Commission Regulation (EEC) No 2568/91 of 11 July 1991 on the characteristics of olive oil and olive-residue oil and on the relevant methods of analysis
Modified by
- Commission Regulation (EEC) No 3682/91of 17 December 1991amending Regulation (EEC) No 2568/91 on the characteristics of olive oil and olive-residue oil and on the relevant methods of analysis, 31991R3682, December 18, 1991
- Commission Regulation (EEC) No 1429/92of 26 May 1992amending Regulation (EEC) No 2568/91 on the characteristics of olive oil and olive-residue oil and on the relevant methods of analysis, 31992R1429, June 2, 1992
- Commission Regulation (EEC) No 1683/92of 29 June 1992amending Regulation (EEC) No 2568/91 on the characteristics of olive oil and olive-residue oil and on the relevant methods of analysis, 31992R1683, June 30, 1992
- Commission Regulation (EEC) No 1996/92of 15 July 1992amending Regulation (EEC) No 2568/91 on the characteristics of olive oil and olive-residue oil and on the relevant methods of analysis, 31992R1996, July 18, 1992
- Commission Regulation (EEC) No 3288/92of 12 November 1992amending Regulation (EEC) No 2568/91 on the characteristics of olive oil and olive-residue oil and of the relevant methods of analysis, 31992R3288, November 13, 1992
- Commission Regulation (EEC) No 183/93of 29 January 1993amending Regulation (EEC) No 2568/91 on the characteristics of olive oil and olive-residue oil and on the relevant methods of analysisCorrigendum to Commission Regulation (EEC) No 183/93 of 29 January 1993 amending Regulation (EEC) No 2568/91 on the characteristics of olive oil and olive-residue oil and on the relevant methods of analysis(Official Journal of the European Communities No L 22 of 30 January 1993)Commission Regulation (EEC) No 826/93of 6 April 1993amending Regulation (EEC) No 183/93 amending Regulation (EEC) No 2568/91 on the characteristics of olive oil and olive-residue oil and on the relevant methods of analysis, 31993R018331993R0183R(02)31993R0826, January 30, 1993
- Commission Regulation (EEC) No 826/93of 6 April 1993amending Regulation (EEC) No 183/93 amending Regulation (EEC) No 2568/91 on the characteristics of olive oil and olive-residue oil and on the relevant methods of analysis, 31993R0826, April 7, 1993
- Commission Regulation (EEC) No 620/93of 17 March 1993amending Regulation (EEC) No 2568/91 on the characteristics of olive oil and olive-residue oil and on the relevant methods of analysis, 31993R0620, March 18, 1993
- Commission Regulation (EC) No 177/94of 28 January 1994amending Regulation (EEC) No 2568/91 on the characteristics of olive oil and olive-residue oil and on the relevant methods of analysis, 31994R0177, January 29, 1994
- Commission Regulation (EC) No 2632/94of 28 October 1994amending Regulation (EEC) No 2568/91 on the characteristics of olive oil and olive-residue oil and on the relevant methods of analysis, 31994R2632, October 29, 1994
- Commission Regulation (EC) No 656/95of 28 March 1995amending Regulation (EEC) No 2568/91 on the characteristics of olive oil and olive-residue oil and on the relevant methods of analysis and Council Regulation (EEC) No 2658/87 on the tariff and statistical nomenclature and on the Common Customs Tariff, 31995R0656, March 29, 1995
- Commission Regulation (EC) No 2527/95of 27 October 1995amending Regulation (EEC) No 2568/91 on the characteristics of olive oil and olive-residue oil and on the relevant methods of analysis, 31995R2527, October 28, 1995
- Commission Regulation (EC) No 2472/97of 11 December 1997amending Regulation (EEC) No 2568/91 on the characteristics of olive oil and olive-residue oil and on the relevant methods of analysis and Council Regulation (EEC) No 2658/87 on the tariff and statistical nomenclature and on the Common Customs TariffCorrigendum to Commission Regulation (EC) No 2472/97 of 11 December 1997 amending Regulation (EEC) No 2568/91 on the characteristics of olive oil and olive-residue oil and on the relevant methods of analysis and Council Regulation (EEC) No 2658/87 on the tariff and statistical nomenclature and on the Common Customs Tariff(Official Journal of the European Communities L 341 of 12 December 1997), 31997R247231997R2472R(04), December 12, 1997
- Commission Regulation (EC) No 282/98of 3 February 1998amending Regulation (EEC) No 2568/91 on the characteristics of olive oil and olive-residue oil and on the relevant methods of analysis, 31998R0282, February 4, 1998
- Commission Regulation (EC) No 2248/98of 19 October 1998amending Regulation (EEC) No 2568/91 on the characteristics of olive oil and olive-residue oil and on the relevant methods of analysis and the additional notes in Annex I to Council Regulation (EEC) No 2658/87 on the tariff and statistical nomenclature and on the Common Customs Tariff, 31998R2248, October 20, 1998
- Commission Regulation (EC) No 379/1999of 19 February 1999amending Regulation (EEC) No 2568/91 on the characteristics of olive oil and olive-residue oil and on the relevant methods of analysis, 31999R0379, February 20, 1999
- Commission Regulation (EC) No 455/2001of 6 March 2001amending Regulation (EEC) No 2568/91 on the characteristics of olive oil and olive-residue oil and on the relevant methods of analysis, 32001R0455, March 7, 2001
- Commission Regulation (EC) No 2042/2001of 18 October 2001amending Regulation (EEC) No 2568/91 on the characteristics of olive oil and olive-residue oil and on the relevant methods of analysis and the Additional Note in Annex I to Council Regulation (EEC) No 2658/87 on the tariff and statistical nomenclature and on the Common Customs Tariff, 32001R2042, October 19, 2001
- Commission Regulation (EC) No 796/2002of 6 May 2002amending Regulation (EEC) No 2568/91 on the characteristics of olive oil and olive-pomace oil and on the relevant methods of analysis and the additional notes in the Annex to Council Regulation (EEC) No 2658/87 on the tariff and statistical nomenclature and on the Common Customs Tariff, 32002R0796, May 15, 2002
- Commission Regulation (EC) No 1989/2003of 6 November 2003amending Regulation (EEC) No 2568/91 on the characteristics of olive oil and olive-pomace oil and on the relevant methods of analysis, 32003R1989, November 13, 2003
- Commission Regulation (EC) No 702/2007of 21 June 2007amending Commission Regulation (EEC) No 2568/91 on the characteristics of olive oil and olive-residue oil and on the relevant methods of analysis, 32007R0702, June 22, 2007
- Commission Regulation (EC) No 640/2008of 4 July 2008amending Regulation (EEC) No 2568/91 on the characteristics of olive oil and olive-residue oil and on the relevant methods of analysis, 32008R0640, July 5, 2008
- Commission Regulation (EU) No 61/2011of 24 January 2011amending Regulation (EEC) No 2568/91 on the characteristics of olive oil and olive-residue oil and on the relevant methods of analysis, 32011R0061, January 27, 2011
- Commission Implementing Regulation (EU) No 661/2012of 19 July 2012correcting the Slovenian version of Commission Regulation (EEC) No 2568/91 on the characteristics of olive oil and olive-residue oil and on the relevant methods of analysis, 32012R0661, July 20, 2012
- Commission Implementing Regulation (EU) No 299/2013of 26 March 2013amending Regulation (EEC) No 2568/91 on the characteristics of olive oil and olive-residue oil and on the relevant methods of analysis, 32013R0299, March 28, 2013
- Commission Implementing Regulation (EU) No 1348/2013of 16 December 2013amending Regulation (EEC) No 2568/91 on the characteristics of olive oil and olive-residue oil and on the relevant methods of analysis, 32013R1348, December 17, 2013
- Commission Delegated Regulation (EU) 2015/1830of 8 July 2015amending Regulation (EEC) No 2568/91 on the characteristics of olive oil and olive-residue oil and on the relevant methods of analysis, 32015R1830, October 13, 2015
- Commission Implementing Regulation (EU) 2015/1833of 12 October 2015amending Regulation (EEC) No 2568/91 on the characteristics of olive oil and olive-residue oil and on the relevant methods of analysis, 32015R1833, October 13, 2015
- Commission Implementing Regulation (EU) 2016/1227of 27 July 2016amending Regulation (EEC) No 2568/91 on the characteristics of olive oil and olive-residue oil and on the relevant methods of analysis, 32016R1227, July 28, 2016
- Commission Implementing Regulation (EU) 2016/1784of 30 September 2016amending Regulation (EEC) No 2568/91 on the characteristics of olive oil and olive-residue oil and on the relevant methods of analysis, 32016R1784, October 8, 2016
- Commission Delegated Regulation (EU) 2016/2095of 26 September 2016amending Regulation (EEC) No 2568/91 on the characteristics of olive oil and olive-residue oil and on the relevant methods of analysisCorrigendum to Commission Delegated Regulation (EU) 2016/2095 of 26 September 2016 amending Regulation (EEC) No 2568/91 on the characteristics of olive oil and olive-residue oil and on the relevant methods of analysis(Official Journal of the European Union L 326 of 1 December 2016), 32016R209532016R2095R(01), December 1, 2016
- Commission Implementing Regulation (EU) 2019/1604of 27 September 2019amending Regulation (EEC) No 2568/91 on the characteristics of olive oil and olive-residue oil and on the relevant methods of analysis, 32019R1604, September 30, 2019
Corrected by
- Corrigendum to Commission Regulation (EEC) No 2568/91 of 11 July 1991 on the characteristics of olive oil and olive-residue oil and on the relevant methods of analysis, 31991R2568R(05), November 28, 1992
- Corrigendum to Commission Regulation (EEC) No 183/93 of 29 January 1993 amending Regulation (EEC) No 2568/91 on the characteristics of olive oil and olive-residue oil and on the relevant methods of analysis, 31993R0183R(02), July 20, 1993
- Corrigendum to Commission Regulation (EC) No 2472/97 of 11 December 1997 amending Regulation (EEC) No 2568/91 on the characteristics of olive oil and olive-residue oil and on the relevant methods of analysis and Council Regulation (EEC) No 2658/87 on the tariff and statistical nomenclature and on the Common Customs Tariff, 31997R2472R(04), March 28, 1998
- Corrigendum to Commission Delegated Regulation (EU) 2016/2095 of 26 September 2016 amending Regulation (EEC) No 2568/91 on the characteristics of olive oil and olive-residue oil and on the relevant methods of analysis, 32016R2095R(01), August 17, 2017
(a) for the determination of the free fatty acids, expressed as the percentage of oleic acid, the method set out in Annex II; (b) for the determination of the peroxide index, the method set out in Annex III; (c) for determination of the wax content, the method set out in Annex IV; (d) for the determination of the composition and content of sterols and triterpene dialcohols by capillary-column gas chromatography, the method set out in Annex V; (e) for the determination of the percentage of 2- glyceryl monopalmitate, the method set out in Annex VII; (f) for spectrophotometric analysis, the method set out in Annex IX; (g) for the determination of the fatty acid composition, the method set out in Annex X; (h) for the determination of the volatile halogenated solvents, the method set out in Annex XI; (i) for the evaluation of the organoleptic characteristics of virgin olive oil, the method set out in Annex XII; (j) for the determination of stigmastadienes, the method set out in Annex XVII; (k) for determining the content of triglycerides with ECN42, the method set out in Annex XVIII; (l) for the determination of the composition and content of sterols and for the determination of alcoholic compounds, by capillary column gas chromatography, the method set out in Annex XIX; (m) for the determination of the content of waxes, fatty acid methyl esters and fatty acid ethyl esters, the method set out in Annex XX.
(a) the category of oil, the period of production, the price of oils in relation to other vegetable oils, the blending and packing operations, the storage facilities and conditions, the country of origin, the country of destination, the means of transport or the volume of the lot; (b) the position of the operators in the marketing chain, the volume and/or value marketed by them, the range of oil categories they market, the type of business carried out such as milling, storage, refining, blending, packaging or retail sale; (c) findings made during previous checks including the number and type of defects found, the usual quality of oils marketed, the performance of technical equipment used; (d) the reliability of operators’ quality assurance systems or self-checking systems related to the conformity to marketing standards; (e) the place where the check is carried out, in particular if it is the first point of entry into the Union, the last point of exit from the Union or the place where the oils are produced, packaged, loaded or sold to the final consumer; (f) any other information that might indicate a risk of non-compliance.
(a) the criteria for assessing the risk of non-conformity of lots; (b) on the basis of a risk analysis for each risk category, the minimum number of operators or lots and/or quantities which will be subject to a conformity check.
(a) carrying out, in any order, the analyses set out in Annex I; or (b) following the order set out in Annex Ib on the flowchart, until one of the decisions appearing in the flowchart is reached.
the requirements of Annex XII.4 are met, the panel head is given training recognised for this purpose by the Member State, continued approval depends on performance in annual checks arranged by the Member State.
maximum content of each halogenated solvent detected: 0,1 mg/kg, maximum total content of halogenated solvents detected: 0,2 mg/kg.
Category | K | K | Delta-K | Organoleptic evaluation | ||||
---|---|---|---|---|---|---|---|---|
Median of defect (Md) (*) | Fruity median (Mf) | |||||||
≤ 0,80 | ≤ 20,0 | ≤ 2,50 | ≤ 0,22 | ≤ 0,01 | Md = 0,0 | Mf > 0,0 | ≤ 35 | |
≤ 2,0 | ≤ 20,0 | ≤ 2,60 | ≤ 0,25 | ≤ 0,01 | Md ≤ 3,5 | Mf > 0,0 | — | |
> 2,0 | — | — | — | — | Md > 3,5 | — | — | |
≤ 0,30 | ≤ 5,0 | — | ≤ 1,25 | ≤ 0,16 | — | — | ||
≤ 1,00 | ≤ 15,0 | — | ≤ 1,15 | ≤ 0,15 | — | — | ||
— | — | — | — | — | — | — | ||
≤ 0,30 | ≤ 5,0 | — | ≤ 2,00 | ≤ 0,20 | — | — | ||
≤ 1,00 | ≤ 15,0 | — | ≤ 1,70 | ≤ 0,18 | — | — |
Category | Fatty acid composition | ||||||||||
---|---|---|---|---|---|---|---|---|---|---|---|
≤ 0,03 | ≤ 1,00 | ≤ 0,60 | ≤ 0,50 | ≤ 0,20 | ≤ 0,20 | ≤ 0,05 | ≤ 0,05 | ≤ 0,05 | ≤ |0,20| | ≤ 0,9 if total palmitic acid % ≤ 14,00 % | |
≤ 1,0 if total palmitic acid % > 14,00 % | |||||||||||
≤ 0,03 | ≤ 1,00 | ≤ 0,60 | ≤ 0,50 | ≤ 0,20 | ≤ 0,20 | ≤ 0,05 | ≤ 0,05 | ≤ 0,05 | ≤ |0,20| | ≤ 0,9 if total palmitic acid % ≤ 14,00 % | |
≤ 1,0 if total palmitic acid % > 14,00 % | |||||||||||
≤ 0,03 | ≤ 1,00 | ≤ 0,60 | ≤ 0,50 | ≤ 0,20 | ≤ 0,20 | ≤ 0,10 | ≤ 0,10 | ≤ 0,50 | ≤ |0,30| | ≤ 0,9 if total palmitic acid % ≤ 14,00 % | |
≤ 1,1 if total palmitic acid % > 14,00 % | |||||||||||
≤ 0,03 | ≤ 1,00 | ≤ 0,60 | ≤ 0,50 | ≤ 0,20 | ≤ 0,20 | ≤ 0,20 | ≤ 0,30 | — | ≤|0,30| | ≤ 0,9 if total palmitic acid % ≤ 14,00 % | |
≤ 1,1 if total palmitic acid % > 14,00 % | |||||||||||
≤ 0,03 | ≤ 1,00 | ≤ 0,60 | ≤ 0,50 | ≤ 0,20 | ≤ 0,20 | ≤ 0,20 | ≤ 0,30 | — | ≤ |0,30| | ≤ 0,9 if total palmitic acid % ≤ 14,00 % | |
≤ 1,0 if total palmitic acid % > 14,00 % | |||||||||||
≤ 0,03 | ≤ 1,00 | ≤ 0,60 | ≤ 0,50 | ≤ 0,30 | ≤ 0,20 | ≤ 0,20 | ≤ 0,10 | — | ≤ |0,60| | ≤ 1,4 | |
≤ 0,03 | ≤ 1,00 | ≤ 0,60 | ≤ 0,50 | ≤ 0,30 | ≤ 0,20 | ≤ 0,40 | ≤ 0,35 | — | ≤ |0,50| | ≤ 1,4 | |
≤ 0,03 | ≤ 1,00 | ≤ 0,60 | ≤ 0,50 | ≤ 0,30 | ≤ 0,20 | ≤ 0,40 | ≤ 0,35 | — | ≤ |0,50| | ≤ 1,2 |
Category | Sterols composition | ||||||||
---|---|---|---|---|---|---|---|---|---|
≤ 0,5 | ≤ 0,1 | ≤ 4,0 | < Camp. | ≥ 93,0 | ≤ 0,5 | ≥ | ≤ 4,5 | C | |
≤ 0,5 | ≤ 0,1 | ≤ 4,0 | < Camp. | ≥ 93,0 | ≤ 0,5 | ≥ | ≤ 4,5 | C | |
≤ 0,5 | ≤ 0,1 | ≤ 4,0 | — | ≥ 93,0 | ≤ 0,5 | ≥ | ≤ 4,5 | C | |
≤ 0,5 | ≤ 0,1 | ≤ 4,0 | < Camp. | ≥ 93,0 | ≤ 0,5 | ≥ | ≤ 4,5 | C | |
≤ 0,5 | ≤ 0,1 | ≤ 4,0 | < Camp. | ≥ 93,0 | ≤ 0,5 | ≥ | ≤ 4,5 | C | |
≤ 0,5 | ≤ 0,2 | ≤ 4,0 | — | ≥ 93,0 | ≤ 0,5 | ≥ | > 4,5 | C | |
≤ 0,5 | ≤ 0,2 | ≤ 4,0 | < Camp. | ≥ 93,0 | ≤ 0,5 | ≥ | > 4,5 | C | |
≤ 0,5 | ≤ 0,2 | ≤ 4,0 | < Camp. | ≥ 93,0 | ≤ 0,5 | ≥ | > 4,5 | C |
Where the immediate packaging has a capacity of | The primary sample must comprise the oil from |
---|---|
Number of packages in the lot | Minimum number of increments to be selected |
---|---|
Up to 10 | |
From … 11 to 150 | |
From … 151 to 500 | |
From … 501 to | |
From … | |
> | 1 extra increment |
Size of batch (litres) | Number of primary samples |
---|---|
Less than | |
From | |
From | |
From | |
Equal to and more than | 6 + 1 each |
4.1 Analytical balance; 4.2 250 ml conical flask; 4.3 10 ml burette class A, graduated in 0,05 ml, or equivalent automatic burette.
Mass of sample (g) | Weighing accuracy (g) | |
---|---|---|
0 to 2 | 10 | 0,02 |
> 2 to 7,5 | 2,5 | 0,01 |
> 7,5 | 0,5 | 0,001 |
(a) to two decimal places for values from 0 up to and including 1; (b) to one decimal place for values from 1 up to and including 100.
m KIO3 is the mass of potassium iodate, in gramsV 1 is the volume of the potassium iodate solution, in millilitres (5 ml or 10 ml)V 2 is the total volume of potassium iodate solution, in millilitres (250 ml or 500 ml)V 3 is the volume of the sodium thiosulfate solution, in millilitresw KIO3 is the purity of potassium iodate in g/100 gM KIO3 is the molecular mass of potassium iodate (214 g/mol)T is the exact molarity of the sodium thiosulphate solution (mol/l).
0 to 12 | 5,0 to 2,0 |
12 to 20 | 2,0 to 1,2 |
20 to 30 | 1,2 to 0,8 |
30 to 50 | 0,8 to 0,5 |
50 to 90 | 0,5 to 0,3 |
pure hydrogen for gas chromatography, pure air for gas chromatography.
The n-hexane/ethyl ether mixture (99:1) must be prepared every day. For a visual check on the correct elution of the waxes 100 μl of 1 % Sudan in the elution mixture can be added to the sample in solution. Since the colourant has an intermediate retention, between waxes and triglycerides, when the coloration has reached the bottom of the column the elution should be suspended because all the waxes will have been eluted.
column temperature: 20 °C/minute 5 °C/minute 20 °C/minute Initially 80 °C (1′) → 240 °C→ 325 °C(6′) → 340 °C(10′) detector temperature: 350 °C; quantity of substance injected: 1 μl of the n-heptane solution (2-4 ml); carrier gas: helium or hydrogen at the correct linear velocity for the gas selected (see Appendix); instrument sensitivity: suitable for the following conditions:
3.1. 250 ml flask fitted with a reflux condenser with ground-glass joints. 3.2. 500 ml separating funnel. 3.3. 250 ml flasks. 3.4. Complete apparatus for analysis by thin-layer chromatography using 20 x 20 cm glass plates. 3.5. Ultraviolet lamp with a wavelength of 254 or 366 nm. 3.6. 100 μl and 500 μl microsyringes. 3.7. Cylindrical filter funnel with a G3 porous septum (porosity 15-40 μm) of diameter approximately 2 cm and a depth of 5 cm, suitable for filtration under vacuum with male ground-glass joint. 3.8. 50 ml vacuum conical flask with ground-glass female joint, which can be fitted to the filter funnel (point 3.7). 3.9. 10 ml test tube with a tapering bottom and a sealing glass stopper. 3.10. Gas chromatograph suitable for use with a capillary column with split injection system, consisting of: 3.10.1. A thermostatic chamber for columns capable of maintaining the desired temperature with an accuracy of ± 1°C; 3.10.2. A temperature-adjustable injection unit with a persilanised glass vaporising element and split system; 3.10.3. A flame ionisation detector (FID); 3.10.4. Data acquisition system suitable for use with the FID detector (point 3.10.3.), capable of manual integration.
3.11. Fused-silica capillary column of length 20 to 30 m, internal diameter 0,25 to 0,32 mm, coated with 5 % diphenyl - 95 % dimethylpolysiloxane (SE-52 or SE-54 stationary phase or equivalent), to a uniform thickness between 0,10 and 0,30 μm. 3.12. Microsyringe, of 10 ml capacity, for gas chromatography, with cemented needle suitable for split injection. 3.13. Calcium dichloride desiccator
Column temperature: 260 ± 5 °C; Injector temperature: 280-300 °C; Detector temperature: 280-300 °C; Linear velocity of the carrier gas: helium 20 to 35 cm/s; hydrogen 30 to 50 cm/s; Splitting ratio: from 1:50 to 1:100; Instrument sensitivity: from 4 to 16 times the minimum attenuation; Recording sensitivity: 1 to 2 mV full scale; Amount of substance injected: 0,5 to 1 μl of TMSE solution.
The retention time for the ß-sitosterol peak should be at 20 ± 5 min; The campesterol peak should be: for olive oil (mean content 3 %) 20 ± 5 % of full scale; for soybean oil (average content 20 %) 80 ± 10 % of full scale; All the present sterols must be separated. In addition to being separated the peaks, they must also be completely resolved, i.e. the peak trace should return to the base line before leaving for the next peak. Incomplete resolution is, however, tolerated, provided that the peak at RRT 1,02 (Sitostanol) can be quantified using the perpendicular.
Injector temperature (on-column injector) lower than solvent boiling point (68 °C); Detector temperature: 350 °C; Column temperature: programming of furnace temperature: 60 °C for 1 minute, increasing by 15 °C per minute up to 180 °C, then by 5 °C per minute up to 340 °C, then 340 °C for 13 minutes; Carrier gas: hydrogen or helium, set at a linear velocity sufficient to obtain the resolution reflected in Figure 1. The retention time of the C 54 triglyceride must be 40 ± 5 minutes (see Figure 2). (The operating conditions indicated above are indicative. Operators will have to optimise them to obtain the desired resolution. The peak corresponding to 2-glyceryl monopalmitate must have a minimum height equal to 10 % of the recorder scale.)Quantity of substance injected: 0,5-1 μl of the n-hexane solution (5 ml) (5.3.3).
reference to this method, all the information needed for a full identification of the sample, the analysis result, any deviation from the method, whether as the result of a decision by the parties concerned or for another reason, details to identify the laboratory, the date of the analysis and the signatures of those responsible for the analysis.
Category of oil | Method |
---|---|
Virgin olive oil with acidity ≤ 2,0 % |
|
Refined olive oil | |
Olive oil composed of refined olive oil and virgin olive oils | |
Refined olive pomace oil | |
Olive pomace oil | |
|
Injector temperature: | 250 °C |
Detector temperature: | 250 °C |
Oven temperature: | 165 °C (8 min) to 210 °C at 2 °C/min |
Carrier gas hydrogen: | column head pressure, 179 kPa |
Total flow: | 154,0 ml/min; |
Split ratio: | 1:100 |
Injection volume: | 1 μl |
d r(I) is the retention distance of peak I;d r(II) is the retention distance of peak II;t r(I) is the retention time of peak I;t r(II) is the retention time of peak II;ω (I) is the width of the base of peak I;ω (II) is the width of the base of peak II;ω 0,5 is the peak width of the specified compound, at mid-height of the peak;
A i is the area under the peak of the individual fatty acid methyl esteri ;ΣA is the sum of the areas under all the peaks of all the individual fatty acid methyl esters.
m is the mass of the FAMEi i in the reference mixture;Σm is the total of the masses of the various components as FAMEs of the reference mixture.
A i is the area of the FAMEi in the reference mixture;ΣA is the sum of all the areas of all the FAMEs of the reference mixture.
A is the area the FAMEi i ;A is the area of the internal standard;IS F is the correction factor of the fatty acidi i , expressed as FAME;F is the correction factor of the internal standard;IS m is the mass of the test portion, in milligrams m is the mass of the internal standard, in milligrams.IS
injector temperature: 150 °C, column temperature: 70 to 80 °C, detector temperature: 200 to 250 °C.
Fusty/muddy sediment : Characteristic flavour of oil obtained from olives piled or stored in such conditions as to have undergone an advanced stage of anaerobic fermentation, or of oil which has been left in contact with the sediment that settles in underground tanks and vats and which has also undergone a process of anaerobic fermentation.Musty-humid-earthy : Characteristic flavour of oils obtained from fruit in which large numbers of fungi and yeasts have developed as a result of its being stored in humid conditions for several days or of oil obtained from olives that have been collected with earth or mud on them and which have not been washed.Winey-vinegary-acid-sour : Characteristic flavour of certain oils reminiscent of wine or vinegar. This flavour is mainly due to a process of aerobic fermentation in the olives or in olive paste left on pressing mats which have not been properly cleaned and leads to the formation of acetic acid, ethyl acetate and ethanol.Rancid : Flavour of oils which have undergone an intense process of oxidation.Frostbitten olives (wet wood) : Characteristic flavour of oils extracted from olives which have been injured by frost while on the tree.
Characteristic flavour of oils caused by excessive and/or prolonged heating during processing, particularly when the paste is thermally mixed, if this is done under unsuitable thermal conditions. | |
Characteristic flavour of certain oils produced from olives that have dried out. | |
Thick, pasty mouthfeel sensation produced by certain old oils. | |
Flavour of oil reminiscent of that of diesel oil, grease or mineral oil. | |
Flavour acquired by the oil as a result of prolonged contact with vegetable water which has undergone fermentation processes. | |
Flavour of oil extracted from olives which have been preserved in brine. | |
Flavour that is reminiscent of metals. It is characteristic of oil which has been in prolonged contact with metallic surfaces during crushing, mixing, pressing or storage. | |
Characteristic flavour of oil obtained from olives pressed in new esparto mats. The flavour may differ depending on whether the mats are made of green esparto or dried esparto. | |
Flavour of oil obtained from olives which have been heavily attacked by the grubs of the olive fly ( | |
Flavour produced when an oil is hermetically packed for too long, particularly in tin containers, and which is attributed to the formation of 2,6 nonadienal. |
Set of olfactory sensations characteristic of the oil which depends on the variety and comes from sound, fresh olives, either ripe or unripe. It is perceived directly and/or through the back of the nose. | |
Characteristic primary taste of oil obtained from green olives or olives turning colour. It is perceived in the circumvallate papillae on the "V" region of the tongue. | |
Biting tactile sensation characteristic of oils produced at the start of the crop year, primarily from olives that are still unripe. It can be perceived throughout the whole of the mouth cavity, particularly in the throat. |
Robust , when the median of the attribute is more than 6,0;Medium , when the median of the attribute is more than 3,0 and less or equal to 6,0;Delicate , when the median of the attribute is less or equal to 3,0.
Set of olfactory sensations characteristic of the oil which depends on the variety of olive and comes from sound, fresh olives in which neither green nor ripe fruitiness predominates. It is perceived directly and/or through the back of the nose. | |
Set of olfactory sensations characteristic of the oil which is reminiscent of green fruit, depends on the variety of olive and comes from green, sound, fresh olives. It is perceived directly and/or through the back of the nose. | |
Set of olfactory sensations characteristic of the oil which is reminiscent of ripe fruit, depends on the variety of olive and comes from sound, fresh olives. It is perceived directly and/or through the back of the nose. | |
Oil which does not display a lack of balance, by which is meant the olfactory-gustatory and tactile sensation where the median of the bitter attribute and the median of the pungent attribute are not more than 2,0 points above the median of the fruitiness. | |
Oil for which the median of the bitter and pungent attributes is 2,0 or less. |
Terms subject to production of an organoleptic test certificate | Median of the attribute |
---|---|
Fruitiness | — |
Ripe fruitiness | — |
Green fruitiness | — |
Delicate fruitiness | ≤ 3,0 |
Medium fruitiness | 3,0 < Me ≤ 6,0 |
Robust fruitiness | > 6,0 |
Delicate ripe fruitiness | ≤ 3,0 |
Medium ripe fruitiness | 3,0 < Me ≤ 6,0 |
Robust ripe fruitiness | > 6,0 |
Delicate green fruitiness | ≤ 3,0 |
Medium green fruitiness | 3,0 < Me ≤ 6,0 |
Robust green fruitiness | > 6,0 |
Delicate bitterness | ≤ 3,0 |
Medium bitterness | 3,0 < Me ≤ 6,0 |
Robust bitterness | > 6,0 |
Delicate pungency | ≤ 3,0 |
Medium pungency | 3,0 < Me ≤ 6,0 |
Robust pungency | > 6,0 |
Well balanced oil | The median of the bitter attribute and the median of the pungent attribute are not more than 2,0 points above the median of the fruitiness. |
Mild oil | The median of the bitter attribute and the median of the pungent attribute are 2,0 or less. |
glasses (standardised) containing the samples, code numbered, covered with a watch-glass and kept at 28 °C ± 2 °C; profile sheet (see Figure 1) on hard copy, or on soft copy provided that the conditions of the profile sheet are met, together with the instructions for its use if necessary pen or indelible ink trays with slices of apple and/or water, carbonated water and/or rusks glass of water at ambient temperature sheet recalling the general rules listed in sections 8.4 and 9.1.1 spittoons.
They shall not smoke or drink coffee at least 30 minutes before the time set for the test. They must not have used any fragrance, cosmetic or soap whose smell could linger until the time of the test. They must use an unperfumed soap to wash their hands which they shall then rinse and dry as often as necessary to eliminate any smell. They shall fast at least one hour before the tasting is carried out. Should they feel physically unwell, and in particular if their sense of smell or taste is affected, or if they are under any psychological effect that prevents them from concentrating on their work, the tasters shall refrain from tasting and shall inform the panel leader accordingly. When they have complied with the above, the tasters shall take up their place in the booth allotted to them in an orderly, quiet manner. They shall carefully read the instructions given on the profile sheet and shall not begin to examine the sample until fully prepared for the task they have to perform (relaxed and unhurried). If any doubts should arise, they should consult the panel leader in private. They must remain silent while performing their tasks. They must keep their mobile phone switched off at all times to avoid interfering with the concentration and work of their colleagues.
(a) Extra virgin olive oil: the median of the defects is 0,0 and the median of the fruity attribute is above 0,0; (b) Virgin olive oil: the median of the defects is above 0,0 but not more than 3,5 and the median of the fruity attribute is above 0,0; (c) Lampante virgin olive oil: the median of the defects is above 3,5 or the median of the defects is less than or equal to 3,5 and the fruity median is equal to 0,0.
Fusty/muddy sediment | ||||
Musty/humid/earthy | ||||
Rancid | ||||
Other negative attributes: | ||||
Descriptor: | ||||
Fruity | ||||
Green□ | Ripe□ | |||
Bitter | ||||
Pungent | ||||
Name of taster: | Taster code: | |||
Sample code: | Signature: | |||
Date: | ||||
Comments: |
beaker, 300 ml, tall, laboratory centrifuge with 100 ml tubes, beaker, 250 ml, round-bottomed flasks, 100 ml, separating funnel, 1 litre.
aqueous solution of 12 % sodium hydroxide, ethyl alcohol solution of 1 % phenolphtalein, pure hexane, AR, pure propan-2-ol of AR.
round-bottomed flask, 250 ml, with three ground glass necks for the insertion of: (a) a thermometer graduated in degrees and allowing readings to be taken at 90° C; (b) a mechanical stirrer operating at 250 to 300 revolutions per minute, equipped to operate in a vacuum; (c) a vacuum pump connection,
vacuum pump, with a manometer, capable of giving residual pressure of 15 to 30 millibars.
Tabble I: Fatty acid composition as percentage of total fatty acids | Table II: Sterol composition as percentage of total sterols | ||
---|---|---|---|
Myristic acid | M 0,1 | Cholesterol | M 0,5 |
Linolenic acid | M 0,9 | Brassicasterol | M 0,2 |
Arachidic | M 0,7 | Campesterol | M 4,0 |
Eicosanoic acid | M 0,5 | Stigmasterol | < Campesterol |
Behenic acid | M 0,3 | Betasitosterol | m 93,0 |
Lignoceric acid | M 0,5 | Delta-7-stigmastzerol | M 0,5 |
(a) awax content not exceeding 350 mg/kg; (b) an erythrodical and uvaol content not exceeding 4,5 %; (c) a content in saturated fatty acids at the 2-position in the triglycerides not exceeding 1,3 % and/or (d) the sum of transoleic isomers lower than 0,10 % and the sum of translinoleic + translinolenic isomers lower than 0,10 %; (e) one or more of the following characteristics: (i) a periode number exceeding 20 meq 0 2 /kg;(ii) a content in volatile halogenated solvents exceeding 0,1 mg/kg for any one solvent; (iii) a K 270 (100) extinction coefficient higher than 0,250 and, after treatment of the oil with activated alumina, not higher than 0,11. In point of fact some oils having a free fatty acid content, expressed as oleic acid, of more than 3,3 g per 100 g may, after passage through activated alumina, in accordance with the method set out in Annex IX to Regulation (EEC) No 2568/91, may have a K270 extinction coefficient higher than 0,10. If so, after neutralization and decolorization in the laboratory, in accordance with the method set ou in Annex XIII to the aforementioned Regulation, they must have the following characteristics:aK 270 extinction coefficient not higher than 1,20,an extinction coefficient variation (Delta K), in the 270 nm region, higher than 0,01 but not higher than 0,16, i.e.: K m the extinction coefficient at the wavelength of the peak of the absorption curve in the 270 nm region, K m - 4 en Km+4 the extinction coefficients at wavelengths 4 nm lower and higher than the K m wavelength;
(iv) organoleptic organoleptic characteristics which include detectable defects exceeding the limits of acceptability and a panel test score lower than 3,5 in accordance with Annex XII to Regulation (EEC) No 2568/91.
(a) an acid content, expressed as oleic acid, not exceeding 3,3 g per 100 g; (b) a peroxide number not exceeding 20 meq active 0 2 /kg;(c) awax content not exceeding 250 mg/kg; (d) a content in volatile halogenated solvents not exceeding 0,2 mg/kg overall and not exceeding 0,1 mg/kg for each solvent; (e) a K 270 extinction coefficient not higher than 0,250 and, after treatment of the oil with activated alumina, not higher than 0,10;(f) an extinction coefficient variation (Delta K), in the 270 nm region, not higher than 0,01; (g) organoleptic characteristics which may include detectable defects within the limits of acceptability and a panel test score higher than 3,5 in accordance with Annex XII to Regulation (EEC) No 2568/91; (h) an erythrodiol and uvaol content not exceeding 4,5 %; (i) a content in saturated fatty acids at the 2-position in the triglycerides not exceeding; (j) the sum of transoleic isomers lower than 0,03 % and the sum of translinoleic + translinolenic isomers lower than 0,03 %.
(a) an acid content, expressed as oleic acid, not exceeding 3,3 g per 100 g; (b) awax content not exceeding 350 mg/kg; (c) a K 270 extinction coefficient (100) not higher than 1,20;(d) an extinction coefficient variation (Δ K), in the 270 nm region, not higher than 0,16; (e) an erythrodiol and uvaol content not exceeding 4,5 %; (f) a content in saturated fatty acids at the 2-position in the triglycerides not exceeding 1,5 %; (g) the sum of transoleic isomeres lower than 0,20 % and the sum of translinoleic + translinolenic isomeres lower than 0,30 %.
(a) an acid content, expressed as oleic acid, greater than 2 g per 100 g; (b) an erythrodiol and uvaol content exceeding 12 %; (c) a content in saturated fatty acids at the 2-position in the triglycerides not exceeding 1,8 %; (d) the sum of transoleic isomers lower than 0,20 % and the sum of translinoleic + translinolenic isomers lower than 0,10 %.
(a) residues resulting from the treatment of fatty substances containing oil having in iodine index, determined in accordance with the metod laid down in Annex XVI to Regulation (EEC) No 2568/91, lower than 70 or higher than 100; (b) residues resulting from the treatment of fatty substances containing oil having an iodine index lower than 70 or higher than 100, of which the peadk area representing the retention volume of Beta-Sitosterol , determined in accordance with Annex V to Regulation (EEC) No 2568/91, is less than 93 % of the total sterol peak areas.Delta-5,23-Stigmastadienol + Chlerosterol + Beta-Sitosterol + Sitostanol + Delta-5-Avenasterol + Delta-5,24-Stigmastadienol.
suitable extraction apparatus fitted with a 200 to 250 ml round-bottomed flask, electrically heated bath (e.g., sand bath, water bath) or hotplate, analytical balance, oven regulated to a maximum of 80° C, electrically heated oven fitted with a thermostatic device regulated to 103 ± 2° C and one that can be swept with a stream of air or operated at reduced pressure, mechanical mill, easy to clean, and one that allows the olive residues to be ground without a rise in their temperature or any appreciable alteration in their content of moisture, volatile matter or substances extractable with hexane, extraction thimble and cotton wool or filter paper from which substances extractable with hexane have already been removed, dessicator, sieve with 1 mm diameter apertures, small particles of previously dried pumice stone.
(a) The extract expressed as a percentage by mass of the product as received is equal to: where: S = is the percentage by mass of extract of the product as received, m 0 = is the mass, in grams, of the test portion, m 1 = is the mass, in grams, of the extract after drying.
Take as the result the arithmetic mean of the duplicate determinations, providing the repeatability conditions are satisfied. Express the result to the first decimal place. (b) The extract is expressed on a dry matter basis by using the formula: where: S is the percentage of extract by means of the product as received (see (a)), U is its moisture and volatile matter content.
Expected iodine value | |
---|---|
less than 5 | |
5 to 20 | |
21 to 50 | |
51 to 100 | |
101 to 150 | |
151 to 200 |
injector temperature: 300 °C, detector temperature: 320 °C, integrator-recorder: the parameters for integration should be fixed so as to give a correct assessment of the areas. Valley-valley integration mode is recommended, sensitivity: about 16 times the minimum attenuation, amount of solution injected: 1μl, oven programming temperatures: initial 235 °C for six minutes and then rising at 2 °C/minute up to 285 °C, injector with 1: 15 flow divider, carrier: helium or hydrogen at about 120 kPa pressure.
where: |
(a) First fraction (30 ml) from a virgin oil, spiked with standard. (b) Second fraction (40 ml) from an olive oil containing 0,10 mg/kg of stigmastadienes. (c) Second fraction (40 ml) containing a small proportion of the first fraction.
Fatty acid (FA) | Abbreviation | ECN | |
---|---|---|---|
Palmitic acid | P | ||
Palmitoleic acid | Po | ||
Stearic acid | S | ||
Oleic acid | O | ||
Linoleic acid | L | ||
Linolenic acid | Ln |
LLL PoLL and the positional isomer LPoL OLLn and the positional isomers OLnL and LnOL PoPoL and the positional isomer PoLPo PoOLn and the positional isomers OPoLn and OLnPo PLLn and the positional isomers LLnP and LnPL PoPoPo SLnLn and the positional isomer LnSLn PPoLn and the positional isomers PLnPo and PoPLn
FA | P | S | Po | O | L | Ln |
---|---|---|---|---|---|---|
MW | ||||||
Area % |
FA in | 1,3-pos | 2-pos |
---|---|---|
P | ||
S | ||
Po | ||
O | ||
L | ||
Ln | ||
Sum |
LLL PoPoPo PoLL with 1 positional isomer SLnLn with 1 positional isomer PoPoL with 1 positional isomer PPoLn with 2 positional isomers OLLn with 2 positional isomers PLLn with 2 positional isomers PoOLn with 2 positional isomers
3.1. Round bottomed flask fitted with a reflux condenser with ground-glass joints, 250 mL. 3.2. Separating funnel, 500 mL. 3.3. Flasks, 250 mL. 3.4. Microsyringes, 100 μL and 500 μL. 3.5. Cylindrical filter funnel with a G3 porous septum (porosity 15-40 μm) of diameter approximately 2 cm and a depth of 5 cm, suitable for filtration under vacuum with male ground-glass joint. 3.6. Conical flask with ground-glass female joint, 50 mL, which can be fitted to the filter funnel (3.5). 3.7. Test tube with a tapering bottom and a sealing glass stopper, 10 mL. 3.8. Calcium dichloride desiccator.
4.1. Potassium hydroxide minimum titre 85 %. 4.2. Potassium hydroxide ethanolic solution, approximately 2 M. Dissolve 130 g of potassium hydroxide (4.1) with cooling in 200 ml of distilled water and then make up to one litre with ethanol (4.7). Keep the solution in well-stoppered dark glass bottles and stored maximum 2 days. 4.3. Ethyl ether, for analysis quality. 4.4. Anhydrous sodium sulphate, for analysis quality. 4.5. Acetone, for chromatography quality. 4.6. Ethyl ether, for chromatography quality. 4.7. Ethanol of analytical quality. 4.8. Ethyl acetate of analytical quality. 4.9. Internal standard, α-cholestanol, purity more than 99 % (purity must be checked by GC analysis). 4.10. Internal standard solution of α-cholestanol, 0,2 solution (m/V) in ethyl acetate (4.8). 4.11. Phenolphthalein solution, 10 g/L in ethanol (4.7). 4.12. A 0,1 % (m/v) solution of 1-eicosanol in ethyl acetate (internal standard).
3.1. Complete apparatus for analysis by thin-layer chromatography using 20 × 20 cm glass plates. 3.2. Ultraviolet lamp with a wavelength of 366 or 254 nm. 3.3. Microsyringes, 100 μL and 500 μL. 3.4. Cylindrical filter funnel with a G3 porous septum (porosity 15-40 μm) of diameter approximately 2 cm and a depth of 5 cm, suitable for filtration under vacuum with male ground-glass joint. 3.5. Conical flask with ground-glass female joint, 50 mL which can be fitted to the filter funnel (3.4). 3.6. Test tube with a tapering bottom and a sealing glass stopper, 10 mL. 3.7. Calcium dichloride desiccator. 3.8. HPLC system, consisting of: 3.8.1. Binary pump. 3.8.2. Manual or automatic injector equipped with 200 μL injection loop. 3.8.3. In-line degasser. 3.8.4. UV-VIS or IR detector.
3.9. HPLC column (25 cm × 4 mm i.d.) with silica gel 60 (5 μm particle size). 3.10. Syringe filter, 0,45 μm. 3.11. Conical flask 25 mL.
4.1. Potassium hydroxide minimum titre 85 %. 4.2. Potassium hydroxide ethanolic solution, approximately 2 M. Dissolve 130 g of potassium hydroxide (4.1) with cooling in 200 ml of distilled water and then make up to one litre with ethanol (4.9). Keep the solution in well-stoppered dark glass bottles and stored maximum 2 days. 4.3. Ethyl ether, for analysis quality. 4.4. Potassium hydroxide ethanolic solution, approximately 0,2 M. Dissolve 13 g of potassium hydroxide (4.1) in 20 ml of distilled water and make up to one litre with ethanol (4.9). 4.5. Glass 20x20 plates coated with silica gel, without fluorescence indicator, thickness 0,25 mm (commercially available ready for use). 4.6. Acetone, for chromatography quality. 4.7. n-Hexane, for chromatography quality. 4.8. Ethyl ether, for chromatography quality. 4.9. Ethanol of analytical quality. 4.10. Ethyl acetate of analytical quality. 4.11. Reference solution for thin-layer chromatography: cholesterol, phytosterols, alcohols and Erythrodiol 5 % solution in Ethyl acetate (4.10). 4.12. Solution of 2,7-dichlorofluorescein, 0,2 % in ethanolic solution. Make slightly basic by adding a few drops of 2 M alcoholic potassium hydroxide solution (4.2). 4.13. n-Hexane (4.7)/ethyl ether (4.8) mixture 65:35 (V/V). 4.14. HPLC mobile phase n-hexane (4.7)/ethyl ether (4.8) (1:1) (V/V).
3.1. Test tube with a tapering bottom and a sealing glass stopper, 10 mL. 3.2. Gas chromatograph suitable for use with a capillary column with split injection system, consisting of: 3.2.1. A thermostatic chamber for columns capable of maintaining the desired temperature with an accuracy of ± 1 °C; 3.2.2. A temperature-adjustable injection unit with a persilanised glass vaporising element and split system; 3.2.3. A flame ionisation detector (FID); 3.2.4. Data acquisition system suitable for use with the FID detector (3.10.3.), capable of manual integration.
3.3. Fused-silica capillary column of length 20 to 30 m, internal diameter 0,25 to 0,32 mm, coated with 5 % Diphenyl - 95 % Dimethylpolysiloxane (SE-52 or SE-54 stationary phase or equivalent), to a uniform thickness between 0,10 and 0,30 μm. 3.4. Microsyringe, of 10 μL capacity, for gas chromatography, with cemented needle suitable for split injection.
4.1. Anhydrous pyridine, for chromatography quality. 4.2. Hexamethyl disilazane of analytical quality. 4.3. Trimethylchlorosilane of analytical quality. 4.4. Sample solutions of sterol trimethylsilyl ethers. To be prepared at the time of use from sterols and erythrodiol obtained from oils containing them. 4.5. Standard solutions of trimethylsilyl ethers of aliphatic alcohols from C20 to C28. They may be prepared from mixtures of pure alcohols at the time they are required for use. 4.6. Carrier gas: hydrogen or helium, gas-chromatographic purity. 4.7. Auxiliary gases: hydrogen, helium, nitrogen and air, of gas-chromatographic purity. 4.8. Silylation reagent, consisting of a 9:3:1 (V/V/V) mixture of pyridine/hexamethyl disilazane/trimethylchlorosilane. 4.9. n-Hexane, for chromatography quality.
Oven Program | 180 °C (8 min.) → 260 °C (at 5 °C/min) → 260 °C (15 min) |
---|---|
Injector Temperature | 280 °C |
Detector Temperature | 290 °C |
Linear Velocity of Carrier gas | Helium (20 to 30 cm/s); Hydrogen (30 to 50 cm/s) |
Split Ratio | 1:50 to 1:100 |
Volume Injected | 0,5 to 1 μL of TMSE solution |
Oven Program | 260 ± 5 °C Isothermal |
---|---|
Injector Temperature | 280 – 300 °C |
Detector Temperature | 280 – 300 °C |
Linear Velocity of Carrier gas | Helium (20 to 30 cm/s); Hydrogen (30 to 50 cm/s) |
Split Ratio | 1:50 to 1:100 |
Volume Injected | 0,5 to 1 μL of TMSE solution |
Alcohol C26 retention time shall be 18 ± 5 minutes. Alcohol C22 peak shall be 80 ± 20 % of the full-scale value for olive oil and 40 ± 20 % of the full-scale value for olive-pomace oil. The retention time for the β-sitosterol peak should be at 20 ± 5 min. The campesterol peak should be: for olive oil (mean content 3 %) 20 ± 5 % of full scale. All the present sterols must be separated. In addition to being separated, the peaks must also be completely resolved, i.e. the peak trace should return to the base line before leaving for the next peak. Incomplete resolution is, however, tolerated, provided that the peak at RRT 1,02 (Sitostanol) can be quantified using the perpendicular.
Hydrogen, pure, gas chromatography grade. Air, pure, gas chromatography grade.
4.3.1. Degasser for the mobile phase. 4.3.2. Rheodyne injector valve with a 10 μL loop. 4.3.3. High pressure pump unit. 4.3.4. Thermostatic oven for the HPLC column capable of maintaining sub-ambient temperatures (15-20 °C), (for example, Peltier type). 4.3.5. Refractive index detector. 4.3.6. Computerised data acquisition system provided with an integration program.
4.4.1. Split injector. 4.4.2. Flame ionisation detector (FID). 4.4.3. Oven with programmable temperature. 4.4.4. Computerised data acquisition system provided with an integration program.
Palmitic; | P (C16:0) | = | methyl ester + ethyl ester |
Stearic; | S (C18:0) | = | methyl ester |
Palmitoleic; | Po (C16:1) | = | sum of methyl esters of the two |
Oleic; | O (C18:1) | = | sum of methyl esters of the two |
Linoleic; | L (C18:2) | = | methyl ester+ ethyl ester + |
Linolenic; | Ln (C18:3) | = | methyl ester + |
Arachidic; | A (C20:0) | = | methyl ester |
Eicosenoic (gondoic); | G (C20:1) | = | methyl ester |
ECN | HPLC peaks | TAGs | Sample 1 | Sample 2 | Sample 3 | Sample 4 | Sample 5 | |||||
---|---|---|---|---|---|---|---|---|---|---|---|---|
Mean (%) | RSD | Mean (%) | RSD | Mean (%) | RSD | Mean (%) | RSD | Mean (%) | RSD | |||
LLL | ||||||||||||
OLLn+ PoLL | ||||||||||||
PLLn | ||||||||||||
OLL | ||||||||||||
OOLn+ PoOL | ||||||||||||
PLL+ PoPoO | ||||||||||||
POLn+ PpoPo+ PpoL | ||||||||||||
OOL+ LnPP | ||||||||||||
PoOO | ||||||||||||
SLL+ PLO | ||||||||||||
PoOP+ SpoL+ SOLn+ SpoPo | ||||||||||||
OOO+ PLP+ PoPP | ||||||||||||
SOL | ||||||||||||
POO | ||||||||||||
POP | ||||||||||||
SOO | ||||||||||||
POS+ SLS |
Labelling | Chemical parameters | Organoleptic characteristics | Final conclusion | ||||||||||||||
---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
Sample | Category | Country of origin | Place of inspection | Legal name | Designation of origin | Storage conditions | Erroneous information | Legibility | C/NC | If so, please indicate which one(s) | C/NC | Median defect | Fruity Median | C/NC | Required action | Sanction | |
(a) for the determination of the free fatty acids, expressed as the percentage of oleic acid, the method set out in Annex II; (b) for the determination of the peroxide index, the method set out in Annex III; (c) for determination of the wax content, the method set out in Annex IV; (d) for the determination of the composition and content of sterols and triterpene dialcohols by capillary-column gas chromatography, the method set out in Annex V; (e) for the determination of the percentage of 2- glyceryl monopalmitate, the method set out in Annex VII; (f) for spectrophotometric analysis, the method set out in Annex IX; (g) for the determination of the fatty acid composition, the method set out in Annex X; (h) for the determination of the volatile halogenated solvents, the method set out in Annex XI; (i) for the evaluation of the organoleptic characteristics of virgin olive oil, the method set out in Annex XII; (j) for the determination of stigmastadienes, the method set out in Annex XVII; (k) for determining the content of triglycerides with ECN42, the method set out in Annex XVIII; (l) for the determination of the composition and content of sterols and for the determination of alcoholic compounds, by capillary column gas chromatography, the method set out in Annex XIX; (m) for the determination of the content of waxes, fatty acid methyl esters and fatty acid ethyl esters, the method set out in Annex XX.
(a) the category of oil, the period of production, the price of oils in relation to other vegetable oils, the blending and packing operations, the storage facilities and conditions, the country of origin, the country of destination, the means of transport or the volume of the lot; (b) the position of the operators in the marketing chain, the volume and/or value marketed by them, the range of oil categories they market, the type of business carried out such as milling, storage, refining, blending, packaging or retail sale; (c) findings made during previous checks including the number and type of defects found, the usual quality of oils marketed, the performance of technical equipment used; (d) the reliability of operators’ quality assurance systems or self-checking systems related to the conformity to marketing standards; (e) the place where the check is carried out, in particular if it is the first point of entry into the Union, the last point of exit from the Union or the place where the oils are produced, packaged, loaded or sold to the final consumer; (f) any other information that might indicate a risk of non-compliance.
(a) the criteria for assessing the risk of non-conformity of lots; (b) on the basis of a risk analysis for each risk category, the minimum number of operators or lots and/or quantities which will be subject to a conformity check.
(a) carrying out, in any order, the analyses set out in Annex I; or (b) following the order set out in Annex Ib on the flowchart, until one of the decisions appearing in the flowchart is reached.
the requirements of Annex XII.4 are met, the panel head is given training recognised for this purpose by the Member State, continued approval depends on performance in annual checks arranged by the Member State.
maximum content of each halogenated solvent detected: 0,1 mg/kg, maximum total content of halogenated solvents detected: 0,2 mg/kg.
Category | K | K | Delta-K | Organoleptic evaluation | ||||
---|---|---|---|---|---|---|---|---|
Median of defect (Md) (*) | Fruity median (Mf) | |||||||
≤ 0,80 | ≤ 20,0 | ≤ 2,50 | ≤ 0,22 | ≤ 0,01 | Md = 0,0 | Mf > 0,0 | ≤ 35 | |
≤ 2,0 | ≤ 20,0 | ≤ 2,60 | ≤ 0,25 | ≤ 0,01 | Md ≤ 3,5 | Mf > 0,0 | — | |
> 2,0 | — | — | — | — | Md > 3,5 | — | — | |
≤ 0,30 | ≤ 5,0 | — | ≤ 1,25 | ≤ 0,16 | — | — | ||
≤ 1,00 | ≤ 15,0 | — | ≤ 1,15 | ≤ 0,15 | — | — | ||
— | — | — | — | — | — | — | ||
≤ 0,30 | ≤ 5,0 | — | ≤ 2,00 | ≤ 0,20 | — | — | ||
≤ 1,00 | ≤ 15,0 | — | ≤ 1,70 | ≤ 0,18 | — | — |
Category | Fatty acid composition | ||||||||||
---|---|---|---|---|---|---|---|---|---|---|---|
≤ 0,03 | ≤ 1,00 | ≤ 0,60 | ≤ 0,50 | ≤ 0,20 | ≤ 0,20 | ≤ 0,05 | ≤ 0,05 | ≤ 0,05 | ≤ |0,20| | ≤ 0,9 if total palmitic acid % ≤ 14,00 % | |
≤ 1,0 if total palmitic acid % > 14,00 % | |||||||||||
≤ 0,03 | ≤ 1,00 | ≤ 0,60 | ≤ 0,50 | ≤ 0,20 | ≤ 0,20 | ≤ 0,05 | ≤ 0,05 | ≤ 0,05 | ≤ |0,20| | ≤ 0,9 if total palmitic acid % ≤ 14,00 % | |
≤ 1,0 if total palmitic acid % > 14,00 % | |||||||||||
≤ 0,03 | ≤ 1,00 | ≤ 0,60 | ≤ 0,50 | ≤ 0,20 | ≤ 0,20 | ≤ 0,10 | ≤ 0,10 | ≤ 0,50 | ≤ |0,30| | ≤ 0,9 if total palmitic acid % ≤ 14,00 % | |
≤ 1,1 if total palmitic acid % > 14,00 % | |||||||||||
≤ 0,03 | ≤ 1,00 | ≤ 0,60 | ≤ 0,50 | ≤ 0,20 | ≤ 0,20 | ≤ 0,20 | ≤ 0,30 | — | ≤|0,30| | ≤ 0,9 if total palmitic acid % ≤ 14,00 % | |
≤ 1,1 if total palmitic acid % > 14,00 % | |||||||||||
≤ 0,03 | ≤ 1,00 | ≤ 0,60 | ≤ 0,50 | ≤ 0,20 | ≤ 0,20 | ≤ 0,20 | ≤ 0,30 | — | ≤ |0,30| | ≤ 0,9 if total palmitic acid % ≤ 14,00 % | |
≤ 1,0 if total palmitic acid % > 14,00 % | |||||||||||
≤ 0,03 | ≤ 1,00 | ≤ 0,60 | ≤ 0,50 | ≤ 0,30 | ≤ 0,20 | ≤ 0,20 | ≤ 0,10 | — | ≤ |0,60| | ≤ 1,4 | |
≤ 0,03 | ≤ 1,00 | ≤ 0,60 | ≤ 0,50 | ≤ 0,30 | ≤ 0,20 | ≤ 0,40 | ≤ 0,35 | — | ≤ |0,50| | ≤ 1,4 | |
≤ 0,03 | ≤ 1,00 | ≤ 0,60 | ≤ 0,50 | ≤ 0,30 | ≤ 0,20 | ≤ 0,40 | ≤ 0,35 | — | ≤ |0,50| | ≤ 1,2 |
Category | Sterols composition | ||||||||
---|---|---|---|---|---|---|---|---|---|
≤ 0,5 | ≤ 0,1 | ≤ 4,0 | < Camp. | ≥ 93,0 | ≤ 0,5 | ≥ | ≤ 4,5 | C | |
≤ 0,5 | ≤ 0,1 | ≤ 4,0 | < Camp. | ≥ 93,0 | ≤ 0,5 | ≥ | ≤ 4,5 | C | |
≤ 0,5 | ≤ 0,1 | ≤ 4,0 | — | ≥ 93,0 | ≤ 0,5 | ≥ | ≤ 4,5 | C | |
≤ 0,5 | ≤ 0,1 | ≤ 4,0 | < Camp. | ≥ 93,0 | ≤ 0,5 | ≥ | ≤ 4,5 | C | |
≤ 0,5 | ≤ 0,1 | ≤ 4,0 | < Camp. | ≥ 93,0 | ≤ 0,5 | ≥ | ≤ 4,5 | C | |
≤ 0,5 | ≤ 0,2 | ≤ 4,0 | — | ≥ 93,0 | ≤ 0,5 | ≥ | > 4,5 | C | |
≤ 0,5 | ≤ 0,2 | ≤ 4,0 | < Camp. | ≥ 93,0 | ≤ 0,5 | ≥ | > 4,5 | C | |
≤ 0,5 | ≤ 0,2 | ≤ 4,0 | < Camp. | ≥ 93,0 | ≤ 0,5 | ≥ | > 4,5 | C |
Where the immediate packaging has a capacity of | The primary sample must comprise the oil from |
---|---|
Number of packages in the lot | Minimum number of increments to be selected |
---|---|
Up to 10 | |
From … 11 to 150 | |
From … 151 to 500 | |
From … 501 to | |
From … | |
> | 1 extra increment |
Size of batch (litres) | Number of primary samples |
---|---|
Less than | |
From | |
From | |
From | |
Equal to and more than | 6 + 1 each |
4.1 Analytical balance; 4.2 250 ml conical flask; 4.3 10 ml burette class A, graduated in 0,05 ml, or equivalent automatic burette.
Mass of sample (g) | Weighing accuracy (g) | |
---|---|---|
0 to 2 | 10 | 0,02 |
> 2 to 7,5 | 2,5 | 0,01 |
> 7,5 | 0,5 | 0,001 |
(a) to two decimal places for values from 0 up to and including 1; (b) to one decimal place for values from 1 up to and including 100.
m KIO3 is the mass of potassium iodate, in gramsV 1 is the volume of the potassium iodate solution, in millilitres (5 ml or 10 ml)V 2 is the total volume of potassium iodate solution, in millilitres (250 ml or 500 ml)V 3 is the volume of the sodium thiosulfate solution, in millilitresw KIO3 is the purity of potassium iodate in g/100 gM KIO3 is the molecular mass of potassium iodate (214 g/mol)T is the exact molarity of the sodium thiosulphate solution (mol/l).
0 to 12 | 5,0 to 2,0 |
12 to 20 | 2,0 to 1,2 |
20 to 30 | 1,2 to 0,8 |
30 to 50 | 0,8 to 0,5 |
50 to 90 | 0,5 to 0,3 |
pure hydrogen for gas chromatography, pure air for gas chromatography.
The n-hexane/ethyl ether mixture (99:1) must be prepared every day. For a visual check on the correct elution of the waxes 100 μl of 1 % Sudan in the elution mixture can be added to the sample in solution. Since the colourant has an intermediate retention, between waxes and triglycerides, when the coloration has reached the bottom of the column the elution should be suspended because all the waxes will have been eluted.
column temperature: 20 °C/minute 5 °C/minute 20 °C/minute Initially 80 °C (1′) → 240 °C→ 325 °C(6′) → 340 °C(10′) detector temperature: 350 °C; quantity of substance injected: 1 μl of the n-heptane solution (2-4 ml); carrier gas: helium or hydrogen at the correct linear velocity for the gas selected (see Appendix); instrument sensitivity: suitable for the following conditions:
3.1. 250 ml flask fitted with a reflux condenser with ground-glass joints. 3.2. 500 ml separating funnel. 3.3. 250 ml flasks. 3.4. Complete apparatus for analysis by thin-layer chromatography using 20 x 20 cm glass plates. 3.5. Ultraviolet lamp with a wavelength of 254 or 366 nm. 3.6. 100 μl and 500 μl microsyringes. 3.7. Cylindrical filter funnel with a G3 porous septum (porosity 15-40 μm) of diameter approximately 2 cm and a depth of 5 cm, suitable for filtration under vacuum with male ground-glass joint. 3.8. 50 ml vacuum conical flask with ground-glass female joint, which can be fitted to the filter funnel (point 3.7). 3.9. 10 ml test tube with a tapering bottom and a sealing glass stopper. 3.10. Gas chromatograph suitable for use with a capillary column with split injection system, consisting of: 3.10.1. A thermostatic chamber for columns capable of maintaining the desired temperature with an accuracy of ± 1°C; 3.10.2. A temperature-adjustable injection unit with a persilanised glass vaporising element and split system; 3.10.3. A flame ionisation detector (FID); 3.10.4. Data acquisition system suitable for use with the FID detector (point 3.10.3.), capable of manual integration.
3.11. Fused-silica capillary column of length 20 to 30 m, internal diameter 0,25 to 0,32 mm, coated with 5 % diphenyl - 95 % dimethylpolysiloxane (SE-52 or SE-54 stationary phase or equivalent), to a uniform thickness between 0,10 and 0,30 μm. 3.12. Microsyringe, of 10 ml capacity, for gas chromatography, with cemented needle suitable for split injection. 3.13. Calcium dichloride desiccator
Column temperature: 260 ± 5 °C; Injector temperature: 280-300 °C; Detector temperature: 280-300 °C; Linear velocity of the carrier gas: helium 20 to 35 cm/s; hydrogen 30 to 50 cm/s; Splitting ratio: from 1:50 to 1:100; Instrument sensitivity: from 4 to 16 times the minimum attenuation; Recording sensitivity: 1 to 2 mV full scale; Amount of substance injected: 0,5 to 1 μl of TMSE solution.
The retention time for the ß-sitosterol peak should be at 20 ± 5 min; The campesterol peak should be: for olive oil (mean content 3 %) 20 ± 5 % of full scale; for soybean oil (average content 20 %) 80 ± 10 % of full scale; All the present sterols must be separated. In addition to being separated the peaks, they must also be completely resolved, i.e. the peak trace should return to the base line before leaving for the next peak. Incomplete resolution is, however, tolerated, provided that the peak at RRT 1,02 (Sitostanol) can be quantified using the perpendicular.
Injector temperature (on-column injector) lower than solvent boiling point (68 °C); Detector temperature: 350 °C; Column temperature: programming of furnace temperature: 60 °C for 1 minute, increasing by 15 °C per minute up to 180 °C, then by 5 °C per minute up to 340 °C, then 340 °C for 13 minutes; Carrier gas: hydrogen or helium, set at a linear velocity sufficient to obtain the resolution reflected in Figure 1. The retention time of the C 54 triglyceride must be 40 ± 5 minutes (see Figure 2). (The operating conditions indicated above are indicative. Operators will have to optimise them to obtain the desired resolution. The peak corresponding to 2-glyceryl monopalmitate must have a minimum height equal to 10 % of the recorder scale.)Quantity of substance injected: 0,5-1 μl of the n-hexane solution (5 ml) (5.3.3).
reference to this method, all the information needed for a full identification of the sample, the analysis result, any deviation from the method, whether as the result of a decision by the parties concerned or for another reason, details to identify the laboratory, the date of the analysis and the signatures of those responsible for the analysis.
Category of oil | Method |
---|---|
Virgin olive oil with acidity ≤ 2,0 % |
|
Refined olive oil | |
Olive oil composed of refined olive oil and virgin olive oils | |
Refined olive pomace oil | |
Olive pomace oil | |
|
Injector temperature: | 250 °C |
Detector temperature: | 250 °C |
Oven temperature: | 165 °C (8 min) to 210 °C at 2 °C/min |
Carrier gas hydrogen: | column head pressure, 179 kPa |
Total flow: | 154,0 ml/min; |
Split ratio: | 1:100 |
Injection volume: | 1 μl |
d r(I) is the retention distance of peak I;d r(II) is the retention distance of peak II;t r(I) is the retention time of peak I;t r(II) is the retention time of peak II;ω (I) is the width of the base of peak I;ω (II) is the width of the base of peak II;ω 0,5 is the peak width of the specified compound, at mid-height of the peak;
A i is the area under the peak of the individual fatty acid methyl esteri ;ΣA is the sum of the areas under all the peaks of all the individual fatty acid methyl esters.
m is the mass of the FAMEi i in the reference mixture;Σm is the total of the masses of the various components as FAMEs of the reference mixture.
A i is the area of the FAMEi in the reference mixture;ΣA is the sum of all the areas of all the FAMEs of the reference mixture.
A is the area the FAMEi i ;A is the area of the internal standard;IS F is the correction factor of the fatty acidi i , expressed as FAME;F is the correction factor of the internal standard;IS m is the mass of the test portion, in milligrams m is the mass of the internal standard, in milligrams.IS
injector temperature: 150 °C, column temperature: 70 to 80 °C, detector temperature: 200 to 250 °C.
Fusty/muddy sediment : Characteristic flavour of oil obtained from olives piled or stored in such conditions as to have undergone an advanced stage of anaerobic fermentation, or of oil which has been left in contact with the sediment that settles in underground tanks and vats and which has also undergone a process of anaerobic fermentation.Musty-humid-earthy : Characteristic flavour of oils obtained from fruit in which large numbers of fungi and yeasts have developed as a result of its being stored in humid conditions for several days or of oil obtained from olives that have been collected with earth or mud on them and which have not been washed.Winey-vinegary-acid-sour : Characteristic flavour of certain oils reminiscent of wine or vinegar. This flavour is mainly due to a process of aerobic fermentation in the olives or in olive paste left on pressing mats which have not been properly cleaned and leads to the formation of acetic acid, ethyl acetate and ethanol.Rancid : Flavour of oils which have undergone an intense process of oxidation.Frostbitten olives (wet wood) : Characteristic flavour of oils extracted from olives which have been injured by frost while on the tree.
Characteristic flavour of oils caused by excessive and/or prolonged heating during processing, particularly when the paste is thermally mixed, if this is done under unsuitable thermal conditions. | |
Characteristic flavour of certain oils produced from olives that have dried out. | |
Thick, pasty mouthfeel sensation produced by certain old oils. | |
Flavour of oil reminiscent of that of diesel oil, grease or mineral oil. | |
Flavour acquired by the oil as a result of prolonged contact with vegetable water which has undergone fermentation processes. | |
Flavour of oil extracted from olives which have been preserved in brine. | |
Flavour that is reminiscent of metals. It is characteristic of oil which has been in prolonged contact with metallic surfaces during crushing, mixing, pressing or storage. | |
Characteristic flavour of oil obtained from olives pressed in new esparto mats. The flavour may differ depending on whether the mats are made of green esparto or dried esparto. | |
Flavour of oil obtained from olives which have been heavily attacked by the grubs of the olive fly ( | |
Flavour produced when an oil is hermetically packed for too long, particularly in tin containers, and which is attributed to the formation of 2,6 nonadienal. |
Set of olfactory sensations characteristic of the oil which depends on the variety and comes from sound, fresh olives, either ripe or unripe. It is perceived directly and/or through the back of the nose. | |
Characteristic primary taste of oil obtained from green olives or olives turning colour. It is perceived in the circumvallate papillae on the "V" region of the tongue. | |
Biting tactile sensation characteristic of oils produced at the start of the crop year, primarily from olives that are still unripe. It can be perceived throughout the whole of the mouth cavity, particularly in the throat. |
Robust , when the median of the attribute is more than 6,0;Medium , when the median of the attribute is more than 3,0 and less or equal to 6,0;Delicate , when the median of the attribute is less or equal to 3,0.
Set of olfactory sensations characteristic of the oil which depends on the variety of olive and comes from sound, fresh olives in which neither green nor ripe fruitiness predominates. It is perceived directly and/or through the back of the nose. | |
Set of olfactory sensations characteristic of the oil which is reminiscent of green fruit, depends on the variety of olive and comes from green, sound, fresh olives. It is perceived directly and/or through the back of the nose. | |
Set of olfactory sensations characteristic of the oil which is reminiscent of ripe fruit, depends on the variety of olive and comes from sound, fresh olives. It is perceived directly and/or through the back of the nose. | |
Oil which does not display a lack of balance, by which is meant the olfactory-gustatory and tactile sensation where the median of the bitter attribute and the median of the pungent attribute are not more than 2,0 points above the median of the fruitiness. | |
Oil for which the median of the bitter and pungent attributes is 2,0 or less. |
Terms subject to production of an organoleptic test certificate | Median of the attribute |
---|---|
Fruitiness | — |
Ripe fruitiness | — |
Green fruitiness | — |
Delicate fruitiness | ≤ 3,0 |
Medium fruitiness | 3,0 < Me ≤ 6,0 |
Robust fruitiness | > 6,0 |
Delicate ripe fruitiness | ≤ 3,0 |
Medium ripe fruitiness | 3,0 < Me ≤ 6,0 |
Robust ripe fruitiness | > 6,0 |
Delicate green fruitiness | ≤ 3,0 |
Medium green fruitiness | 3,0 < Me ≤ 6,0 |
Robust green fruitiness | > 6,0 |
Delicate bitterness | ≤ 3,0 |
Medium bitterness | 3,0 < Me ≤ 6,0 |
Robust bitterness | > 6,0 |
Delicate pungency | ≤ 3,0 |
Medium pungency | 3,0 < Me ≤ 6,0 |
Robust pungency | > 6,0 |
Well balanced oil | The median of the bitter attribute and the median of the pungent attribute are not more than 2,0 points above the median of the fruitiness. |
Mild oil | The median of the bitter attribute and the median of the pungent attribute are 2,0 or less. |
glasses (standardised) containing the samples, code numbered, covered with a watch-glass and kept at 28 °C ± 2 °C; profile sheet (see Figure 1) on hard copy, or on soft copy provided that the conditions of the profile sheet are met, together with the instructions for its use if necessary pen or indelible ink trays with slices of apple and/or water, carbonated water and/or rusks glass of water at ambient temperature sheet recalling the general rules listed in sections 8.4 and 9.1.1 spittoons.
They shall not smoke or drink coffee at least 30 minutes before the time set for the test. They must not have used any fragrance, cosmetic or soap whose smell could linger until the time of the test. They must use an unperfumed soap to wash their hands which they shall then rinse and dry as often as necessary to eliminate any smell. They shall fast at least one hour before the tasting is carried out. Should they feel physically unwell, and in particular if their sense of smell or taste is affected, or if they are under any psychological effect that prevents them from concentrating on their work, the tasters shall refrain from tasting and shall inform the panel leader accordingly. When they have complied with the above, the tasters shall take up their place in the booth allotted to them in an orderly, quiet manner. They shall carefully read the instructions given on the profile sheet and shall not begin to examine the sample until fully prepared for the task they have to perform (relaxed and unhurried). If any doubts should arise, they should consult the panel leader in private. They must remain silent while performing their tasks. They must keep their mobile phone switched off at all times to avoid interfering with the concentration and work of their colleagues.
(a) Extra virgin olive oil: the median of the defects is 0,0 and the median of the fruity attribute is above 0,0; (b) Virgin olive oil: the median of the defects is above 0,0 but not more than 3,5 and the median of the fruity attribute is above 0,0; (c) Lampante virgin olive oil: the median of the defects is above 3,5 or the median of the defects is less than or equal to 3,5 and the fruity median is equal to 0,0.
Fusty/muddy sediment | ||||
Musty/humid/earthy | ||||
Rancid | ||||
Other negative attributes: | ||||
Descriptor: | ||||
Fruity | ||||
Green□ | Ripe□ | |||
Bitter | ||||
Pungent | ||||
Name of taster: | Taster code: | |||
Sample code: | Signature: | |||
Date: | ||||
Comments: |
beaker, 300 ml, tall, laboratory centrifuge with 100 ml tubes, beaker, 250 ml, round-bottomed flasks, 100 ml, separating funnel, 1 litre.
aqueous solution of 12 % sodium hydroxide, ethyl alcohol solution of 1 % phenolphtalein, pure hexane, AR, pure propan-2-ol of AR.
round-bottomed flask, 250 ml, with three ground glass necks for the insertion of: (a) a thermometer graduated in degrees and allowing readings to be taken at 90° C; (b) a mechanical stirrer operating at 250 to 300 revolutions per minute, equipped to operate in a vacuum; (c) a vacuum pump connection,
vacuum pump, with a manometer, capable of giving residual pressure of 15 to 30 millibars.
Tabble I: Fatty acid composition as percentage of total fatty acids | Table II: Sterol composition as percentage of total sterols | ||
---|---|---|---|
Myristic acid | M 0,1 | Cholesterol | M 0,5 |
Linolenic acid | M 0,9 | Brassicasterol | M 0,2 |
Arachidic | M 0,7 | Campesterol | M 4,0 |
Eicosanoic acid | M 0,5 | Stigmasterol | < Campesterol |
Behenic acid | M 0,3 | Betasitosterol | m 93,0 |
Lignoceric acid | M 0,5 | Delta-7-stigmastzerol | M 0,5 |
(a) awax content not exceeding 350 mg/kg; (b) an erythrodical and uvaol content not exceeding 4,5 %; (c) a content in saturated fatty acids at the 2-position in the triglycerides not exceeding 1,3 % and/or (d) the sum of transoleic isomers lower than 0,10 % and the sum of translinoleic + translinolenic isomers lower than 0,10 %; (e) one or more of the following characteristics: (i) a periode number exceeding 20 meq 0 2 /kg;(ii) a content in volatile halogenated solvents exceeding 0,1 mg/kg for any one solvent; (iii) a K 270 (100) extinction coefficient higher than 0,250 and, after treatment of the oil with activated alumina, not higher than 0,11. In point of fact some oils having a free fatty acid content, expressed as oleic acid, of more than 3,3 g per 100 g may, after passage through activated alumina, in accordance with the method set out in Annex IX to Regulation (EEC) No 2568/91, may have a K270 extinction coefficient higher than 0,10. If so, after neutralization and decolorization in the laboratory, in accordance with the method set ou in Annex XIII to the aforementioned Regulation, they must have the following characteristics:aK 270 extinction coefficient not higher than 1,20,an extinction coefficient variation (Delta K), in the 270 nm region, higher than 0,01 but not higher than 0,16, i.e.: K m the extinction coefficient at the wavelength of the peak of the absorption curve in the 270 nm region, K m - 4 en Km+4 the extinction coefficients at wavelengths 4 nm lower and higher than the K m wavelength;
(iv) organoleptic organoleptic characteristics which include detectable defects exceeding the limits of acceptability and a panel test score lower than 3,5 in accordance with Annex XII to Regulation (EEC) No 2568/91.
(a) an acid content, expressed as oleic acid, not exceeding 3,3 g per 100 g; (b) a peroxide number not exceeding 20 meq active 0 2 /kg;(c) awax content not exceeding 250 mg/kg; (d) a content in volatile halogenated solvents not exceeding 0,2 mg/kg overall and not exceeding 0,1 mg/kg for each solvent; (e) a K 270 extinction coefficient not higher than 0,250 and, after treatment of the oil with activated alumina, not higher than 0,10;(f) an extinction coefficient variation (Delta K), in the 270 nm region, not higher than 0,01; (g) organoleptic characteristics which may include detectable defects within the limits of acceptability and a panel test score higher than 3,5 in accordance with Annex XII to Regulation (EEC) No 2568/91; (h) an erythrodiol and uvaol content not exceeding 4,5 %; (i) a content in saturated fatty acids at the 2-position in the triglycerides not exceeding; (j) the sum of transoleic isomers lower than 0,03 % and the sum of translinoleic + translinolenic isomers lower than 0,03 %.
(a) an acid content, expressed as oleic acid, not exceeding 3,3 g per 100 g; (b) awax content not exceeding 350 mg/kg; (c) a K 270 extinction coefficient (100) not higher than 1,20;(d) an extinction coefficient variation (Δ K), in the 270 nm region, not higher than 0,16; (e) an erythrodiol and uvaol content not exceeding 4,5 %; (f) a content in saturated fatty acids at the 2-position in the triglycerides not exceeding 1,5 %; (g) the sum of transoleic isomeres lower than 0,20 % and the sum of translinoleic + translinolenic isomeres lower than 0,30 %.
(a) an acid content, expressed as oleic acid, greater than 2 g per 100 g; (b) an erythrodiol and uvaol content exceeding 12 %; (c) a content in saturated fatty acids at the 2-position in the triglycerides not exceeding 1,8 %; (d) the sum of transoleic isomers lower than 0,20 % and the sum of translinoleic + translinolenic isomers lower than 0,10 %.
(a) residues resulting from the treatment of fatty substances containing oil having in iodine index, determined in accordance with the metod laid down in Annex XVI to Regulation (EEC) No 2568/91, lower than 70 or higher than 100; (b) residues resulting from the treatment of fatty substances containing oil having an iodine index lower than 70 or higher than 100, of which the peadk area representing the retention volume of Beta-Sitosterol , determined in accordance with Annex V to Regulation (EEC) No 2568/91, is less than 93 % of the total sterol peak areas.Delta-5,23-Stigmastadienol + Chlerosterol + Beta-Sitosterol + Sitostanol + Delta-5-Avenasterol + Delta-5,24-Stigmastadienol.
suitable extraction apparatus fitted with a 200 to 250 ml round-bottomed flask, electrically heated bath (e.g., sand bath, water bath) or hotplate, analytical balance, oven regulated to a maximum of 80° C, electrically heated oven fitted with a thermostatic device regulated to 103 ± 2° C and one that can be swept with a stream of air or operated at reduced pressure, mechanical mill, easy to clean, and one that allows the olive residues to be ground without a rise in their temperature or any appreciable alteration in their content of moisture, volatile matter or substances extractable with hexane, extraction thimble and cotton wool or filter paper from which substances extractable with hexane have already been removed, dessicator, sieve with 1 mm diameter apertures, small particles of previously dried pumice stone.
(a) The extract expressed as a percentage by mass of the product as received is equal to: where: S = is the percentage by mass of extract of the product as received, m 0 = is the mass, in grams, of the test portion, m 1 = is the mass, in grams, of the extract after drying.
Take as the result the arithmetic mean of the duplicate determinations, providing the repeatability conditions are satisfied. Express the result to the first decimal place. (b) The extract is expressed on a dry matter basis by using the formula: where: S is the percentage of extract by means of the product as received (see (a)), U is its moisture and volatile matter content.
Expected iodine value | |
---|---|
less than 5 | |
5 to 20 | |
21 to 50 | |
51 to 100 | |
101 to 150 | |
151 to 200 |
injector temperature: 300 °C, detector temperature: 320 °C, integrator-recorder: the parameters for integration should be fixed so as to give a correct assessment of the areas. Valley-valley integration mode is recommended, sensitivity: about 16 times the minimum attenuation, amount of solution injected: 1μl, oven programming temperatures: initial 235 °C for six minutes and then rising at 2 °C/minute up to 285 °C, injector with 1: 15 flow divider, carrier: helium or hydrogen at about 120 kPa pressure.
where: |
(a) First fraction (30 ml) from a virgin oil, spiked with standard. (b) Second fraction (40 ml) from an olive oil containing 0,10 mg/kg of stigmastadienes. (c) Second fraction (40 ml) containing a small proportion of the first fraction.
Fatty acid (FA) | Abbreviation | ECN | |
---|---|---|---|
Palmitic acid | P | ||
Palmitoleic acid | Po | ||
Stearic acid | S | ||
Oleic acid | O | ||
Linoleic acid | L | ||
Linolenic acid | Ln |
LLL PoLL and the positional isomer LPoL OLLn and the positional isomers OLnL and LnOL PoPoL and the positional isomer PoLPo PoOLn and the positional isomers OPoLn and OLnPo PLLn and the positional isomers LLnP and LnPL PoPoPo SLnLn and the positional isomer LnSLn PPoLn and the positional isomers PLnPo and PoPLn
FA | P | S | Po | O | L | Ln |
---|---|---|---|---|---|---|
MW | ||||||
Area % |
FA in | 1,3-pos | 2-pos |
---|---|---|
P | ||
S | ||
Po | ||
O | ||
L | ||
Ln | ||
Sum |
LLL PoPoPo PoLL with 1 positional isomer SLnLn with 1 positional isomer PoPoL with 1 positional isomer PPoLn with 2 positional isomers OLLn with 2 positional isomers PLLn with 2 positional isomers PoOLn with 2 positional isomers
3.1. Round bottomed flask fitted with a reflux condenser with ground-glass joints, 250 mL. 3.2. Separating funnel, 500 mL. 3.3. Flasks, 250 mL. 3.4. Microsyringes, 100 μL and 500 μL. 3.5. Cylindrical filter funnel with a G3 porous septum (porosity 15-40 μm) of diameter approximately 2 cm and a depth of 5 cm, suitable for filtration under vacuum with male ground-glass joint. 3.6. Conical flask with ground-glass female joint, 50 mL, which can be fitted to the filter funnel (3.5). 3.7. Test tube with a tapering bottom and a sealing glass stopper, 10 mL. 3.8. Calcium dichloride desiccator.
4.1. Potassium hydroxide minimum titre 85 %. 4.2. Potassium hydroxide ethanolic solution, approximately 2 M. Dissolve 130 g of potassium hydroxide (4.1) with cooling in 200 ml of distilled water and then make up to one litre with ethanol (4.7). Keep the solution in well-stoppered dark glass bottles and stored maximum 2 days. 4.3. Ethyl ether, for analysis quality. 4.4. Anhydrous sodium sulphate, for analysis quality. 4.5. Acetone, for chromatography quality. 4.6. Ethyl ether, for chromatography quality. 4.7. Ethanol of analytical quality. 4.8. Ethyl acetate of analytical quality. 4.9. Internal standard, α-cholestanol, purity more than 99 % (purity must be checked by GC analysis). 4.10. Internal standard solution of α-cholestanol, 0,2 solution (m/V) in ethyl acetate (4.8). 4.11. Phenolphthalein solution, 10 g/L in ethanol (4.7). 4.12. A 0,1 % (m/v) solution of 1-eicosanol in ethyl acetate (internal standard).
3.1. Complete apparatus for analysis by thin-layer chromatography using 20 × 20 cm glass plates. 3.2. Ultraviolet lamp with a wavelength of 366 or 254 nm. 3.3. Microsyringes, 100 μL and 500 μL. 3.4. Cylindrical filter funnel with a G3 porous septum (porosity 15-40 μm) of diameter approximately 2 cm and a depth of 5 cm, suitable for filtration under vacuum with male ground-glass joint. 3.5. Conical flask with ground-glass female joint, 50 mL which can be fitted to the filter funnel (3.4). 3.6. Test tube with a tapering bottom and a sealing glass stopper, 10 mL. 3.7. Calcium dichloride desiccator. 3.8. HPLC system, consisting of: 3.8.1. Binary pump. 3.8.2. Manual or automatic injector equipped with 200 μL injection loop. 3.8.3. In-line degasser. 3.8.4. UV-VIS or IR detector.
3.9. HPLC column (25 cm × 4 mm i.d.) with silica gel 60 (5 μm particle size). 3.10. Syringe filter, 0,45 μm. 3.11. Conical flask 25 mL.
4.1. Potassium hydroxide minimum titre 85 %. 4.2. Potassium hydroxide ethanolic solution, approximately 2 M. Dissolve 130 g of potassium hydroxide (4.1) with cooling in 200 ml of distilled water and then make up to one litre with ethanol (4.9). Keep the solution in well-stoppered dark glass bottles and stored maximum 2 days. 4.3. Ethyl ether, for analysis quality. 4.4. Potassium hydroxide ethanolic solution, approximately 0,2 M. Dissolve 13 g of potassium hydroxide (4.1) in 20 ml of distilled water and make up to one litre with ethanol (4.9). 4.5. Glass 20x20 plates coated with silica gel, without fluorescence indicator, thickness 0,25 mm (commercially available ready for use). 4.6. Acetone, for chromatography quality. 4.7. n-Hexane, for chromatography quality. 4.8. Ethyl ether, for chromatography quality. 4.9. Ethanol of analytical quality. 4.10. Ethyl acetate of analytical quality. 4.11. Reference solution for thin-layer chromatography: cholesterol, phytosterols, alcohols and Erythrodiol 5 % solution in Ethyl acetate (4.10). 4.12. Solution of 2,7-dichlorofluorescein, 0,2 % in ethanolic solution. Make slightly basic by adding a few drops of 2 M alcoholic potassium hydroxide solution (4.2). 4.13. n-Hexane (4.7)/ethyl ether (4.8) mixture 65:35 (V/V). 4.14. HPLC mobile phase n-hexane (4.7)/ethyl ether (4.8) (1:1) (V/V).
3.1. Test tube with a tapering bottom and a sealing glass stopper, 10 mL. 3.2. Gas chromatograph suitable for use with a capillary column with split injection system, consisting of: 3.2.1. A thermostatic chamber for columns capable of maintaining the desired temperature with an accuracy of ± 1 °C; 3.2.2. A temperature-adjustable injection unit with a persilanised glass vaporising element and split system; 3.2.3. A flame ionisation detector (FID); 3.2.4. Data acquisition system suitable for use with the FID detector (3.10.3.), capable of manual integration.
3.3. Fused-silica capillary column of length 20 to 30 m, internal diameter 0,25 to 0,32 mm, coated with 5 % Diphenyl - 95 % Dimethylpolysiloxane (SE-52 or SE-54 stationary phase or equivalent), to a uniform thickness between 0,10 and 0,30 μm. 3.4. Microsyringe, of 10 μL capacity, for gas chromatography, with cemented needle suitable for split injection.
4.1. Anhydrous pyridine, for chromatography quality. 4.2. Hexamethyl disilazane of analytical quality. 4.3. Trimethylchlorosilane of analytical quality. 4.4. Sample solutions of sterol trimethylsilyl ethers. To be prepared at the time of use from sterols and erythrodiol obtained from oils containing them. 4.5. Standard solutions of trimethylsilyl ethers of aliphatic alcohols from C20 to C28. They may be prepared from mixtures of pure alcohols at the time they are required for use. 4.6. Carrier gas: hydrogen or helium, gas-chromatographic purity. 4.7. Auxiliary gases: hydrogen, helium, nitrogen and air, of gas-chromatographic purity. 4.8. Silylation reagent, consisting of a 9:3:1 (V/V/V) mixture of pyridine/hexamethyl disilazane/trimethylchlorosilane. 4.9. n-Hexane, for chromatography quality.
Oven Program | 180 °C (8 min.) → 260 °C (at 5 °C/min) → 260 °C (15 min) |
---|---|
Injector Temperature | 280 °C |
Detector Temperature | 290 °C |
Linear Velocity of Carrier gas | Helium (20 to 30 cm/s); Hydrogen (30 to 50 cm/s) |
Split Ratio | 1:50 to 1:100 |
Volume Injected | 0,5 to 1 μL of TMSE solution |
Oven Program | 260 ± 5 °C Isothermal |
---|---|
Injector Temperature | 280 – 300 °C |
Detector Temperature | 280 – 300 °C |
Linear Velocity of Carrier gas | Helium (20 to 30 cm/s); Hydrogen (30 to 50 cm/s) |
Split Ratio | 1:50 to 1:100 |
Volume Injected | 0,5 to 1 μL of TMSE solution |
Alcohol C26 retention time shall be 18 ± 5 minutes. Alcohol C22 peak shall be 80 ± 20 % of the full-scale value for olive oil and 40 ± 20 % of the full-scale value for olive-pomace oil. The retention time for the β-sitosterol peak should be at 20 ± 5 min. The campesterol peak should be: for olive oil (mean content 3 %) 20 ± 5 % of full scale. All the present sterols must be separated. In addition to being separated, the peaks must also be completely resolved, i.e. the peak trace should return to the base line before leaving for the next peak. Incomplete resolution is, however, tolerated, provided that the peak at RRT 1,02 (Sitostanol) can be quantified using the perpendicular.
Hydrogen, pure, gas chromatography grade. Air, pure, gas chromatography grade.
4.3.1. Degasser for the mobile phase. 4.3.2. Rheodyne injector valve with a 10 μL loop. 4.3.3. High pressure pump unit. 4.3.4. Thermostatic oven for the HPLC column capable of maintaining sub-ambient temperatures (15-20 °C), (for example, Peltier type). 4.3.5. Refractive index detector. 4.3.6. Computerised data acquisition system provided with an integration program.
4.4.1. Split injector. 4.4.2. Flame ionisation detector (FID). 4.4.3. Oven with programmable temperature. 4.4.4. Computerised data acquisition system provided with an integration program.
Palmitic; | P (C16:0) | = | methyl ester + ethyl ester |
Stearic; | S (C18:0) | = | methyl ester |
Palmitoleic; | Po (C16:1) | = | sum of methyl esters of the two |
Oleic; | O (C18:1) | = | sum of methyl esters of the two |
Linoleic; | L (C18:2) | = | methyl ester+ ethyl ester + |
Linolenic; | Ln (C18:3) | = | methyl ester + |
Arachidic; | A (C20:0) | = | methyl ester |
Eicosenoic (gondoic); | G (C20:1) | = | methyl ester |
ECN | HPLC peaks | TAGs | Sample 1 | Sample 2 | Sample 3 | Sample 4 | Sample 5 | |||||
---|---|---|---|---|---|---|---|---|---|---|---|---|
Mean (%) | RSD | Mean (%) | RSD | Mean (%) | RSD | Mean (%) | RSD | Mean (%) | RSD | |||
LLL | ||||||||||||
OLLn+ PoLL | ||||||||||||
PLLn | ||||||||||||
OLL | ||||||||||||
OOLn+ PoOL | ||||||||||||
PLL+ PoPoO | ||||||||||||
POLn+ PpoPo+ PpoL | ||||||||||||
OOL+ LnPP | ||||||||||||
PoOO | ||||||||||||
SLL+ PLO | ||||||||||||
PoOP+ SpoL+ SOLn+ SpoPo | ||||||||||||
OOO+ PLP+ PoPP | ||||||||||||
SOL | ||||||||||||
POO | ||||||||||||
POP | ||||||||||||
SOO | ||||||||||||
POS+ SLS |
Labelling | Chemical parameters | Organoleptic characteristics | Final conclusion | ||||||||||||||
---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
Sample | Category | Country of origin | Place of inspection | Legal name | Designation of origin | Storage conditions | Erroneous information | Legibility | C/NC | If so, please indicate which one(s) | C/NC | Median defect | Fruity Median | C/NC | Required action | Sanction | |