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Commission Regulation (EEC) No 2568/91Show full title
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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- Revised 20/10/20193.52 MB
- Revised 04/12/20163.60 MB
- Revised 11/10/20163.55 MB
- Revised 04/08/20163.60 MB
- Revised 16/10/20153.42 MB
- Revised 01/01/20153.68 MB
- Revised 01/03/20143.69 MB
- Revised 01/01/20142.84 MB
- Revised 09/08/20122.49 MB
- Revised 01/04/20112.46 MB
- Revised 01/10/20081.42 MB
- Revised 01/01/20081.42 MB
- Revised 01/11/20035.95 MB
- Revised 22/05/20020.48 MB
- Revised 01/11/20010.66 MB
- Revised 01/07/20010.66 MB
- Revised 01/06/19990.65 MB
- Revised 01/11/19980.65 MB
- Revised 10/02/19980.65 MB
- Revised 31/10/19950.59 MB
- Revised 28/05/19950.59 MB
- Revised 01/11/19940.55 MB
- Revised 19/02/19940.55 MB
- Revised 05/02/19940.55 MB
- Revised 01/05/19930.55 MB
- Revised 21/03/19930.56 MB
- Revised 20/02/19930.56 MB
- Revised 01/11/19920.55 MB
- Revised 21/07/19920.55 MB
- Revised 03/07/19920.54 MB
- Revised 05/06/19920.54 MB
- Revised 21/12/19910.52 MB
- Revised 06/09/19910.52 MB
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Changes over time for: Division 4.3.
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- Signature words omitted by S.I. 2019/1422 reg. 6(10)
- Art. 1(8) inserted by S.I. 2019/1422 reg. 6(2)(b)
- Art. 1(8)(a)(ii)(bb) omitted in earlier amending provision S.I. 2019/1422, reg. 6(2)(b) by S.I. 2020/1453 reg. 14(16)(a)(i)
- Art. 1(8)(b) words substituted in earlier amending provision S.I. 2019/1422, reg. 6(2)(b) by S.I. 2020/1453 reg. 14(16)(a)(ii)
- Art. 1(8)(c)(ii) omitted in earlier amending provision S.I. 2019/1422, reg. 6(2)(b) by S.I. 2020/1453 reg. 14(16)(a)(iii)
- Annex 1a para. 1.1 words substituted by S.I. 2019/1422 reg. 6(11)(a)
- Annex 1a para. 1.2 words substituted by S.I. 2019/1422 reg. 6(11)(b)
- Art. 2a(3)(e) words substituted by S.I. 2019/1422 reg. 6(4)(c) (This amendment not applied to legislation.gov.uk. Reg. 6(4)(c) substituted immediately before IP completion day by S.I. 2020/1453, regs. 1(2)(b), 14(16)(c)(ii))
- Art. 2a(3)(e) words substituted by S.I. 2019/1422, reg. 6(4)(c) (as substituted) by S.I. 2020/1453 reg. 14(16)(c)(ii)
- Art. 3 words substituted by S.I. 2019/1422 reg. 6(5)(a)
- Art. 3 words substituted by S.I. 2019/1422 reg. 6(5)(b)
[F14.3. Sample preparation U.K.
As a number of interfering substances can give rise to false positive results, the sample must always be purified according to IUPAC method 2.507, used for the determination of polar compounds in frying fats.
4.3.1. Chromatographic column preparation U.K.
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 silica gel (4.2.4) in 80 ml of elution mixture (4.2.3), then transfer it to the column by means of a glass funnel (4.1.6).
To ensure the complete transfer of the silica gel to the column, wash the beaker with the elution mixture and transfer the washing portions to the column too.
Open the cock and let the solvent elute from the column until its level is about 1 cm over the silica gel.
4.3.2. Column chromatography U.K.
Weigh with the accuracy of 0,001 g, 2,5 ± 0,1 g of oil, previously filtered, homogenised and anhydrified, if necessary, in a 50 ml volumetric flask (4.1.7).
Dissolve 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 the solvent elute to the silica gel 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 60-70 minutes to pass through the column).
The eluate is recovered in a 250 ml round-bottomed flask (4.1.1) previously tared in an oven and exactly weighed. Eliminate the solvent at reduced pressure in a rotary evaporator (4.1.9) 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 the extra virgin, virgin, ordinary, refined and olive oil categories, and a minimum of 80 % for lampante and olive-pomace oils.
4.3.3. SPE purification U.K.
Silica SPE column is activated by passing 6 ml of hexane (4.2.3) under vacuum, avoiding dryness.
Weigh to an accuracy of 0,001 g, 0,12 g in a 2 ml vial (4.1.15) and dissolve with 0,5 ml of hexane (4.2.3).
Load the SPE column with the solution and elute with 10 ml of hexane-diethyl ether (87:13 v/v) (4.2.3) under vacuum.
The collected fraction is evaporated to dryness in a rotary evaporator (4.1.9) under reduced pressure at room temperature. The residue is dissolved in 2 ml of acetone (4.2.6) for triacylglycerol (TAG) analysis.]
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