EN ISO 22959:2009

Animal and vegetable fats and oils - Determination of polycyclic aromatic hydrocarbons by on-line donor-acceptor complex chromatography and HPLC with fluorescence detection (ISO 22959:2009)

ISO 22959:2009 specifies a high performance liquid chromatographic (HPLC) procedure for the determination of polycyclic aromatic hydrocarbons (PAHs) in edible fats and oils.
The method has been validated for coconut, olive, sunflower, and soybean oil, and is possibly applicable to other oils, dependent on the determination of appropriate parameters.
The lowest level of quantification for the PAHs is 0,1 µg/kg. The lowest possible amount of each PAH which can be distinguished from the baseline noise has not been determined. The validated concentration range of the method is 0,1 µg/kg to 3,5 µg/kg for each individual PAH. For samples containing (light) PAH contents > 3,5 µg/kg, dilution to bring the contents into the validated range is possible. It is also possible to adjust the range of the calibration curves. However, ranges exceeding 3,5 µg/kg have not been validated.
PAHs which can be determined by this method are: anthracene, phenanthrene, fluoranthene, pyrene, chrysene, benzo[a]anthracene, benzo[e]pyrene, benzo[a]pyrene, perylene, benzo[ghi]perylene, anthanthrene, dibenzo[a,h]anthracene, coronene, indeno[1,2,3-cd]pyrene, benzo[a]fluoranthene, benzo[b]fluoranthene, benzo[k]fluoranthene.

Tierische und pflanzliche Fette und Öle - Bestimmung polycyclischer aromatischer Kohlenwasserstoffe durch gekoppelte Donor-Akzeptor-Komplex-Chromatographie und HPLC mit Fluoreszenzdetektion (ISO 22959:2009)

Diese Internationale Norm legt ein hochleistungs-flüssigchromatographisches (HPLC, en.: high performance liquid chromatographic) Verfahren zur Bestimmung von polycyclischen aromatischen Kohlenwasserstoffen (PAK) in Speise¬fetten und -ölen.
Das Verfahren wurde bereits für Kokosnuss- (CN, en.: coconut), Oliven- (OV, en.: olive), Sonnenblumen- (SF, en.: sunflower) und Sojabohnenöl (BO, en.: Soyabean) validiert und ist möglicherweise anwendbar auf andere Öle, abhängig von der Bestimmung geeig¬neter Parameter.
Das geringste Niveau der Quantifizierung von PAKs beträgt 0,1 µg/kg. Die geringste mögliche Menge jedes PAK, die aus dem Basislinienrauschen differenziert werden kann, ist nicht ermittelt worden. Der validierte Konzentrationsbereich des Verfahrens liegt zwischen 0,1 µg/kg und 3,5 µg/kg für jeden einzelnen PAK. Für Proben, die (leichte) PAK-Gehalte > 3,5 µg/kg haben, ist eine Verdünnung möglich, um die Gehalte in einen validierten Bereich zu bringen. Eine Anpassung des Bereiches der Kalibrierkurven ist ebenfalls möglich. Bereiche oberhalb 3,5 µg/kg sind jedoch nicht validiert.
PAK, die mit diesem Verfahren bestimmt werden können sind: Anthracen, Phenanthren, Fluoranthen, Pyren, Chrysen, Benzo[a]anthracen, Benzo[e]pyren, Benzo[a]pyren, Perylen, Benzo[g,h,i]perylen, Anthanthren, Dibenzo[a,h]anthracen, Coronen, Indeno[1,2,3-cd]pyren, Benzo[a]fluoranthen, Benzo[b]fluoranthen, Benzo[k]fluoran¬then.

Corps gras d'origines animale et végétale - Détermination de la teneur en hydrocarbures aromatiques polycycliques par chromatographie de complexe donneur-accepteur et CLHP avec détection par fluorescence (ISO 22959:2009)

L'ISO 22959:2009 spécifie un mode opératoire de chromatographie liquide à haute performance (CLHP) permettant de déterminer la teneur en hydrocarbures aromatiques polycycliques (HAP) dans les corps gras comestibles.
La méthode a été validée pour l'huile de coco (CN), l'huile d'olive (OV), l'huile de tournesol (SF) et l'huile de soja (BO) et peut être applicable à d'autres huiles après détermination des paramètres appropriés.
La plus faible limite de quantification pour l'ensemble des HAP est fixée à 0,1 μg/kg. La plus petite quantité de chaque HAP qu'il est possible de distinguer des signaux parasites n'a pas été déterminée. La plage de concentration validée pour la méthode est comprise entre 0,1 μg/kg et 3,5 μg/kg pour chaque HAP. Dans le cas de teneurs en HAP (légers) supérieures à 3,5 μg/kg, il est possible de diluer les échantillons afin d'amener la teneur dans la plage validée. Il est également possible de régler le domaine de travail des courbes d'étalonnage. Cependant, les domaines supérieurs à 3,5 μg/kg n'ont pas été validés.
La présente méthode permet de déterminer les HAP suivants: anthracène, phénanthrène, fluoranthène, pyrène, chrysène, benz[a]anthracène, benzo[e]pyrène, benzo[a]pyrène, pérylène, benzo[ghi]pérylène, anthanthrène, dibenz[a,h]anthracène, coronène, indéno[1,2,3-cd]pyrène, benzo[a]fluoranthène, benzo[b]fluoranthène, benzo[k]fluoranthène.

Živalske in rastlinske maščobe in olja - Določevanje policikličnih aromatskih ogljikovodikov z neposredno kompleksno "donor-akceptor" kromatografijo in HPLC s fluorescenčno detekcijo (ISO 22959:2009)

General Information

• Status: Published
• Publication Date: 14-May-2009
• Withdrawal Date: 29-Nov-2009
• ICS: 67.200.10 - Animal and vegetable fats and oils
• Technical Committee: CEN/TC 307 - Oilseeds, vegetables and animal fats and oils and their by-products - Methods of sampling and analys
• Drafting Committee: ISO/TC 34 - ISO/TC 34
• Current Stage: 6060 - Definitive text made available (DAV) - Publishing
• Start Date: 15-May-2009
• Completion Date: 15-May-2009
• Ref Project: SIST EN ISO 22959:2009 - Animal and vegetable fats and oils - Determination of polycyclic aromatic hydrocarbons by on-line donor acceptor complex chromatography and HPLC with fluorescence detection (ISO 22959:2009)

Standards Content (Sample)

SLOVENSKI STANDARD
01-september-2009
äLYDOVNHLQUDVWOLQVNHPDãþREHLQROMD'RORþHYDQMHSROLFLNOLþQLKDURPDWVNLK
RJOMLNRYRGLNRY]QHSRVUHGQRNRPSOHNVQRGRQRUDNFHSWRUNURPDWRJUDILMRLQ
+3/&VIOXRUHVFHQþQRGHWHNFLMR,62
Animal and vegetable fats and oils - Determination of polycyclic aromatic hydrocarbons
by on-line donor acceptor complex chromatography and HPLC with fluorescence
detection (ISO 22959:2009)
Tierische und pflanzliche Fette und Öle - Bestimmung polycyclischer aromatischer
Kohlenwasserstoffe durch direkte Donor-Akzeptor-Komplex-Chromatographie und HPLC
mit Fluoreszenzdetektion (ISO 22959:2009)
Corps gras d'origines animale et végétale - Détermination de la teneur en hydrocarbures
aromatiques polycycliques par chromatographie de complexe donneur -accepteur et
CLHP avec détection par fluorescence (ISO 22959:2009)
Ta slovenski standard je istoveten z: EN ISO 22959:2009
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 22959
NORME EUROPÉENNE
EUROPÄISCHE NORM
May 2009
ICS 67.200.10
English Version
Animal and vegetable fats and oils - Determination of polycyclic
aromatic hydrocarbons by on-line donor-acceptor complex
chromatography and HPLC with fluorescence detection (ISO
22959:2009)
Corps gras d'origines animale et végétale - Détermination Tierische und pflanzliche Fette und Öle - Bestimmung
de la teneur en hydrocarbures aromatiques polycycliques polycyclischer aromatischer Kohlenwasserstoffe durch
par chromatographie de complexe donneur-accepteur et gekoppelte Donor-Akzeptor-Komplex-Chromatographie und
CLHP avec détection par fluorescence (ISO 22959:2009) HPLC mit Fluoreszenzdetektion (ISO 22959:2009)
This European Standard was approved by CEN on 1 May 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 22959:2009: E
worldwide for CEN national Members.

Contents Page
Foreword .3

Foreword
This document (EN ISO 22959:2009) 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 November 2009, and conflicting national standards shall be withdrawn
at the latest by November 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.
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 22959:2009 has been approved by CEN as a EN ISO 22959:2009 without any modification.

INTERNATIONAL ISO
STANDARD 22959
First edition
2009-05-15
Animal and vegetable fats and oils —
Determination of polycyclic aromatic
hydrocarbons by on-line donor-acceptor
complex chromatography and HPLC with
fluorescence detection
Corps gras d'origines animale et végétale — Détermination de la teneur
en hydrocarbures aromatiques polycycliques par chromatographie de
complexe donneur-accepteur et CLHP avec détection par fluorescence

Reference number
ISO 22959:2009(E)
©
ISO 2009
ISO 22959:2009(E)
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ISO 22959:2009(E)
Contents Page
Foreword. iv
Introduction . v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions. 1
4 Principle. 2
5 Reagents, materials and standards . 3
6 Apparatus . 5
7 Sampling and preparation of the test sample. 5
8 Sample preparation . 6
9 Procedure . 7
9.1 HPLC analysis . 7
9.2 Identification of PAHs. 7
10 Calculation of individual PAHs. 7
11 Method validation data. 8
11.1 Accuracy. 8
11.2 Within-laboratory precision . 8
11.3 Recovery. 8
11.4 Dynamic range . 8
11.5 Limit of quantification . 8
12 Precision. 9
12.1 International collaborative trial . 9
12.2 Repeatability. 9
12.3 Reproducibility. 9
13 Test report . 9
Annex A (informative) Example of the individual parts of an HPLC system. 10
Annex B (informative) Example of the operating conditions of the pumps of the HPLC system. 11
Annex C (informative) Example of the operating conditions of the column thermostat and
the detector of the HPLC system . 12
Annex D (informative) Example of the autosampler programme of the HPLC system. 13
Annex E (informative) Tubing connections of the HPLC system. 14
Annex F (informative) Chromatogram of a standard calibration sample . 15
Annex G (informative) Determination precision for a sunflower oil, range 0,1 µg/kg to 3,5 µg/kg. 16
Annex H (informative) Determination precision for an olive oil, range 0,1 µg/kg to 3,5 µg/kg. 17
Annex I (informative) Determination precision for a soybean oil, range 0,1 µg/kg to 3,5 µg/kg. 18
Annex J (informative) Determination precision for a coconut oil, range 0,1 µg/kg to 3,5 µg/kg. 19
Annex K (informative) Interlaboratory test . 20
Bibliography . 22

ISO 22959:2009(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 22959 was prepared by Technical Committee ISO/TC 34, Food products, Subcommittee SC 11, Animal
and vegetable fats and oils.
iv © ISO 2009 – All rights reserved

ISO 22959:2009(E)
Introduction
Polycyclic aromatic hydrocarbons (PAHs) are formed during pyrolytic processes such as the incomplete
combustion of organic substances or have a petrogenic origin (mineral oils). Edible fats and oils may be
contaminated by environmental pollution and/or processing s
...