- Y Diweddaraf sydd Ar Gael (Diwygiedig)
- Pwynt Penodol mewn Amser (01/01/2008)
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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
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Textual Amendments
F1 Inserted by 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.
Determination of the composition of triacylglycerols (TAGs) in olive oils, in terms of their equivalent carbon number by differences between the analytical results obtained by high performance liquid chromatography (HPLC) and the theoretical content, calculated starting from the fatty acid composition.
The standard is applicable to olive oils. The method is applicable to the detection of the presence of small amounts of seed oils (rich in linoleic acid) in every class of olive oils.
The content of triacylglycerols with ECN42 determined by HPLC analysis and the theoretical content of triacylglycerols with ECN42 (calculated on the basis of GLC determination of fatty acid composition) correspond within a certain limit for pure oils. A difference larger than the values stated in the Regulation for each type of oil points out that the oil contains seed oils.
The method for calculation of theoretical content of triacylglycerols with ECN42 and of the difference between the HPLC data and this one essentially is made by the coordination of analytical data obtained by means of other methods: it is possible to distinguish three phases: determination of fatty acid composition by capillary gas chromatography, calculation of theoretical composition of triacylglycerols with ECN42, HPLC determination of ECN42 triacylglycerols
The reagents should be of analytical purity. Elution solvents should be de-gassed, and may be recycled several times without effect on the separations.
As a number of interfering substances can rise false positive results, the sample must always be purified according to IUPAC method 2.507, used for determination of polar substances in oxidised oils.
Fill the column (4.1.3) with about 30 ml of elution solvent (4.2.3), then introduce inside the column some glass wool (4.2.5) pushing it to the bottom of the column by means of the glass rod (4.1.5).
In a 100 ml beaker, suspend 25 g of silicagel (4.2.4) in 80 ml of elution mixture (4.2.3), then transfer it inside the column, by means of a glass funnel (4.1.6).
To ensure the complete transfer of silicagel inside the column, wash the beaker with the elution mixture and transfer the washing portions inside the column, too.
Open the cock and let solvent elute from the column until its level is about 1 cm over the silicagel.
Weigh with the accuracy of 0,001 g, 2,5 ± 0,1 g of oil, previously filtered, homogenized and anhydrified, if necessary, in a 50 ml volumetric flask (4.1.7). Solve it in about 20 ml of elution solvent (4.2.3), if necessary, slightly heat it to make the dissolution easily. Cool at room temperature and adjust the volume with elution solvent.
By means of a volumetric pipette, introduce 20 ml of solution inside the column prepared according to 4.3.1, open the cock and let solvent elute to the silicagel layer level.
Then elute with 150 ml of elution solvent (4.2.3), adjusting the solvent rate at about 2 ml/min (150 ml will take about 60 to 70 minutes to pass through the column).
The eluated is recovered in a 250 ml round bottom flask (4.1.1) previously tared in an oven and exactly weighted. Eliminate solvent at reduce pressure (Rotavapor) and weigh the residue that will be used to prepare the solution for HPLC analysis and for methyl ester preparation.
The sample recovery from the column must be 90 % at least for extra virgin, virgin, ordinary refined and olive oil categories, and a minimum of 80 % for lampante and residue olive oils.
A 5 % solution of the sample to be analysed is prepared by weighing 0,5 ± 0,001 g of the sample into a 10 ml graduated flask and making up to 10 ml with the solubilization solvent (4.2.9).
Set up the chromatographic system. Pump elution solvent (4.2.8) at a rate of 1,5 ml/min to purge the entire system. Wait until a stable base line is obtained. Inject 10 μl of the sample prepared as in 4.3.
Use the area normalization method, i.e. assume that the sum of the areas of the peaks corresponding to TAGs from ECN42 up to ECN52 is equal to 100 %. Calculate the relative percentage of each triglyceride using the formula:
% triglyceride = area of peak × 100/ sum of peak areas.
The results are to be given to within at least two decimal places.
The elution order can be determined by calculating the equivalent carbon numbers, often defined by the relation ECN = CN-2n, where CN is the carbon number and n is the number of double bounds, it can be calculated more precisely by taking into account the origin of the double bond. If n o , n l and n ln are the numbers of double bonds attributed to oleic, linoleic and linolenic acids respectively, the equivalent carbon number can be calculated by means of the relation of the formula: U.K.
ECN = CN - d o n o - d l n l - d ln n ln ,
where the coefficient do, d l and d ln can be calculated by means of the reference triglycerides. Under the conditions specified in this method, the relation obtained will be close in:
ECN = CN - (2,60 n o ) - (2,35 n l ) - (2,17 n ln )
Examples: | Lichrosorb (Merck) RP 18 Art 50333 |
Lichrosphere or equivalent (Merck) 100 CH18 Art 50377. |
With several reference triglycerides, it is also possible to calculate the resolution with respect to triolein: U.K.
α = RT' / RT triolein
by use of the reduced retention time RT' = RT - RT solvent.
The graph of log α against f (number of double bonds) enables the retention values to be determined for all the triglycerides of fatty acids contained in the reference triglycerides — see figure 2.
The efficiency of the column should permit clear separation of the peak of trilinoein from the peaks of the triglycerides with an adjacent RT. The elution is carried out up to ECN52 peak. U.K.
A correct measure of the areas of all peaks of interest for the present determination is ensured if the second peak corresponding to ECN50 is 50 % of full scale of the recorder. U.K.
Fatty acid composition is carried out by means of the EEC gas chromatographic method reported in Annex X A of Regulation (EEC) No 2568/91, by means of a capillary column. The methyl esters preparation is carried out according to Annex X B (sodium methylate alcohol solution).
Glycerides are grouped by their equivalent carbon number (ECN), taking into account the following equivalencies between ECN and fatty acids. Only fatty acids with 16 and 18 carbon atoms were taken in consideration, because only these are important for olive oil.
Fatty acid (FA) | Abbreviation | Molecular weight (MW) | ECN |
---|---|---|---|
Palmatic acid | P | 256,4 | 16 |
Palmatoleic acid | Po | 254,4 | 14 |
Stearic acid | S | 284,5 | 18 |
Oleic acid | O | 282,5 | 16 |
Linoleic acid | L | 280,4 | 14 |
Linolenic acid | Ln | 278,4 | 12 |
The result gives the percentage of each fatty acid in moles % in the overall (1,2,3-) position of the TAGs.
Then the sum of the saturated fatty acids P and S (SFA) and the unsaturated fatty acids Po, O, L and Ln (UFA) are calculated:
moles % SFA = moles % P + moles % S | (3) |
moles UFA = 100 - moles % SFA |
The fatty acids are distributed to three pools as follows: two identical for 1- and 3- positions and one for 2- position, with different coefficients for the saturated (P and S) and unsaturated acids (Po, O, L and Ln).
moles % P(2) = moles % P (1,2,3) * 0,06 | (4) |
moles % S(2) = moles % S (1,2,3) * 0,06 |
The following triglycerides with ECN42 are calculated according equation 7, 8 and 9 in order of expected elution in HPLC (normally only three peaks).
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
The triacylglycerides with ECN42 are given by the sum of the nine triacylglycerols including their positional isomers. The results to be given with at least two decimal places.
The calculated theoretical content and the content determined by the HPLC analysis are compared. If the difference between HLPC data minus theoretical data is greater than the values states for the appropriate oil category in the Regulation, the sample contains seed oil.
Results are given to within one decimal figure. U.K.
The following data are obtained for the fatty acid composition by GLC:
FA MW | P 256,4 | S 284,5 | Po 254,4 | O 282,5 | L 280,4 | Ln 278,4 |
---|---|---|---|---|---|---|
area % | 10,0 | 3,0 | 1,0 | 75,0 | 10,0 | 1,0 |
Sum of the saturated and unsaturated fatty acids in the 1,2,3- position of TAGs
moles % SFA = 10,888 % + 2,944 % = 13,831 % | See formula (3) |
moles % UFA = 100,000 % — 13,831 % = 86,169 % | See formula (3) |
moles % P(2) = 10,888 % * 0,06 = 0,653 moles % | See formula (4) |
moles % S(2) = 2,944 % * 0,06 = 0,177 moles % | See formula (4) |
From the calculated fatty acid composition in sn-2- and sn-1,3- positions (see above):
FA in | 1,3-pos. | 2-pos. |
---|---|---|
P | 16,005 % | 0,653 % |
S | 4,327 % | 0,177 % |
Po | 1,015 % | 1,263 % |
O | 68,522 % | 85,295 % |
L | 9,205 % | 11,458 % |
Ln | 0,927 % | 1,154 % |
Sum | 100,0 % | 100,0 % |
the following triacylglycerols are calculated:
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.
La = lauric acid; My = myristic acid; P = palmitic acid; St = stearic acid; O = oleic acid; L = linoleic acid; Ln = linolenic acid.] ] U.K.
Textual Amendments
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