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Page 1: The Extra-Virgin Olive Oil Handbook (Peri/The Extra-Virgin Olive Oil Handbook) || Virgin olive oil: definition and standards

2Virgin olive oil: definitionand standardsManuela MariottiDepartment of Food, Environmental and Nutritional Sciences,University of Milan, Milan, Italy

Abstract

Basic information is given about virgin olive oil standards according to Europeanlegislation. Standards are divided into two groups: (i) quality standards aimed atclassifying extra-virgin, virgin and inedible ‘lampante’ olive oil and (ii) authenticitystandards aimed at identifying oil adulteration by mixing virgin olive oil with refinedolive oil or oil of other kinds. The importance and meaning of free acidity, peroxidevalue, UV absorption values and sensory defects are discussed.

2.1 The legal definition of virgin olive oil

Definitions and standards for virgin olive oil are primarily based on European legis-lation, especially Commission Regulation (EC) No. 1019/2002 of 13 June 2002, onmarketing standards for olive oil, and Commission Regulation (EC) No. 702/2007of 21 June 2007, on the characteristics of olive oil and on the relevant methodsof analysis. Other standardization organizations, such as the International OliveCouncil (IOC; www.internationaloliveoil.org/) and The Codex Alimentarius Com-mission (www.codexalimentarius.org/), take part in defining olive oil standards, butEuropean legislation is the first and main reference worldwide. The European Com-munity recognizes several categories of olive oil, each with its particular qualitiesand market value.

Virgin olive oil is defined by EC Regulation No 1019/2002 (Art. 3) as follows:‘Virgin olive oil is the olive oil obtained directly from olives and solely by mechani-cal means.’ Conformity with this definition is the basic authenticity requirement forvirgin olive oil.

The Extra-Virgin Olive Oil Handbook, First Edition. Edited by Claudio Peri.© 2014 John Wiley & Sons, Ltd. Published 2014 by John Wiley & Sons, Ltd.

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12 CH02 VIRGIN OLIVE OIL: DEFINITION AND STANDARDS

Three categories of virgin olive oil are further defined, based on quality criteria, as:‘extra-virgin olive oil’, ‘virgin olive oil’ and ‘lampante olive oil’. Lampante (literally‘lamp oil’ according to its use in ancient times) is a virgin olive oil obtained frombad fruit or careless processing and it is of such a low quality that it cannot be usedfor human consumption and must be refined in order to become edible.

Regulation (EU) No 29/2012, dated 13 January 2012, codifies the substantialamendments that have taken place since regulation No 1019 on olive oil market-ing standards was introduced in 2002. One of those, Council Regulation (EC) No1234/2007 of 22 October 2007, establishes a common organization of agriculturalmarkets and specific provisions for certain agricultural products, olive oil included.According to this regulation, ‘virgin olive oils’ are defined as:

“oils obtained from the fruit of the olive tree solely by mechanical or other physi-cal means under conditions that do not lead to alterations in the oil, which have notundergone any treatment other than washing, decantation, centrifugation or filtration,to the exclusion of oils obtained using solvents or adjuvants having a chemical or bio-chemical action, or by re-esterification processes and any mixture with oils of otherkinds.”

Commission Regulation (EC) No 702/2007 of 21 June 2007 defines the analyticaland sensory standards of all the categories of olive oils, virgin or refined. Only thestandards related to the three categories of virgin olive oil are presented here. Thesestandards have been established by law as indicators of oil quality and authenticity.

Quality standards are analytical parameters that allow virgin olive oils to be classi-fied according to a scale of quality. In general, these parameters indicate oil spoilage.Therefore, it is assumed that the lower their values, the higher the quality of the oil.

Authenticity standards are analytical parameters that allow an oil to be declared as‘virgin’, in compliance with the definition reported above. In general, these param-eters indicate the presence of refined olive oil (violation of the condition of ‘solelyby mechanical means’) or other vegetable oils (violation of the condition of beingobtained ‘directly from olives’).

2.2 Quality standards of virgin olive oil

Quality standards of virgin olive oil can be divided into two groups: chemical andsensory standards.

2.2.1 Chemical quality standards

The chemical standards that must be evaluated for classifying the quality levelsof virgin olive oils are reported in Table 2.1. Quality standards are useful to ver-ify hydrolytic and oxidative degradation that takes place in the olives and the oil

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Table 2.1 Chemical standards of virgin olive oil.

Chemical standard Extra-virgin Virgin Lampante

Free acidity (%) ≤ 0.8 ≤ 2.0 > 2.0

Peroxide index (mEqO2/kg) ≤ 20 ≤ 20 −

K232 ≤ 2.50 ≤ 2.60 −K270 ≤ 0.22 ≤ 0.25 −ΔK ≤ 0.01 ≤ 0.01 −

Spectrophotometric values in the UV at 232 and 270 nm depend on conjugateddouble bonds derived from oxidation (they are therefore quality indicators)or from refining (therefore, they are also authenticity indicators).

during processing and storage. Olive oil producers should concentrate on the qualitystandards presented in Table 2.1, making a coherent decision about the processingprocedure and conditions according to the level of quality they want to achieve.

Free acidity

Hydrolysis of triglycerides due to lipolytic enzymes (lipases) causes free fatty acidsand monoglycerides or diglycerides to be released from the triglycerides. The prod-ucts of the lipolytic reaction are tasteless and odourless and therefore no sensorydefects can be perceived. Hence, it is not correct to refer to ‘acidity’ as a flavoursensation of an olive oil. Sometimes, the sensation of pungency is mistakenly inter-preted as ‘acidity’.

The lipolytic reaction is due to the endogenous lipases that are naturally present inthe olive. When the integrity of the olive is lost due to mechanical action, lipases thatare present in the pulp or in the seed cells come into contact with the oil, originallycontained in specialized vacuoles. At this point, lipolysis starts and free fatty acidsare produced. The reaction accelerates with increase in temperature and is a functionof the time of contact between the lipases and the oil. Lipases are hydrophilic andthey are active only in the presence of an aqueous phase. When water is separated,by decanting and centrifugation, lipolysis slows down or is totally stopped if thewater and cell residues are completely separated from the oil. This is the reasonwhy filtering the oil, removing the suspended materials and partially reducing theamount of water, is important.

In any case, the lipolytic reaction due to the endogenous lipases in the olivesis relatively slow. Oil obtained from healthy fruit, regardless of the cultivar andprocessed just after harvesting, have very low values of free acidity. Free acidityrapidly increases in the presence of moulds and micro-organisms, which producelarge quantities of very active lipases (exogenous lipases). In broken, dirty, unhealthy

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olives, lipase activity causes a rapid increase in free acidity beyond the limits forextra-virgin or virgin olive oils, with an obvious loss in quality and value. A fur-ther and very rapid acceleration of this reaction takes place due to olive fly attacks.The intestines of the olive flies and their excrement, in fact, contain very high con-centrations of lipases that cause a very rapid increase in free acidity. It is mostunfortunate that this happens when the fruit is still on the tree. Thus at harvestingtime, the damage has been irreversibly done. Other factors affecting the integrity ofolives are attacks by parasites, mechanical crushing and bruising, extended contactwith soil, delayed harvesting (over-ripeness), prolonged heaping and storage beforeprocessing.

Free acidity is expressed as the percentage of free fatty acids on the basis of oleicacid, which is the main fatty acid of olive oil. Each producer should be able to deter-mine free acidity at the milling site, not only to verify the quality of the oil, but alsoto avoid mixing good and bad oil.

The legal limit of 0.8% for extra-virgin olive oil is not very demanding. Agood oil should have a free acidity value less than 0.5% and an excellent oil lessthan 0.3%.

Peroxide value and spectrophotometric absorption in the UV

The two main spoiling reactions of olive oil are lipolysis and lipid oxidation. Lipoly-sis can be easily estimated as free acidity, but oxidation is more difficult and complexto evaluate.

Assessment of the degree of olive oil oxidation is based on determinations of boththe primary and secondary products of oxidation. The primary stage of oxidation isthe formation of hydroperoxides from polyunsaturated fatty acids, through a radicalmechanism (see Chapter 6).

Peroxides are primary oxidation products and they are used as indicators of oilquality and stability. Their value increases, reaches a maximum and then decreasesbecause of their further degradation into secondary products of oxidation such asaldehydes, ketones and conjugated dienes. These substances, that are formed at anadvanced stage of oxidation, are responsible for the rancid flavour of the oil.

Thus, the peroxide value is a measure of the degree of oxidation of the oil atan early stage of oxidative spoilage, long before a rancid smell or taste becomesperceivable. An increase in the peroxide value should be considered as a warningsignal that oxidation is taking place.

Spectrophotometric values: Specific absorbances (conventionally indicated as K)are measured in the UV region, at the wavelengths corresponding to the maximumabsorption (about 232 and 270 nm) of secondary products formed in the autoxidationprocess. An increase in absorption at K232 and K270, may also be due to the pres-ence of conjugated dienes and trienes, which are formed in oils that have been heatedduring the refining process. Conjugated dienes contain two double bonds that alter-nate with single bonds. A conjugated triene contains three alternating double bonds.

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Therefore, a high spectrometric value can be considered an indicator of oxidationor of adulteration of the oil.

Peroxide and spectrophotometric values are not easy to evaluate (see framed notebelow). However, they are so important that a good producer seeking high qualitymust have one or both of the analyses carried out as an essential tool of processcontrol.

Lipid oxidation is greatly accelerated by lipolysis because free fatty acids aremore easily oxidizable than fatty acids linked in a triglyceride molecule. Thismeans that there is a synergy between lipid hydrolysis and oxidation in acceleratingoil spoilage. Oil oxidation is also greatly accelerated by the presence of oxidativeenzymes (lipoxidases, lipoxygenases) that are naturally present in the olive pulpand seed cells, and much more in case of moulds and fly spoilage. The removalof water may prevent or eliminate enzymatic oxidizing activity. However, unlikelipolysis, oxidation can also take place in the absence of water by a purely chemical,autocatalytic mechanism.

The legal limit of the peroxide value is 20 meqO2/kg for extra-virgin oil, whichis a very poor standard, as a good oil must have a peroxide value of less than 12,and an excellent oil less than 8. The same can be said for K232, the most reliablespectrophotometric indicator of oil oxidation. The limit of 2.50 is not very selective;it should be lower than 2.10 for a good extra-virgin olive oil and lower than 1.90 foran excellent extra-virgin olive oil.

Analytical methods

Official methods of analysis of olive oils are thoroughly described in Euro-pean legal prescriptions (Commission Regulation (EEC) No 702/2007 amend-ing Commission Regulation (EEC) No 2568/91 on characteristics of olive oiland olive-residue oil and on relevant methods of analysis, 21 June 2007).

According to the official procedure for free acidity, the (filtered) sample isdissolved in a mixture of solvents and the free fatty acids present are titrated withan ethanolic solution of potassium hydroxide using phenolphthalein as indicator.Results are expressed as a percentage by weight of oleic acid. This method isrelatively slow (7–8 samples/h) and solvent consuming (100–150 mL/sample).

The peroxide value is the quantity of those substances in the sample,expressed in terms of milliequivalents of active oxygen per kilogram (meq/kg),which oxidize iodide. The method is based on treatment of the sample insolution in acetic acid and chloroform, with a solution of potassium iodide.The freed iodine is titrated with a standardized sodium thiosulphate solution inthe presence of a starch solution as indicator.

This method is slow and relatively complex, so well-trained technicians areneeded to obtain reliable results.

For the analysis of specrophotometric values, the oil is dissolved in spec-trophotometric pure iso-octane and extinction of the solution is determined at the

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specified wavelengths (232 and 270 nm) with reference to pure solvent. Specificextinctions are calculated from the spectrophotometric readings.

Absorptions are expressed as specific extinctions of a 1% solution of the oilin the specified solvent, in a thickness of 1 cm.

This determination is also relatively complex and requires a spectrophotome-ter for measuring extinction in the ultraviolet between 220 and 360 nm, with thepossibility of reading individual nanometric units.

Simple, portable, easy-to-use, rapid analytical apparatuses are available forfree acidity, peroxide value and, in some cases, total phenolic compounds aswell an oil stability index. These are very useful tools for online control of theproduct. Attention and care are needed for maintenance and calibration and peri-odical testing versus the official methods.

2.2.2 Sensory quality standards

The sensory analysis as a method for the legal recognition and classification of virginolive oil was proposed by the International Olive Council in June 1987, and recog-nized by the European Commission in July 1991 (Commission Regulation (EEC)No 702/2007 amending Commission Regulation (EEC) No 2568/91 on characteris-tics of olive oil and olive-residue oil and on relevant methods of analysis, 21 June2007). The method was further modified and replaced by subsequent amendmentsand finally updated by Commission Regulation (EC) No 640/2008 of 4 July 2008amending Regulation (EEC) No 2568/91 on sensory characteristics of olive oil andthe relevant methods of analysis. The sensory standards for classifying the variouslevels of quality of virgin olive oil are reported in Table 2.2 (see Chapter 4).

Table 2.2 Sensory standards of virgin olive oil.

Sensory standard Extra-virgin Virgin Lampante

Median defect (Md) 0 ≤ 3.5 > 3.5

Median fruity (Mf) > 0 > 0 −

Nonconformity with the requirement of a fruitiness note greater than zero is rare,as it is almost impossible to have a virgin olive oil without any odour and taste.Therefore, conformity to this requirement is very easy to achieve. Nonconformityto the prescription of zero defects, on the other hand, is frequent and may be theconsequence of minor mistakes in processing. Therefore, conformity to this require-ment is difficult to achieve. In addition, due to some difficulties in standardizing andobtaining reproducible results from different panels of tasters, sensory standards aredifficult to be universally defined. The inclusion of sensory requirements among thelegal standards for virgin olive oil was a ‘daring’ decision because sensory analysis

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can detect very low concentrations of good or bad oil components and because it isdifficult to obtain reproducible results of positive and negative sensory attributes.

Probably, when establishing the sensory standards, the legislators did not takeenough care in considering the difference between this requirement and the others. Infact, while the chemical standards measure concentrations of negative componentsat the level of per cent or per thousand, sensory defects are easily detected by humanodour and taste receptors at concentrations that may be in the range of ppm (partsper million) or even ppb (parts per billion). It has been found that when mixing1 mL of rancid oil with 10 L of a perfect oil (1:10 000 dilution), a defect is easilyperceived by trained sensory assessors, while no significant change occurs in thevalues of the chemical indices. In addition, a variation in free acidity or peroxidevalue or K232 requires a massive evolution of spoilage reactions; on the contrary,the presence of a smell or flavour of staleness or rancidity may be due to a veryminor contamination of a good oil. Thus, it is not surprising that some oils thathave very good chemical standards may fail to be classified as extra-virgin oliveoil because of the presence of sensory defects. These defects often arise from thepresence of dead spots in the milling plant (for example, improper plant design) orto uneven distribution of residence times at critical temperature conditions (see the

Table 2.3 Authenticity standards of virgin olive oil: fraudulent mixing with refined olive oil.

Standard Extra-virgin Virgin Lampante Comment

Erythrodiol anduvaol (%)

≤ 4.5 ≤ 4.5 ≤ 4.5 The concentration ofthese components ishigher in refinedolive oil derivedfrom pomace.

Waxes (ppb) ≤ 250 ≤ 250 ≤ 300

Total trans-oleicisomers (%)

≤ 0.05 ≤ 0.05 ≤ 0.10 These components areformed in therefining process.They indicatemixing with refinedolive oil and alsoseed oils.

Total trans-linoleic+trans-linolenicisomers (%)

≤ 0.05 ≤ 0.05 ≤ 0.10

Stigmastediene(mg/kg)a

≤ 0.10 ≤ 0.10 ≤ 0.50

2-glycerilmonopalmitateb

≤ 0.9 or 1.0dependingon palmiticacid con-centration

≤ 0.9 or 1.0dependingon palmiticacid con-centration

≤ 0.9 or 1.0dependingon palmiticacid con-centration

This is an unnaturalarrangement of fattyacids in atriglyceride; itderives fromesterified olive oil.

Notes: aDecreasing the limit value for stigmastediene in virgin olive oil makes it possible to achievebetter separation of virgin and refined olive oil. bExperts have concluded that quantification ofthe percentage of 2-glyceryl monopalmitate is more precise for the detection of esterified oils(Commission Regulation (EC) No 702/2007.)

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hygienic design in Annex 21.1 in Chapter 21). Small quantities of olive paste oroil undergoing intense spoilage, in fact, may act as sensory contaminants of largequantities of good oil.

The identification of olive oil defects through sensory analysis has the disadvan-tage of being a lengthy and expensive methodology, whose final result depends onmany factors, especially the training and experience of the panelists. In recent years,instrumental methods have been proposed, based on the analysis of volatile com-pounds by dynamic headspace high-resolution gas chromatography. This is a moreprecise and reliable technique, but has two critical limitations: in the first place itrequires the use of complex and expensive analytical instruments by highly skilledanalysts; in the second place, establishing a reliable relationship between the instru-mental response and the perceived sensations of a panelist or a consumer is still amatter of research and long-term experience. An interesting alternative for rapid,in-line evaluation of both negative and positive odour notes is the use of sensorsto detect the volatile compounds present in the headspace of an oil container (theelectronic nose). An interesting review on the different techniques applied to oliveoil aroma analysis, with their advantages and disadvantages, has been published byEscuderos et al. (2007).

Table 2.4 Authenticity standards of virgin olive oil: fraudulent mixing with other vegetable oils.

Standard Extra-virgin Virgin Lampante Comment

ECN42a ≤ 0.2 ≤ 0.2 ≤ 0.3 A higher value of thisstandard indicatesmixing with seed oilsrich in linoleic acid

Fatty acids (%)(myristic,linolenic,arachidic,eicosenoic,behenic,lignoceric andothers)

A maximumvaluedepending onthe fatty acid(range:0.05–1.0)

A maximumvaluedepending onthe fatty acid(range:0.05–1.0)

A maximumvaluedepending onthe fatty acid(range:0.05–1.0)

The fatty acid compositionof oils is considered asa fingerprint of anoil-bearing species.Therefore the presenceand concentration ofsome fatty acidsindicates mixing withother vegetable oils

β-sitosterol ≥ 93.0 ≥ 93.0 ≥ 93.0 93.0% β-sitosterol is theminimum for olive oil;mixing with other oilsresults in a lowerconcentration of thissterol

Note: aECN – equivalent chain number. The ECN is the actual carbon number minus twice thenumber of double bonds per molecule. Olive oil, different from most seed oils, has mainly triglyc-erides with ECNs 44, 46, 48, and 50; triglycerides with ECN40 and ECN42 are absent or foundin trace amounts, respectively. Therefore, evaluation of ECN42, which varies according to thecontent of glycerol trilinoleate, is an effective tool to detect more unsaturated oils.

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2.3 Authenticity standards of virgin olive oil

Authenticity standards are used to detect frauds that may derive from: (i) the use ofprohibited additives or technological adjuvants; (ii) the use of prohibited technologi-cal operations as, for example, deacidifying and deodorizing by vacuum evaporationand steam stripping, or (iii) mixing with refined olive oil or other vegetable oils.

The main chemical standards that are evaluated for detecting extra-virgin oliveoil adulteration are reported in Tables 2.3 and 2.4.

Reference

Escuderos, M.E., Uceda, M., Sánchez, S. and Jiménez, A. (2007) Olive oil sensoryanalysis techniques evolution. European Journal of Lipid Science and Technology109, 536–546.


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