EN ISO 16931:2009
(Main)Animal and vegetable fats and oils - Determination of polymerized triacylglycerols by high-performance size-exclusion chromatography (HPSEC) (ISO 16931:2009)
Animal and vegetable fats and oils - Determination of polymerized triacylglycerols by high-performance size-exclusion chromatography (HPSEC) (ISO 16931:2009)
ISO 16931:2009 specifies a method using high-performance size-exclusion chromatography (HPSEC) to determine the contents, as mass fractions, of polymerized triacylglycerols (PTAGs) in oils and fats which contain at least 3 % (from peak areas) of these polymers. PTAGs (strictly speaking dimeric and oligomeric triacylglycerols) are formed during the heating of fats and oils, and thus, the method serves to assess the thermal deterioration of frying fats after use.
This method is applicable to frying fats and fats and oils that have been thermally treated, provided that the content of PTAGs is at least 3 %. It can also be applied to the determination of polymers in fats for animal feedstuffs, although in this case, the extraction method used can have an influence on the result.
Tierische und pflanzliche Fette und Öle - Bestimmung von polymerisierten Triacylglycerinen mit Hochleistungs-Ausschlusschromatographie (HPSEC) (ISO 16931:2009)
Diese Internationale Norm legt ein Verfahren zur Bestimmung der Gehalte an polymerisierten Triglyceriden in Ölen und Fetten, die mindestens 3 % (bezogen auf die Peakflächen) dieser Polymere enthalten, durch Hochleistungs-Größenausschlusschromatographie (en: high-performance size-exclusion chromatography (HPSEC)) fest. Polymerisierte Triglyceride (genau genommen dimere und oligomere Triglyceride) werden bei der Erhitzung von Fetten und Ölen gebildet; folglich dient dieses Verfahren der Beurteilung der thermisch bedingten Qualitätsminderung von Frittierfetten im Verlaufe ihrer Verwendung.
Das Verfahren ist auf Frittierfette anwendbar, die thermisch behandelt wurden, vorausgesetzt, der Gehalt an polymerisierten Triglyceriden beträgt mindestens 3 %. Es kann auch zur Bestimmung von Polymeren in Futterfetten angewendet werden. In diesem Fall kann das angewendete Extraktionsverfahren das Ergebnis beeinflussen (siehe ISO 6492).
Corps gras d'origines animale et végétale - Détermination de la teneur en triacylglycérols polymérisés par chromatographie liquide d'exclusion à haute performance (CLHP d'exclusion) (ISO 16931:2009)
L'ISO 16931:2009 spécifie une méthode utilisant la chromatographie liquide d'exclusion à haute performance (CLHP d'exclusion) pour la détermination de la teneur en triacylglycérols polymérisés (PTAG), en fraction massique, dans les corps gras contenant au moins 3 % (à partir des aires de pics) de ces polymères. Les PTAG (à proprement parler les triacylglycérols dimériques et oligomériques) se forment pendant le chauffage des corps gras; par conséquent, cette méthode sert à évaluer la détérioration thermique des corps gras ayant été utilisés en friture.
Cette méthode est applicable aux graisses de friture et aux corps gras ayant été traités thermiquement, à condition que la teneur en PTAG soit au moins égale à 3 %. Elle peut également être appliquée à la détermination des polymères dans les graisses contenues dans les aliments pour animaux. Dans ce cas, la méthode d'extraction utilisée peut avoir une influence sur le résultat.
Rastlinske in živalske maščobe in olja - Določevanje polimeriziranih triacilglicerolov s kromatografijo visoke ločljivosti z ločevanjem po velikosti (HPSEC) (ISO 16931:2009)
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
01-julij-2009
1DGRPHãþD
SIST EN ISO 16931:2002
5DVWOLQVNHLQåLYDOVNHPDãþREHLQROMD'RORþHYDQMHSROLPHUL]LUDQLK
WULDFLOJOLFHURORYVNURPDWRJUDILMRYLVRNHORþOMLYRVWL]ORþHYDQMHPSRYHOLNRVWL
+36(& ,62
Animal and vegetable fats and oils - Determination of polymerized triacylglycerols by
high-performance size-exclusion chromatography (HPSEC) (ISO 16931:2009)
Tierische und pflanzliche Fette und Öle - Bestimmung von polymerisierten
Triacylglycerinen mit Hochleistungs-Ausschlusschromatographie (HPSEC) (ISO
16931:2009)
Corps gras d'origines animale et végétale - Détermination de la teneur en triacylglycérols
polymérisés par chromatographie liquide d'exclusion à haute performance (CLHP
d'exclusion) (ISO 16931:2009)
Ta slovenski standard je istoveten z: EN ISO 16931:2009
ICS:
67.200.10 5DVWOLQVNHLQåLYDOVNH Animal and vegetable fats
PDãþREHLQROMD and oils
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
EUROPEAN STANDARD
EN ISO 16931
NORME EUROPÉENNE
EUROPÄISCHE NORM
April 2009
ICS 67.200.10 Supersedes EN ISO 16931:2001
English Version
Animal and vegetable fats and oils - Determination of
polymerized triacylglycerols by high-performance size-exclusion
chromatography (HPSEC) (ISO 16931:2009)
Corps gras d'origines animale et végétale - Détermination Tierische und pflanzliche Fette und Öle - Bestimmung des
de la teneur en triacylglycérols polymérisés par Gehaltes an polymerisierten Triglyceriden mit
chromatographie liquide d'exclusion à haute performance Hochleistungs-Ausschlusschromatographie (HPSEC) (ISO
(CLHP d'exclusion) (ISO 16931:2009) 16931:2009)
This European Standard was approved by CEN on 16 March 2009.
CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European
Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national
standards may be obtained on application to the CEN Management Centre or to any CEN member.
This European Standard exists in three official versions (English, French, German). A version in any other language made by translation
under the responsibility of a CEN member into its own language and notified to the CEN Management Centre has the same status as the
official versions.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland,
France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal,
Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: Avenue Marnix 17, B-1000 Brussels
© 2009 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 16931:2009: E
worldwide for CEN national Members.
Contents Page
Foreword .3
Foreword
This document (EN ISO 16931:2009) has been prepared by Technical Committee ISO/TC 34 "Agricultural
food products" in collaboration with Technical Committee CEN/TC 307 “Oilseeds, vegetable and animal fats
and oils and their by-products - Methods of sampling and analysis”, the secretariat of which is held by
AFNOR.
This European Standard shall be given the status of a national standard, either by publication of an identical
text or by endorsement, at the latest by October 2009, and conflicting national standards shall be withdrawn at
the latest by October 2009.
Attention is drawn to the possibility that some of the elements of this document may be the subject of patent
rights. CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent rights.
This document supersedes EN ISO 16931:2001.
According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following
countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Cyprus, Czech
Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia,
Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain,
Sweden, Switzerland and the United Kingdom.
Endorsement notice
The text of ISO 16931:2009 has been approved by CEN as a EN ISO 16931:2009 without any modification.
INTERNATIONAL ISO
STANDARD 16931
Second edition
2009-04-15
Animal and vegetable fats and oils —
Determination of polymerized
triacylglycerols by high-performance
size-exclusion chromatography (HPSEC)
Corps gras d'origines animale et végétale — Détermination de la teneur
en triacylglycérols polymérisés par chromatographie liquide d'exclusion
à haute performance (CLHP d'exclusion)
Reference number
ISO 16931:2009(E)
©
ISO 2009
ISO 16931:2009(E)
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ii © ISO 2009 – All rights reserved
ISO 16931:2009(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 16931 was prepared by Technical Committee ISO/TC 34, Food products, Subcommittee SC 11, Animal
and vegetable fats and oils.
This second edition cancels and replaces the first edition (ISO 16931:2001), which has been technically
revised.
INTERNATIONAL STANDARD ISO 16931:2009(E)
Animal and vegetable fats and oils — Determination of
polymerized triacylglycerols by high-performance size-
exclusion chromatography (HPSEC)
1 Scope
This International Standard specifies a method using high-performance size-exclusion chromatography
(HPSEC) to determine the contents, as mass fractions, of polymerized triacylglycerols (PTAGs) in oils and fats
which contain at least 3 % (from peak areas) of these polymers. PTAGs (strictly speaking dimeric and
oligomeric triacylglycerols) are formed during the heating of fats and oils, and thus, the method serves to
assess the thermal deterioration of frying fats after use.
This method is applicable to frying fats and fats and oils that have been thermally treated, provided that the
content of PTAGs is at least 3 %. It can also be applied to the determination of polymers in fats for animal
feedstuffs, although in this case, the extraction method used can have an influence on the result.
[4]
NOTE For further details, see ISO 6492 .
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 International Standard, the following terms and definitions apply.
3.1
polymerized triacylglycerols
PTAGs
constituents of heated fats and oils that are determined by HPSEC under the conditions specified in this
International Standard
NOTE The content of PTAGs is expressed as a percentage mass fraction, in grams per 100 g, of all peaks from
eluted polymerized and mono-, di-, and triacylglycerols (PTAGs, MAGs, DAGs, and TAGs).
4 Principle
The sample is homogeneously mixed with tetrahydrofuran (THF) and PTAGs separated by gel permeation
chromatography according to molecular size. The compounds are detected by means of a refractive index
detector.
NOTE For better resolution, two columns in series (2 × 300 mm) are used.
ISO 16931:2009(E)
5 Reagents
Use only reagents of recognized analytical grade.
WARNING — Attention is drawn to the regulations which specify the handling of hazardous
substances. Technical, organizational and personal safety measures shall be followed.
5.1 Tetrahydrofuran (THF), for HPLC, possibly stabilized with butylhydroxytoluene (BHT), degassed, free
of water.
Ensure that the THF used as a diluent for the sample has the same water content as the eluent; otherwise a
negative peak can be observed.
5.2 Toluene, for HPLC.
5.3 Extra virgin olive oil, as standard reference: add 100 mg to 300 mg of oil to 10 ml THF and
homogenize the mixture.
NOTE Extra virgin olive oil does not contain PTAGs and can be used to determine the retention time of the
monomeric TAGs.
6 Apparatus
Usual laboratory apparatus and, in particular, the following.
6.1 Solvent reservoir, capacity 500 ml to 1 000 ml, with a polytetrafluoroethylene mobile-phase line filter.
6.2 HPLC pump, pulseless, with a volume flow rate of 0,5 ml/min to 1,5 ml/min.
6.3 Injection valve, with a 20 µl loop and a suitable syringe with a volume of 50 µl to 100 µl, or a suitable
autosampler.
6.4 Stainless-steel columns, length 2 × 300 mm, internal diameter 7,5 mm to 7,8 mm, packed with
spheres, diameter 5 µm, of high-performance styrene-divinylbenzene co-polymer gel; of pore size 10 nm or
1)
50 nm .
NOTE The chromatograms in Annex A show the required resolution with two columns.
The use of a guard column is recommended. The efficiency of the column, determined as the number, n, of
theoretical plates for monomeric TAGs, should be at least 6 000.
Maintain the temperature of the column between 30 °C and 35 °C by means of a control device.
If necessary, the column can be stored in toluene (5.2), although experience has shown that it is better to
keep the system running with THF.
6.5 Detector, temperature-controlled refractive index detector.
The ideal temperature for the detector is just above that of the column (30 °C to 35 °C).
6.6 Chromatography data system (CDS), to allow display and accurate quantification of the peak areas.
6.7 Single-use syringes, capacity 1 ml.
1) 1 nm = 10 Å
2 © ISO 2009 – All rights reserved
ISO 16931:2009(E)
2)
6.8 Nylon filters, pore size 0,45 µm .
6.9 HPLC syringe, capacity 50 µl to 100 µl.
7 Sampling
It is important that the laboratory receive a sample which is truly representative and has not been damaged or
changed during transportation or storage.
Sampling is not part of the method specified in this International Standard. A recommended sampling method
[1]
is given in ISO 5555 .
8 Preparation of test sample
The test sample shall be prepared in accordance with ISO 661.
9 Procedure
9.1 Starting up the HPLC equipment
It is advisable to follow carefully the manufacturers' recommendations. Switch on the system and pump THF
at a volume flow rate of between 0,5 ml/min and 1 ml/min to purge the whole system up to the injection valve.
Connect the column to the injection valve and wash it with about 30 ml of THF. Connect the column to the
sample cell of the detector. Fill the reference cell with THF. Adjust the mobile-phase flow to between
0,5 ml/min and 1,0 ml/min. Wait until a convenient stabilization of the system (no appreciable deviation of the
baseline) is obtained.
If the column recommended in this subclause is used, an acceptable stabilization of the
...
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