prEN ISO 12872
(Main)Olive oils and olive-pomace oils - Determination of the 2-glyceryl monopalmitate content (ISO/DIS 12872:2022)
Olive oils and olive-pomace oils - Determination of the 2-glyceryl monopalmitate content (ISO/DIS 12872:2022)
This document specifies a procedure for the determination of the content, as a percentage mass fraction, of 2-glyceryl monopalmitate in olive oils and olive-pomace oils that are liquid at ambient temperature (20 °C).
NOTE This document is based on COI/T.20/Doc. No 23/Rev.1:2017[7].
Olivenöle und Oliventresteröle – Bestimmung des Gehalts an 2-Glycerylmonopalmitat (ISO/DIS 12872:2022)
Huiles d'olive et huiles de grignons d'olive - Détermination de la teneur en 2-glycéryl monopalmitate (ISO/DIS 12872:2022)
Le présent document spécifie une méthode pour la détermination de la teneur, sous forme de fraction massique en pourcentage, en 2-glycéryl monopalmitate des huiles d’olive et des huiles de grignons d’olive liquides à température ambiante (20 °C).
NOTE Le présent document est fondé sur la COI/T.20/Doc. 23/Rév. 1:2017[7].
Oljčna olja in olja iz oljčnih tropin - Določevanje vsebnosti 2-gliceril monopalmitata (ISO/DIS 12872:2022)
General Information
RELATIONS
Standards Content (sample)
SLOVENSKI STANDARD
oSIST prEN ISO 12872:2022
01-maj-2022
Oljčna olja in olja iz oljčnih tropin - Določevanje vsebnosti 2-gliceril monopalmitata
(ISO/DIS 12872:2022)Olive oils and olive-pomace oils - Determination of the 2-glyceryl monopalmitate content
(ISO/DIS 12872:2022)Olivenöle und Oliventresteröle – Bestimmung des Gehalts an 2-Glycerylmonopalmitat
(ISO/DIS 12872:2022)Huiles d'olive et huiles de grignons d'olive - Détermination de la teneur en 2-glycéryl
monopalmitate (ISO/DIS 12872:2022)Ta slovenski standard je istoveten z: prEN ISO 12872
ICS:
67.200.10 Rastlinske in živalske Animal and vegetable fats
maščobe in olja and oils
oSIST prEN ISO 12872:2022 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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oSIST prEN ISO 12872:2022
DRAFT INTERNATIONAL STANDARD
ISO/DIS 12872
ISO/TC 34/SC 11 Secretariat: BSI
Voting begins on: Voting terminates on:
2022-03-16 2022-06-08
Olive oils and olive-pomace oils — Determination of the
2-glyceryl monopalmitate content
Huiles d'olive et huiles de grignons d'olive — Détermination de la teneur en 2-glycéryl monopalmitate
ICS: 67.200.10This document is circulated as received from the committee secretariat.
THIS DOCUMENT IS A DRAFT CIRCULATED
FOR COMMENT AND APPROVAL. IT IS
ISO/CEN PARALLEL PROCESSING
THEREFORE SUBJECT TO CHANGE AND MAY
NOT BE REFERRED TO AS AN INTERNATIONAL
STANDARD UNTIL PUBLISHED AS SUCH.
IN ADDITION TO THEIR EVALUATION AS
BEING ACCEPTABLE FOR INDUSTRIAL,
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USER PURPOSES, DRAFT INTERNATIONAL
STANDARDS MAY ON OCCASION HAVE TO
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POTENTIAL TO BECOME STANDARDS TO
WHICH REFERENCE MAY BE MADE IN
Reference number
NATIONAL REGULATIONS.
ISO/DIS 12872:2022(E)
RECIPIENTS OF THIS DRAFT ARE INVITED
TO SUBMIT, WITH THEIR COMMENTS,
NOTIFICATION OF ANY RELEVANT PATENT
RIGHTS OF WHICH THEY ARE AWARE AND TO
PROVIDE SUPPORTING DOCUMENTATION. © ISO 2022
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oSIST prEN ISO 12872:2022
ISO/DIS 12872:2022(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2022
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may
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Published in Switzerland
© ISO 2022 – All rights reserved
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oSIST prEN ISO 12872:2022
ISO/DIS 12872:2022(E)
Contents Page
Foreword ........................................................................................................................................................................................................................................iv
Introduction .................................................................................................................................................................................................................................v
1 Scope ................................................................................................................................................................................................................................. 1
2 Normative references ..................................................................................................................................................................................... 1
3 Terms and definitions .................................................................................................................................................................................... 1
4 Principle ........................................................................................................................................................................................................................ 1
5 Reagents ........................................................................................................................................................................................................................ 1
6 Apparatus .................................................................................................................................................................................................................... 2
7 Sampling ....................................................................................................................................................................................................................... 3
8 Preparation of the test sample.............................................................................................................................................................. 4
9 Procedure ....................................................................................................................................................................................................................4
9.1 Preparatory steps ................................................................................................................................................................................ 4
9.2 Column chromatography ............................................................................................................................................................... 4
9.2.1 Conventional procedure .............................................................................................................................................. 4
9.2.2 Procedure when ready-to-use silica SPE cartridges are employed ...................................... 5
9.3 Hydrolysis with pancreatic lipase ......................................................................................................................................... 5
9.4 Preparation of the silylated derivatives and gas chromatography ......................................................... 5
9.5 Gas chromatography ......................................................................................................................................................................... 5
9.5.1 Operating conditions ...................................................................................................................................................... 5
9.5.2 Identification of peaks ................................................................................................................................................... 5
9.5.3 Quantitative evaluation ............................................................................................................................................... 6
10 Expression of results ....................................................................................................................................................................................... 6
11 Precision ....................................................................................................................................................................................................................... 6
11.1 Interlaboratory test ......... ................................................................................................................................................................... 6
11.2 Repeatability ............................................................................................................................................................................................ 6
11.3 Reproducibility ....................................................................................................................................................................................... 6
12 Test report .................................................................................................................................................................................................................. 6
Annex A (informative) Chromatograms ........................................................................................................................................................... 7
Annex B (informative) Results of an interlaboratory test .........................................................................................................10
Annex C (informative) Preparation and activity of the lipase ..............................................................................................12
Bibliography .............................................................................................................................................................................................................................14
iii© ISO 2022 – All rights reserved
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oSIST prEN ISO 12872:2022
ISO/DIS 12872:2022(E)
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards
bodies (ISO member bodies). The work of preparing International Standards is normally carried out
through ISO technical committees. Each member body interested in a subject for which a technical
committee has been established has the right to be represented on that committee. International
organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.
ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of
electrotechnical standardization.International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.
The main task of technical committees is to prepare International Standards. Draft International
Standards adopted by the technical committees are circulated to the member bodies for voting.
Publication as an International Standard requires approval by at least 75 % of the member bodies
casting a vote.Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. ISO shall not be held responsible for identifying any or all such patent rights.
ISO 12872 was prepared by Technical Committee ISO/TC 34, Food products, Subcommittee SC 11,
Animal and vegetable fats and oils.© ISO 2022 – All rights reserved
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oSIST prEN ISO 12872:2022
ISO/DIS 12872:2022(E)
Introduction
As part of the Trade standard applying to olive oils and olive-pomace oils, the International Olive Council
[6](IOC) published COI/T.20/Doc. 23:2006 . COI/T.20/Doc. 23 was applicable to olive and olive-pomace
oils and was used to distinguish between lampante virgin olive oils and crude olive-pomace oils. Olive
pomace is the residual paste which still contains a variable amount of water and oil after pressing or
centrifuging.In 2008, the IOC submitted the document to ISO/TC 34/SC 11 for adoption as an International Standard.
In 2017, the IOC published a revision of the COI/T.20/Doc. n°23 (Rev.1), and this revised ISO document
is an adoption of the IOC revised method.© ISO 2022 – All rights reserved
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oSIST prEN ISO 12872:2022
DRAFT INTERNATIONAL STANDARD ISO/DIS 12872:2022(E)
Olive oils and olive-pomace oils — Determination of the
2-glyceryl monopalmitate content
1 Scope
This International Standard specifies a procedure for the determination of the content, as a percentage
mass fraction, of 2-glyceryl monopalmitate in olive oils and olive-pomace oils that are liquid at ambient
temperature (20 °C).[6]
NOTE This International Standard is based on COI/T.20/Doc. n°23/Rev.1:2017 .
2 Normative references
The following referenced documents are indispensable for the application of this document. For dated
references, only the edition cited applies. For undated references, the latest edition of the referenced
document (including any amendments) applies.ISO 661, Animal and vegetable fats and oils — Preparation of test sample
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
2-glyceryl monopalmitate content
mass fraction of 2-glyceryl monopalmitate in the monoacylglycerol fraction, determined according to
the method specified in this International StandardNote 1 to entry: The 2-glyceryl monopalmitate content is expressed as a percentage.
4 PrincipleThe oil, after suitable preparation, is subjected to the action of pancreatic lipase. A partial
hydrolysis takes place that is specific for positions 1 and 3 of the triacylglycerol molecule so that
2-monoacylglycerols are obtained as reaction products. The percentage of 2-glyceryl monopalmitate in
the monoacylglycerol fraction is determined, after silylation, by capillary gas chromatography.
5 ReagentsWARNING — Comply with any local regulations which specify the handling of hazardous
substances. Technical, organizational and personal safety measures shall be followed.
During the analysis, unless otherwise stated, use only reagents of recognized analytical grade, and
distilled or demineralized water or water of equivalent purity.5.1 Silica gel, with a particle size of 0,063 mm to 0,200 mm (70/280 mesh), prepared as follows: put
the silica gel into a porcelain cup, dry in an oven at 160 °C for 4 h, then cool at ambient temperature in a
desiccator. Add a volume of water equivalent to 5 % of the mass of the silica gel as follows: weigh 152 g
of silica gel into a 500 ml Erlenmeyer flask, add 8 g of water, stopper and homogenize carefully. Leave to
settle for at least 12 h before using.5.2 n-Hexane, chromatography grade.
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oSIST prEN ISO 12872:2022
ISO/DIS 12872:2022(E)
NOTE Hexane may be replaced by iso-octane (2,2,4- trimethylpentane in chromatography grade), provided
that comparable precision values are achieved (see Precision values of the method with the used of isooctane in
Annex B).5.3 Isopropanol.
5.4 Isopropanol-water mixture, volume fractions 50 ml/100 ml.
5.5 Pancreatic lipase, activity between 2,0 and 10 lipase units per milligram (see Annex C).
NOTE Pancreatic lipase with an activity between 2 and 10 units per mg of enzyme is available commercially.
5.6 Buffer solution of tris(hydroxymethyl)aminomethane: prepare an aqueous solution (1 mol/l)
with pH 8 and mix with concentrated HCl, volume fractions 50 ml/100 ml.5.7 Sodium cholate, special enzyme grade, aqueous solution, mass fraction 0,1 g/100 g.
Use this solution within 15 days of preparation.5.8 Calcium chloride, aqueous solution, mass fraction 22 g/100 g.
5.9 Diethyl ether, chromatography grade.
5.10 Elution solvent 1: mixture of n-hexane-diethyl ether, volume fraction of n-hexane 87 ml/100 ml
and of diethyl ether 13 ml/100 ml.5.11 Sodium hydroxide, aqueous solution, mass fraction 12 g/100 g.
5.12 Phenolphthalein, ethanolic solution, mass concentration 1 g/100 ml.
5.13 Carrier gas: hydrogen or helium, gas chromatography grade.
5.14 Auxiliary gases: hydrogen, free from moisture and organic substances, and synthetic air, gas
chromatography grade.5.15 Silylation reagent: mixture of pyridine, hexamethyldisilazane (HMDS) and trimethylchlorosilane
(TMCS); volume fractions: 9 ml/13 ml, 3 ml/13 ml, and 1 ml/13 ml, respectively.NOTE Ready-to-use solutions are available commercially. Other silylation reagents can be used, e.g. bis
trimethylsilyl trifluoracetamide + 1 % trimethylchlorosilane, diluted with an identical volume of anhydrous
pyridine.5.16 Reference samples: pure monoacylglycerols and mixtures of monoacylglycerols with a known
composition similar to that of the sample.5.17 Elution solvent 2: mixture of n-hexane-diethyl ether, volume fraction of n-hexane 90 ml/100 ml
and of diethyl ether 10 ml/100 ml.6 Apparatus
Usual laboratory equipment and in particular the following.
6.1 Erlenmeyer flasks, of capacity 25 ml.
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oSIST prEN ISO 12872:2022
ISO/DIS 12872:2022(E)
6.2 Beakers, of capacities 100 ml, 250 ml, and 300 ml.
6.3 Glass chromatography column, 21 mm to 23 mm internal diameter, 400 mm in length, with
septum and stopcock.[2]
6.4 Measuring cylinders, of capacities 10 ml, 50 ml, 100 ml, and 200 ml, ISO 4788 class A.
6.5 Round-bottomed flasks, of capacities 100 ml and 250 ml.6.6 Rotary evaporator.
6.7 Centrifuge tubes, conical bottom, of capacity 10 ml, with ground-glass stopper.
6.8 Centrifuge, suitable for 10 ml and 100 ml tubes.6.9 Water bath, capable of maintaining a temperature of (40 ± 0,5) °C.
[1]
6.10 Graduated pipettes, of capacities 1 ml and 2 ml, ISO 835 class A.
6.11 Hypodermic syringe, 1 ml.
6.12 Microsyringe, 100 µl.
6.13 Separating funnel, 1 000 ml.
6.14 Gas chromatograph, suitable for use with capillary columns, equipped with the components
specified in 6.14.1 to 6.14.5.6.14.1
...
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