F. Chemical and sensory characterization of Brazilian virgin olive oils. Food Research International, New York, v.126, p.108588, 2019. ).

Crizel et al. (2020) CRIZEL, R.L.; HOFFMANN, J.F.; ZANDONÁ, G.P.; LOBO, P.M.S.; JORGE, R.O; CHAVES, F.C. Characterization of extra virgin olive oil from southern Brazil. European Journal of Lipid Science and Technology, Weinheim, p.1900347, 2020. , demonstrated that harvest and cultivar influence the chemical composition related to the quality of oils produced in Pinheiro Machado, RS.

Among the classes of compounds found in olive oils, phospholipids, found in small amounts in olive oil (usually <150 mg / kg), act as antioxidants in olive oils (KOIDIS; BOSKOU, 2006 KOIDIS, A.; BOSKOU, D. The contents of proteins and phospholipids in cloudy (veiled) virgin olive oils. European Journal of Lipid Science and Technology, Weinheim, v.108, n.4, p.323-328, 2006. ; ALVES et al., 2016 ALVES, E.; MELO, T.; REY, F.; MOREIRA, A.S.; DOMINGUES, P.; DOMINGUES, M.R. Polar lipid profiling of olive oils as a useful tool in helping to decipher their unique fingerprint. LWT -Food Science and Technology, Amsterdam, v.74, p.371-377, 2016. ). Olive oils, in general, contain virtually no wax in their composition because they are extracted via mechanical processing. Thus, the presence of waxes can be indicative of fraudulent mixtures containing vegetable oils, since waxes are dissolved in solvents used during the process of extracting oils from other sources (MAILER et al., 2010 MAILER, R.J.; AYTON, J.; GRAHAM, K. The influence of growing region, cultivar and harvest timing on the diversity of Australian olive oil. Journal of the American Oil Chemists' Society, Champaign, v.87, n.8, p.877-884, 2010. ).

Olive oil also has α-tocopherol, a vitamin E component with antioxidant activity, which contributes to the oil stability and provides health benefits. α-tocopherol levels between 117.47 and 325.00 mg kg-1 have been reported in olive oils from six cultivars produced in southern Brazil in the 2017 and 2018 harvests (CRIZEL et al., 2020 CRIZEL, R.L.; HOFFMANN, J.F.; ZANDONÁ, G.P.; LOBO, P.M.S.; JORGE, R.O; CHAVES, F.C. Characterization of extra virgin olive oil from southern Brazil. European Journal of Lipid Science and Technology, Weinheim, p.1900347, 2020. ). The percentage of tocopherols is strongly influenced by climatic factors, agricultural management, maturation level, and cultivar (SERVILI et al., 2009 SERVILI, M.; ESPOSTO, S.; FABIANI, R.; URBANI, S.; TATICCHI, A.; MARIUCCI, F.; SELVAGGINI, R.; MONTEDORO, G.F. Phenolic compounds in olive oil: antioxidant, health and organoleptic activities according to their chemical structure. Inflammopharmacology, Dordrecht, v.17, n.2, p.76-84, 2009. ; EL RIACHY et al., 2011 EL RIACHY, M.; PRIEGO-CAPOTE, F.; LEÓN, L.; RALLO, L.; LUQUE DE CASTRO, M.D. Hydrophilic antioxidants of virgin olive oil.Part 1: Hydrophilic phenols: A key factor for virgin olive oil quality. European Journal of Lipid Science and Technology, Weinheim, v.113, n.6, p.678-691, 2011. ; RALLO et al., 2018 RALLO, L.; DÍEZ, C.M.; MORALES-SILLERO, A.; MIHO, H.; PRIEGO-CAPOTE, F.; RALLO, P. Quality of olives: A focus on agricultural preharvest factors. Scientia Horticulturae, Wageningen, v.233, p.491-509, 2018. ).

Among pigments responsible for color in olive oil, chlorophylls contribute to the green color while carotenoids to the yellow-orange color. Carotenoids also promote immunological, endocrine and metabolic benefits due to their pro-vitamin A activity. The content of carotenoids in olive oil depends on storage period and conditions as they are susceptible to degradation by exposure to light and high temperatures (RALLO et al., 2018 RALLO, L.; DÍEZ, C.M.; MORALES-SILLERO, A.; MIHO, H.; PRIEGO-CAPOTE, F.; RALLO, P. Quality of olives: A focus on agricultural preharvest factors. Scientia Horticulturae, Wageningen, v.233, p.491-509, 2018. ). Monovarietal olive oils obtained in southern Brazil showed pigment levels varying according to cultivar and year of harvest, with carotenoid content between 3.80 and 31.0 mg kg-1 and chlorophyll content between 0.1 and 7.2 mg kg-¹ (CRIZEL et al., 2020 CRIZEL, R.L.; HOFFMANN, J.F.; ZANDONÁ, G.P.; LOBO, P.M.S.; JORGE, R.O; CHAVES, F.C. Characterization of extra virgin olive oil from southern Brazil. European Journal of Lipid Science and Technology, Weinheim, p.1900347, 2020. ).

Phenolic compounds are minor constituents in olives comprising 1-3% of the fresh pulp weight.

Synthesized by plants during growth and development in part due to responses to stressors, phenolics can act as antimicrobials, photoprotectors, visual attractants, as a defense against herbivores and pathogens, and as instruments of communication between plants and between plants and the environment (NACZK; SHAHIDI, 2004 NACZK, M.; SHAHIDI, F. Extraction and analysis of phenolics in food. Journal of Chromatography A, Amsterdam, v.1054, n.1-2, p.95-111, 2004. ; KARBAN, 2008 KARBAN, R. Plant behaviour and communication. Ecology Letters, Oxford, v.11, n.7, p.727-739, 2008. ). The main class of specialized metabolites typical of the Oleaceae family is represented by secoiridoids, a group of monoterpenoids with a cleaved methylcyclopentane skeleton, the most abundant representatives being oleuropein and ligstroside derivatives (Figure 3) (RYAN; ROBARDS, 1998 RYAN, D.; ROBARDS, K. Critical review. Phenolic compounds in olives. Analyst, New York, v.123, n.5, p.31R-44R, 1998. ; ALAGNA et al., 2012 ALAGNA, F.; MARIOTTI, R.; PANARA, F.; CAPORALI, S.; URBANI, S.; VENEZIANI, G., ESPOSTO, S.; TATICCHI, A.; ROSATI, A.; R.A.O, R.; BALDONI, L. Olive phenolic compounds: metabolic and transcriptional profiling during fruit development. BMC Plant Biology, London, v.12, n.1, p.162, 2012. ).

Figure 3
Examples of secoiridoids and phenolic alcohols commonly found in olive oils.

The class of phenolic constituents influences the nutritional and sensory quality of olive oils, contributing with bitterness, astringency, and pungency. In addition, phenolic compounds present in olive oils prevent lipid oxidation, making the product more stable and with a longer shelf life (SERVILI et al., 2009 SERVILI, M.; ESPOSTO, S.; FABIANI, R.; URBANI, S.; TATICCHI, A.; MARIUCCI, F.; SELVAGGINI, R.; MONTEDORO, G.F. Phenolic compounds in olive oil: antioxidant, health and organoleptic activities according to their chemical structure. Inflammopharmacology, Dordrecht, v.17, n.2, p.76-84, 2009. ; DAĞDELEN et al., 2013 DAGDELEN, A.; TÜMEN, G.; ÖZCAN, M.M.; DÜNDAR, E. Phenolics profiles of olive fruits (Olea europaea L.) and oils from Ayvalik, Domat and Gemlik varieties at different ripening stages. Food Chemistry, London, v.136, n.1, p.41-45, 2013. ; BAJOUB; CARRASCO-PANCORBO et al., 2015 BAJOUB, A.; CARRASCO-PANCORBO, A.; OUAZZANI, N.; FERNÁNDEZ-GUTIÉRREZ, A. Potential of LC–MS phenolic profiling combined with multivariate analysis as an approach for the determination of the geographical origin of north Moroccan virgin olive oils. Food Chemistry, London, v.166, p.292-300, 2015. ). Many of these phenolic compounds also have to beneficial effects on human health, with antioxidant, antiinflammatory, and antimicrobial properties, among others (CARRASCO-PANCORBO et al., 2005 CARRASCO-PANCORBO, A.; CERRETANI, L.; BENDINI, A.; SEGURA-CARRETERO, A.; DEL CARLO, M.; GALLINA-TOSCHI, T.; FERNANDEZ-GUTIERREZ, A. Evaluation of the antioxidant capacity of individual phenolic compounds in virgin olive oil. Journal of Agricultural and Food Chemistry, Washington, v.53, n.23, p.8918-8925, 2005. ; MEDINA et al., 2006 MEDINA, E.; DE CASTRO, A.; ROMERO, C.; BRENES, M. Comparison of the concentrations of phenolic compounds in olive oils and other plant oils: correlation with antimicrobial activity. Journal of Agricultural and Food Chemistry, Washington, v.54, n.14, p.4954-4961, 2006. ; CICERALE et al., 2012 CICERALE, S.; LUCAS, L.; KEAST, R. Antimicrobial, antioxidant and anti-inflammatory phenolic activities in extra virgin olive oil. Current Opinion in Biotechnology, Oxford, v.23, n.2, p.129-135, 2012. ).

The phenolic fraction of olive oils consists of a heterogeneous mixture of compounds belonging to several families with different chemical structures. These compounds belong to five main classes: (i) phenolic acids (e.g., caffeic and syringic acids), (ii) phenolic alcohols (e.g., hydroxytyrosol and tyrosol), (iii) flavonoids (e.g., luteolin and apigenin), (iv) secoiridoids (e.g., oleuropein and ligstroside) and (v) lignans (e.g., pinoresinol and 1-acetoxypinoresinol) (SERVILI et al., 2009 SERVILI, M.; ESPOSTO, S.; FABIANI, R.; URBANI, S.; TATICCHI, A.; MARIUCCI, F.; SELVAGGINI, R.; MONTEDORO, G.F. Phenolic compounds in olive oil: antioxidant, health and organoleptic activities according to their chemical structure. Inflammopharmacology, Dordrecht, v.17, n.2, p.76-84, 2009. ; EL RIACHY et al., 2011 EL RIACHY, M.; PRIEGO-CAPOTE, F.; LEÓN, L.; RALLO, L.; LUQUE DE CASTRO, M.D. Hydrophilic antioxidants of virgin olive oil.Part 1: Hydrophilic phenols: A key factor for virgin olive oil quality. European Journal of Lipid Science and Technology, Weinheim, v.113, n.6, p.678-691, 2011. ; BAJOUB; CARRASCO-PANCORBO et al., 2015 BAJOUB, A.; CARRASCO-PANCORBO, A.; OUAZZANI, N.; FERNÁNDEZ-GUTIÉRREZ, A. Potential of LC–MS phenolic profiling combined with multivariate analysis as an approach for the determination of the geographical origin of north Moroccan virgin olive oils. Food Chemistry, London, v.166, p.292-300, 2015. ).

The main phenolic alcohols in olive oils are hydroxytyrosol, also known as 3,4-dihydroxyphenyl ethanol (3,4-DHPEA) and tyrosol (also known as p-hydroxyphenyl ethanol or p-HPEA). These alcohols are present at low concentrations in fresh oils, but concentrations increase over the storage period as a result of the hydrolysis of secoiridoids (BRENES et al., 2001 BRENES, M.; GARCIA, A.; GARCIA, P.; GARRIDO, A. Acid hydrolysis of secoiridoid aglycons during storage of virgin olive oil. Journal of Agricultural and Food Chemistry, Washington, v.49, n.11, p.5609-5614, 2001. ; EL RIACHY et al., 2011 EL RIACHY, M.; PRIEGO-CAPOTE, F.; LEÓN, L.; RALLO, L.; LUQUE DE CASTRO, M.D. Hydrophilic antioxidants of virgin olive oil.Part 1: Hydrophilic phenols: A key factor for virgin olive oil quality. European Journal of Lipid Science and Technology, Weinheim, v.113, n.6, p.678-691, 2011. ). During olive oil extraction, oleuropein and ligstroside are enzymatically hydrolyzed to dialdehyde (3,4-DHPEA-EDA, p-HPEAEDA) and aldehyde carboxymethyl (3,4-DHPEA-EA and p-HPEAEA, respectively from oleuropein and ligstroside). Its concentration in olive oil varies considerably according to the management practices adopted, maturation level, geographical region, and oil extraction conditions (MALHEIRO et al., 2015 MALHEIRO, R.; RODRIGUES, N.; PEREIRA, J.A. Olive oil phenolic composition as affected by geographic origin, olive cultivar, and cultivation systems. In: BOSKOU, D. Olive and olive oil bioactive constituents. London: AOCS Pres, 2015. p.93-121. ). Table 2 shows the levels of phenolic compounds so far found in Brazilian monovarietal olive oils. Among identified compounds, phenolic alcohols appear as the most abundant group of phenolic compounds among analyzed samples, followed by secoiridoids and flavonoids. Higher levels of coumaric, vanillic, and syringic acids, in addition to compounds such as hydroxytyrosol and luteolin, seem to characterize oils from cultivar Arbequina. In addition, regardless of cultivar, compounds such as oleuropein aglycone and oleacin are among the most abundant secoiridoids found in olive oils (CRIZEL et al., 2020 CRIZEL, R.L.; HOFFMANN, J.F.; ZANDONÁ, G.P.; LOBO, P.M.S.; JORGE, R.O; CHAVES, F.C. Characterization of extra virgin olive oil from southern Brazil. European Journal of Lipid Science and Technology, Weinheim, p.1900347, 2020. ).

Table 2
Content of phenolic compounds (mg kg-1) in monovarietal Brazilian olive oil samples

The phenolic composition of olive oils is strongly affected by growing conditions (cultivar, production region, planting density, nutrition, water supply, abiotic stresses, among others) and by technological production conditions (CRIADO et al., 2004 CRIADO, M.N.; MORELLÓ, J.R.; MOTILVA, M.J.; ROMERO, M.P. Effect of growing area on pigment and phenolic fractions of virgin olive oils of the Arbequina variety in Spain. Journal of the American Oil Chemists' Society, Oxford, v.81, n.7, p.633, 2004. ; RANALLI et al., 2005 RANALLI, A.; MALFATTI, A.; LUCERA, L.; CONTENTO, S.; SOTIRIOU, E. Effects of processing techniques on the natural colourings and the other functional constituents in virgin olive oil. Food Research International, New York, v.38, n.8-9, p.873-878, 2005. ; SERVILI et al., 2007 SERVILI, M.; ESPOSTO, S.; LODOLINI, E.; SELVAGGINI, R.; TATICCHI, A.; URBANI, S.; MONTEDORO, G.; SERRAVALLE, M.; GUCCI, R. Irrigation effects on quality, phenolic composition, and selected volatiles of virgin olive oils cv.Leccino. Journal of Agricultural and Food Chemistry, Washington,v.55, n.16, p.6609-6618, 2007. ; TURA et al., 2007 TURA, D.; GIGLIOTTI, C.; PEDO, S.; FAILLA, O.; BASSI, D.; SERRAIOCCO, A. Influence of cultivar and site of cultivation on levels of lipophilic and hydrophilic antioxidants in virgin olive oils (Olea europea L.) and correlations with oxidative stability. Scientia Horticulturae, Wageningen, v.112, n.1, p.108-119, 2007. ). Within this context, olive oils obtained from orchards without irrigation showed higher levels of phenolic compounds compared to irrigated orchards. Nitrogen-rich fertilization seems to reduce the phenolic content. In both cases, regulation of the phenolic composition is influenced by the activity of the phenylalanine ammonia lyase enzyme (PAL) (ROMERO et al., 2016 ROMERO, N.; SAAVEDRA, J.; TAPIA, F.; SEPÚLVEDA, B.; APARICIO, R.Influence of agroclimatic parameters on phenolic and volatile compounds of Chilean virgin olive oils and characterization based on geographical origin, cultivar and ripening stage. Journal of the Science of Food and Agriculture, New York, v.96, n.2, p.583-592, 2016. ).

Both non-targeted metabolomic analysis and the targeted assessment of the phenolic compound profile have been used to differentiate oils from different cultivars and to reveal discriminating characteristics between oils from different geographical origins and therefore can be used as markers to prove the authenticity of olive oils (DABBOU et al., 2009 DABBOU, S.; ISSAOUI, M.; ESPOSTO, S.; SIFI, S.; TATICCHI, A.; SERVILI, M.; HAMMAMI, M. Cultivar and growing area effects on minor compounds of olive oil from autochthonous and European introduced cultivars in Tunisia. Journal of the Science of Food and Agriculture, New York, v.89, n.8, p.1314-1325, 2009. ; BAJOUB, 2016 BAJOUB, A. Virgin olive oil: potential of different omics approaches to authenticate its geographical and botanical origin. 2016. Thesis (Doctor) - Universidad de Granada, Department of Analytical Chemistry, Granada, 2016. ; KALOGIOURI et al., 2016).

Volatile organic compounds (VOC)

Regular consumption of virgin olive oil is associated with health benefits; in addition, this type of product is appreciated all over the world for its flavor and aroma, characterized by the presence of various volatile organic compounds (VOCs) from different chemical classes (CECCHI; ALFEI, 2013 CECCHI, T.; ALFEI, B. Volatile profiles of Italian monovarietal extra virgin olive oils via HS-SPME–GC–MS: Newly identified compounds, flavors molecular markers, and terpenic profile. Food Chemistry, London, v.141, n.3, p.2025-2035, 2013. ). Both positive attributes and sensory defects in olive oils can be associated with volatile compounds. The absence of sensory defects is necessary for the product to be classified as extra virgin olive oil (ANGEROSA et al., 1999 ANGEROSA, F.; BASTI, C.; VITO, R. Virgin olive oil volatile compounds from lipoxygenase pathway and characterization of some Italian cultivars. Journal of Agricultural and Food Chemistry, Washington, v.47, n.3, p.836-839, 1999. ).

The sensory quality of olive oils is largely related to the perception of aroma, flavor and color, decisively influencing recognition, selection, and acceptability of this type of product by consumers. The perception of aroma in olive oils is the result of a complex sensory interaction between compounds responsible for flavor and aroma and human olfactory and taste receptors (BOSKOU, 2012 BOSKOU, D. Olive oil: constituents, quality, health properties and bioconversions. London: BoD–Books on Demand, 2012. 500p. ). Non-volatile components, particularly phenolic compounds, stimulate taste receptors and the free endings of trigeminal nerves, stimulating the perception of bitterness, pungency, and astringency, characteristics considered positive attributes in olive oil (SERVILI et al., 2004 SERVILI, M.; SELVAGGINI, R.; ESPOSTO, S.; TATICCHI, A.; MONTEDORO, G.; MOROZZI, G. Health and sensory properties of virgin olive oil hydrophilic phenols: agronomic and technological aspects of production that affect their occurrence in the oil. Journal of Chromatography A, Amsterdam, v.1054, n.1-2, p.113-127, 2004. ; BENDINI et al., 2007 BENDINI, A.; CERRETANI, L.; CARRASCO-PANCORBO, A.; GÓMEZ-CARAVACA, A.M.; SEGURA-CARRETERO, A.; FERNÁNDEZ-GUTIÉRREZ, A., LERCKER, G. Phenolic molecules in virgin olive oils: a survey of their sensory properties, health effects, antioxidant activity and analytical methods.An overview of the last decade Alessandra. Molecules, Basel, v.12, n.8, p.1679-1719, 2007. ).

Aroma is related to a complex mixture of volatile compounds, which also stimulate the olfactory receptors, providing positive or negative attributes to the oil. The peculiar flavor and aroma of olive oils are characterized by a balance between green, fruity, bitter and pungent sensory notes, which provide both the green character and the impression of freshness (APARICIO; LUNA, 2002 APARICIO, R.; LUNA, G. Characterisation of monovarietal virgin olive oils. European Journal of Lipid Science and Technology, Weinheim, v.104, n.9-10, p.614-627, 2002. ; AKACHA; GARGOURI, 2009 AKACHA, N.B.; GARGOURI, M. Enzymatic synthesis of green notes with hydroperoxide-lyase from olive leaves and alcohol-dehydrogenase from yeast in liquid/gas reactor. Process Biochemistry, Barking, v.44, n.10, p.1122-1127, 2009. ).

VOCs described in literature as aroma components of olive oils are compounds of low molecular weight (<300 Da) and of different chemical nature, being present at very low concentrations. Such compounds, often fat-soluble and capable of binding to proteins (membrane receptors), volatilize at room temperature, so that, when they reach olfactory receptors, they promote an odor sensation (ANGEROSA et al., 2004 ANGEROSA, F.; SERVILI, M.; SELVAGGINI, R.; TATICCHI, A.; ESPOSTO, S.; MONTEDORO, G. Volatile compounds in virgin olive oil: occurrence and their relationship with the quality. Journal of Chromatography A, Amsterdam, v.1054, n.1-2, p.17-31, 2004. ; CECCHI; ALFEI, 2013) CECCHI, T.; ALFEI, B. Volatile profiles of Italian monovarietal extra virgin olive oils via HS-SPME–GC–MS: Newly identified compounds, flavors molecular markers, and terpenic profile. Food Chemistry, London, v.141, n.3, p.2025-2035, 2013. .

VOCs responsible for the aroma of olive oils are derived from the action of lipoxygenase (LOX) on unsaturated fatty acids. Some of the volatile compounds found in olive oils are present in the intact tissue of olives, while others are formed during the disruption of the cell structure during oil processing due to enzymatic reactions in the presence of oxygen. The main precursors of volatile compounds are fatty acids (particularly linoleic and linolenic) and amino acids (leucine, isoleucine, and valine) (LUNA et al., 2006 LUNA, G.; MORALES, M.; APARICIO, R. Characterisation of 39 varietal virgin olive oils by their volatile compositions. Food Chemistry, London, v.98, n.2, p.243-252, 2006. ). Valine and leucine can be converted into volatile compounds such as esters and branched alcohols (KALUA et al., 2007 KALUA, C.M.; ALLEN, M.S.; BEDGOOD JR., D.R.; BISHOP, A.G.; PRENZLER, P.D.; ROBARDS, K. Olive oil volatile compounds, flavour development and quality: A critical review. Food Chemistry, London, v.100, n.1, p.273-286, 2007. ).

During oil extraction, in the crushing stage, olive tissues are broken and enzymes are released and end up hydrolyzing triglycerides and phospholipids, releasing free fatty acids. These fatty acids are then oxidized by LOX to form hydroperoxides (9 and 13-hydroperoxides). The generated hydroperoxides are subsequently cleaved by hydroperoxide lyases, leading to the formation of shortchain aldehydes such as hexanal, cis-hexenal and transhexenal (Figure 4) (ANGEROSA et al., 2004 ANGEROSA, F.; SERVILI, M.; SELVAGGINI, R.; TATICCHI, A.; ESPOSTO, S.; MONTEDORO, G. Volatile compounds in virgin olive oil: occurrence and their relationship with the quality. Journal of Chromatography A, Amsterdam, v.1054, n.1-2, p.17-31, 2004. ; CECCHI; ALFEI, 2013 CECCHI, T.; ALFEI, B. Volatile profiles of Italian monovarietal extra virgin olive oils via HS-SPME–GC–MS: Newly identified compounds, flavors molecular markers, and terpenic profile. Food Chemistry, London, v.141, n.3, p.2025-2035, 2013. ).

Figure 4
Route for the formation of the main volatile compounds in olive oil and enzymes involved (Source: Adapted from Angerosa et al. (2004)).

Six-carbon aldehydes are unstable and, spontaneously or by enzymatic action, are reduced to alcohols by alcohol dehydrogenase enzymes. These six-carbon alcohols can then be esterified by the activity of alcohol acyltransferase (DUDAREVA et al., 2006 DUDAREVA, N.; NEGRE, F.; NAGEGOWDA, D.A.; ORLOVA, I. Plant volatiles: recent advances and future perspectives. Critical Reviews in Plant Sciences, Lodon, v.25, n.5, p.417-440, 2006. ; AKACHA; GARGOURI, 2009 AKACHA, N.B.; GARGOURI, M. Enzymatic synthesis of green notes with hydroperoxide-lyase from olive leaves and alcohol-dehydrogenase from yeast in liquid/gas reactor. Process Biochemistry, Barking, v.44, n.10, p.1122-1127, 2009. ).

The most abundant compounds that favorably contribute to the aroma of olive oils are aldehydes and alcohols originating from the action of LOX, so that compounds such as aldehydes and alcohols with five and six carbons formed from 13-hydroxyperoxides of linoleic and linolenic acids (e.g., hexanal, cis / trans-hexenal, hexanol, hexenol, acetate esters, pentenol), generally comprise 60-80% of the total volatile compounds and contribute to the green odor and astringency of virgin olive oils and are associated with some of the positive attributes: “Pungent-sweet-floral”, “floral”, “apple-green”, “grass”, and “citrus” (APARICIO; LUNA, 2002 APARICIO, R.; LUNA, G. Characterisation of monovarietal virgin olive oils. European Journal of Lipid Science and Technology, Weinheim, v.104, n.9-10, p.614-627, 2002. ; POULIAREKOU et al., 2011 POULIAREKOU, E.; BADEKA, A.; TASIOULA-MARGARI, M.; KONTAKOS, S.; LONGOBARDI, F.; KONTOMINAS, M.G. Characterization and classification of Western Greek olive oils according to cultivar and geographical origin based on volatile compounds. Journal of Chromatography A, Amsterdam, v.1218, n.42, p.7534-7542, 2011. ).

Compounds formed by fermentation of sugars or transformations of amino acids by exogenous enzymes (usually of microbial activity) and oxidative processes provide negative sensory characteristics compromising the olive oil quality (APARICIO; LUNA, 2002 APARICIO, R.; LUNA, G. Characterisation of monovarietal virgin olive oils. European Journal of Lipid Science and Technology, Weinheim, v.104, n.9-10, p.614-627, 2002. ; KALUA et al., 2007 KALUA, C.M.; ALLEN, M.S.; BEDGOOD JR., D.R.; BISHOP, A.G.; PRENZLER, P.D.; ROBARDS, K. Olive oil volatile compounds, flavour development and quality: A critical review. Food Chemistry, London, v.100, n.1, p.273-286, 2007. ; PROCIDA et al., 2016 PROCIDA, G.; CICHELLI, A.; LAGAZIO, C.; CONTE, L.S. Relationships between volatile compounds and sensory characteristics in virgin olive oil by analytical and chemometric approaches. Journal of the Science of Food and Agriculture, New York, v.96, n.1, p.311-318, 2016. ). Volatile components such as monounsaturated aldehydes (7 to 11 carbons), dienes (6 to 10 carbons), branched aldehydes (5 carbons), and alcohols or some ketones (8 carbons) can reach relatively high concentrations in oils and are characterized as “off-flavors”, that is, volatiles that confer sensory defects or strange flavors (APARICIO; LUNA, 2002 APARICIO, R.; LUNA, G. Characterisation of monovarietal virgin olive oils. European Journal of Lipid Science and Technology, Weinheim, v.104, n.9-10, p.614-627, 2002. ; RALLO et al., 2018 RALLO, L.; DÍEZ, C.M.; MORALES-SILLERO, A.; MIHO, H.; PRIEGO-CAPOTE, F.; RALLO, P. Quality of olives: A focus on agricultural preharvest factors. Scientia Horticulturae, Wageningen, v.233, p.491-509, 2018. ).

The contribution of VOCs to the global aroma of olive oils depends not only on their concentration, but also on their sensory threshold values (ANGEROSA et al., 2004 ANGEROSA, F.; SERVILI, M.; SELVAGGINI, R.; TATICCHI, A.; ESPOSTO, S.; MONTEDORO, G. Volatile compounds in virgin olive oil: occurrence and their relationship with the quality. Journal of Chromatography A, Amsterdam, v.1054, n.1-2, p.17-31, 2004. ; KALUA et al., 2005 KALUA, C.M.; ALLEN, M.S.; BEDGOOD, D.R.; BISHOP, A.G.; PRENZLER, PD. Discrimination of olive oils and fruits into cultivars and maturity stages based on phenolic and volatile compounds. Journal of Agricultural and Food Chemistry, Washington, v.53, n.20, p.8054-8062, 2005. ). In addition, antagonism and / or synergism between different molecules can occur and affect the final flavor of olive oils. Chemical aspects of molecules (volatility, hydrophobic character, size, shape, and conformational structure) and the type and position of functional groups affect the sensory threshold value and, therefore, odor and taste intensity. All these aspects contribute to favor the interaction with receptor proteins and, for this reason, the sensory threshold is more important than its concentration. Thus, highly concentrated VOCs are not necessarily the main odor contributors (ANGEROSA et al., 2004 ANGEROSA, F.; SERVILI, M.; SELVAGGINI, R.; TATICCHI, A.; ESPOSTO, S.; MONTEDORO, G. Volatile compounds in virgin olive oil: occurrence and their relationship with the quality. Journal of Chromatography A, Amsterdam, v.1054, n.1-2, p.17-31, 2004. ; POULIAREKOU et al., 2011 POULIAREKOU, E.; BADEKA, A.; TASIOULA-MARGARI, M.; KONTAKOS, S.; LONGOBARDI, F.; KONTOMINAS, M.G. Characterization and classification of Western Greek olive oils according to cultivar and geographical origin based on volatile compounds. Journal of Chromatography A, Amsterdam, v.1218, n.42, p.7534-7542, 2011. ).

The qualitative and quantitative composition of VOCs is strongly dependent on the levels and activity of enzymes involved in the biosynthetic pathway. The production of metabolites also changes in relation to the maturation level, geographic region, and conditions used during olive oil extraction and processing. The content of each volatile compound from the LOX pathway presents a different evolution pattern in relation to the extent of fruit pigmentation; in addition, fruits of different cultivars grown under the same environmental conditions lead to different volatile compound profiles, as well as fruits of the same cultivar produced in different geographic regions (ANGEROSA et al., 1999 ANGEROSA, F.; BASTI, C.; VITO, R. Virgin olive oil volatile compounds from lipoxygenase pathway and characterization of some Italian cultivars. Journal of Agricultural and Food Chemistry, Washington, v.47, n.3, p.836-839, 1999. ; KALUA et al., 2007 KALUA, C.M.; ALLEN, M.S.; BEDGOOD JR., D.R.; BISHOP, A.G.; PRENZLER, P.D.; ROBARDS, K. Olive oil volatile compounds, flavour development and quality: A critical review. Food Chemistry, London, v.100, n.1, p.273-286, 2007. ).

Table 3 shows volatile compounds identified in olive oils obtained from cultivar Arbequina produced in different states of Brazil (Minas Gerais, São Paulo, and Paraná) (ZAGO et al., 2019 ZAGO, L.; SQUEO, G.; BERTONCINI, E.I.; DIFONZO, G.; CAPONIO, F. Chemical and sensory characterization of Brazilian virgin olive oils. Food Research International, New York, v.126, p.108588, 2019. ). Thus, it is possible to verify the effect of the environment on the performance of the same cultivar, since the profile and abundance of volatile compounds varied according to the environmental conditions characteristic of each region. In addition to the influence on the sensory characteristics and flavor profile of olive oils, VOCs can potentially authenticate the geographical origin of this type of product in order to identify markers of geographical or cultivar origin.

Table 3
Volatile compounds (mg kg-1 of olive oil) identified among Brazilian oils from cultivar Arbequina grown in Minas Gerais (MG), São Paulo (SP) and Paraná (PR) *.

In Brazil, sensory analysis is among assessments listed in Normative Instruction No. 01/2012 of MAPA, which establishes identity and quality standards for olive oil. However, the legislation does not require producers to assess the sensory characteristics of their products.

In addition to the need for a permanent team of trained panelists, panel testing is an expensive and slow procedure, which is not always available to small and medium-size companies (ROMERO et al., 2015 ROMERO, I.G.; GARCÍA-GONZÁLEZ, D.L.; APARICIO-RUIZ, R.; MORALES, M.T. Validation of SPME–GCMS method for the analysis of virgin olive oil volatiles responsible for sensory defects. Talanta, New York, v.134, p.394-401, 2015. ). In addition, only laboratories accredited by IOC are able to carry out such an analysis, and in Latin America, only Argentina and Chile have accredited laboratories. The proposal of validating sensory analysis methods independently, similar to what has been performed for other foods, is a research priority to be considered.

The international method for the organoleptic assessment of olive oils, proposed by IOC, is based on the intensity of defects and attributes perceived by a group of selected and trained panelists. The main positive attributes are fruity, bitter, and pungent, while defects include old, mold, wine, acid, rancid, among others. According to the detection and intensity of these sensory defects, olive oils are classified into extra virgin, virgin, ordinary or lampante categories (IOOC, 2013 IOC - International Olive Council. Trade standard applying to olive oil and olive-pomace oil. Madrid, 2013. (COI/T.15/NC No 3/Rev.7) ).

In addition to sensory analysis, many analytical procedures have been used to isolate, identify, and quantify volatile compounds that characterize the aroma of olive oils. The most common analytical method used for the extraction of volatile compounds is solid phase microextraction (SPME). It is a sample preparation technique in which volatile components are adsorbed in a polymeric matrix and later desorbed in the gas chromatography system coupled to flame ionization detector (FID) or mass spectrometry (ANGEROSA et al., 2004 ANGEROSA, F.; SERVILI, M.; SELVAGGINI, R.; TATICCHI, A.; ESPOSTO, S.; MONTEDORO, G. Volatile compounds in virgin olive oil: occurrence and their relationship with the quality. Journal of Chromatography A, Amsterdam, v.1054, n.1-2, p.17-31, 2004. ; TEMIME et al., 2006 TEMIME, S.B.; CAMPEOL, E.; CIONI, P.L.; DAOUD, D.; ZARROUK, M. Volatile compounds from Chétoui olive oil and variations induced by growing area. Food Chemistry, London, v.99, n.2, p.315-325, 2006. ).

In Brazil, sensory analysis is among assessments listed in Normative Instruction No. 01/2012 of MAPA, which establishes identity and quality standards for olive oil. However, the legislation does not require producers to assess the sensory characteristics of their products.

In addition to the need for a permanent team of trained panelists, panel testing is an expensive and slow procedure, which is not always available to small and medium-size companies (ROMERO et al., 2015 ROMERO, I.G.; GARCÍA-GONZÁLEZ, D.L.; APARICIO-RUIZ, R.; MORALES, M.T. Validation of SPME–GCMS method for the analysis of virgin olive oil volatiles responsible for sensory defects. Talanta, New York, v.134, p.394-401, 2015. ). In addition, only laboratories accredited by IOC are able to carry out such an analysis, and in Latin America, only Argentina and Chile have accredited laboratories. The proposal of validating sensory analysis methods independently, similar to what has been performed for other foods, is a research priority to be considered.

The international method for the organoleptic assessment of olive oils, proposed by IOC, is based on the intensity of defects and attributes perceived by a group of selected and trained panelists. The main positive attributes are fruity, bitter, and pungent, while defects include old, mold, wine, acid, rancid, among others. According to the detection and intensity of these sensory defects, olive oils are classified into extra virgin, virgin, ordinary or lampante categories (IOOC, 2013 IOC - International Olive Council. Trade standard applying to olive oil and olive-pomace oil. Madrid, 2013. (COI/T.15/NC No 3/Rev.7) ).

In addition to sensory analysis, many analytical procedures have been used to isolate, identify, and quantify volatile compounds that characterize the aroma of olive oils. The most common analytical method used for the extraction of volatile compounds is solid phase microextraction (SPME). It is a sample preparation technique in which volatile components are adsorbed in a polymeric matrix and later desorbed in the gas chromatography system coupled to flame ionization detector (FID) or mass spectrometry (ANGEROSA et al., 2004 ANGEROSA, F.; SERVILI, M.; SELVAGGINI, R.; TATICCHI, A.; ESPOSTO, S.; MONTEDORO, G. Volatile compounds in virgin olive oil: occurrence and their relationship with the quality. Journal of Chromatography A, Amsterdam, v.1054, n.1-2, p.17-31, 2004. ; TEMIME et al., 2006 TEMIME, S.B.; CAMPEOL, E.; CIONI, P.L.; DAOUD, D.; ZARROUK, M. Volatile compounds from Chétoui olive oil and variations induced by growing area. Food Chemistry, London, v.99, n.2, p.315-325, 2006. ).

The solid phase consists of a fine fused silica fiber covered with polymeric material used as stationary phase in which volatile substances are adsorbed. Fibers with different coatings are available, depending on the type of matrix to be analyzed. In the case of olive oil samples, the best extraction efficiency is obtained by using fibers with coating material composed of three types of material, Divinylbenzene / Carboxen / Polydimethylsiloxane (DVB/ CAR / PDMS) (CAVALLI et al., 2003 CAVALLI, J.F.; FERNANDEZ, X.; LIZZANI-CUVELIER, L.; LOISEAU, A.M. Comparison of static headspace, headspace solid phase microextraction, headspace sorptive extraction, and direct thermal desorption techniques on chemical composition of French olive oils. Journal of Agricultural and Food Chemistry, Washington, v.51, n.26, p.7709-7716, 2003. ; ANGEROSA et al., 2004 ANGEROSA, F.; SERVILI, M.; SELVAGGINI, R.; TATICCHI, A.; ESPOSTO, S.; MONTEDORO, G. Volatile compounds in virgin olive oil: occurrence and their relationship with the quality. Journal of Chromatography A, Amsterdam, v.1054, n.1-2, p.17-31, 2004. ). For the collection of volatile compounds, the method consists of exposing, for a determined period (equilibrium time), the fiber to the vapor phase (headspace) in equilibrium with the sample contained in a temperaturecontrolled flask, sealed with a perforable septum, and under stirring, as illustrated in Figure 5. Thus, substances are concentrated and adsorbed on the fiber, being directly desorbed on the gas chromatograph injector (ANGEROSA et al., 2004 ANGEROSA, F.; SERVILI, M.; SELVAGGINI, R.; TATICCHI, A.; ESPOSTO, S.; MONTEDORO, G. Volatile compounds in virgin olive oil: occurrence and their relationship with the quality. Journal of Chromatography A, Amsterdam, v.1054, n.1-2, p.17-31, 2004. ).

Figure 5
Representation of the procedure for extracting volatile compounds using the solid phase microextraction (SPME) technique (Source: Filoda, P.F).

Olive oil is a complex matrix, containing volatile compounds of different chemical classes, with different physicochemical properties, such as volatility and polarity.

Thus, it is expected that these different compounds have different equilibrium times. As the SPME technique is a multiphase equilibrium process, the tendency is a progressive enrichment of less volatile compounds with the increase in equilibrium time (CUI et al., 2009 CUI, S.; TAN, S.; OUYANG, G.; JIANG, S.; PAWLISZYN, J. Headspace solid-phase microextraction gas chromatography–mass spectrometry analysis of Eupatorium odoratum extract as an oviposition repellent. Journal of Chromatography B, Amsterdan, v.877, n.20-21, p.1901-1906, 2009. ). It is expected that the combination of data from sensory analysis and those from organic volatile compounds would allow distinguishing cultivars and collection sites in order to be used as a distinctive sign for products.

Concluding remarks

The production of olive trees in Brazil is recent (mid-2003) and the knowledge about the crop is based on the performance of cultivars in traditional cultivation regions (Mediterranean Basin). However, it is necessary to generate knowledge from actual cultivation conditions, since different soils and climates found in different regions of Brazil provide different cultivation conditions and, consequently, different characteristics to olive oils. Thus, the measurements of olive oil quality variables can help determine the adaptability of cultivars to the local edaphic and climatic conditions, enabling producers to strengthen the identity of the products and adequately position them in the market.

Acknowledgments

This work was carried out with support from the Coordination for the Improvement of Higher Education Personnel - Brazil (CAPES) - Financing Code 001 (P.F. Filoda, scholarship), and from the National Council for Scientific and Technological Development (CNPq) (J.F. Hoffman, fellowship 312706/2020-0).

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Publication Dates

  • Publication in this collection
    05 July 2021
  • Date of issue
    2021

History

  • Received
    29 Nov 2020
  • Accepted
    20 Apr 2021
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