EN 17517:2021
(Main)Animal feeding stuffs: Methods of sampling and analysis - Determination of mineral oil saturated hydrocarbons (MOSH) and mineral oil aromatic hydrocarbons (MOAH) with on-line HPLC-GC-FID analysis
Animal feeding stuffs: Methods of sampling and analysis - Determination of mineral oil saturated hydrocarbons (MOSH) and mineral oil aromatic hydrocarbons (MOAH) with on-line HPLC-GC-FID analysis
This document specifies a method for the determination of saturated and aromatic hydrocarbons (from C10 to C50) in feed. The method has been interlaboratory validated with on-line-HPLC-GC-FID – see [1], [2] and [3]. This method is not intended to be applied to other matrices.
The method can be used for the analysis of mineral oil saturated hydrocarbons (MOSH) and/or mineral oil aromatic hydrocarbons (MOAH).
The method is applicable for feed materials, in particular vegetable oils and other fat rich feed materials, compound feeds and pre-mixtures. It is not applicable to additives or deodistillates.
NOTE 1 The method was not designed for encapsulated matrices.
The method has been tested in an interlaboratory study via the analysis of both naturally contaminated and spiked samples (pre-mixture, soybean meal, sunflower seeds, chicken feed, pig feed, vegetable oil) ranging from 3 mg/kg to 286 mg/kg for MOSH and from 1 mg/kg to 16 mg/kg for MOAH.
According to the results of the interlaboratory study, the method has been proven suitable for MOSH and MOAH mass concentrations, each above 10 mg/kg. However, the method was not fully validated during the collaborative study for the premixture sample due to too low concentrations of MOSH and MOAH. The method was also not fully validated during the collaborative study for the sunflower seeds sample due to a too low concentration of MOAH.
NOTE 2 The conclusions regarding MOAH are based on 4 analyte / matrix combinations while the IUPAC protocol [4] expects this to be a minimum of 5.
In case of suspected interferences from natural sources, the fossil origin of the MOSH and MOAH fraction can be verified by examination of the pattern by GC-MS.
For the determination of MOSH and MOAH in edible fats and oils, another CEN standard is also available: EN 16995. For more information see [5].
Annex C proposes a manual alternative method to on-line HPLC-GC-FID analysis that can be used as a screening method for the determination of MOSH.
Futtermittel: Probenahme- und Untersuchungsverfahren - Bestimmung von mineralölgesättigten Kohlenwasserstoffen (MOSH) und mineralölaromatischen Kohlenwasserstoffen (MOAH) mit Online-Analyse durch HPLC-GC-FID
Dieses Dokument legt ein Verfahren zur Bestimmung von gesättigten und aromatischen Kohlenwasserstoffen (von C10 bis C50) in Futter fest. Das Verfahren wurde im Ringversuch mit Online-HPLC-GC-FID validiert - siehe [1], [2] und [3]. Dieses Verfahren ist nicht für die Anwendung auf andere Matrices vorgesehen.
Das Verfahren kann für die Analyse von gesättigten Mineralöl Kohlenwasserstoffen (MOSH) und/oder aromatischen Mineralöl Kohlenwasserstoffen (MOAH) verwendet werden.
Das Verfahren ist anwendbar für Futtermittel, insbesondere Pflanzenöle und andere fettreiche Futtermittel, Mischfuttermittel und Vormischungen. Es ist nicht anwendbar auf Zusatzstoffe oder Deodestillate.
ANMERKUNG 1 Das Verfahren ist nicht für gekapselte Matrizen ausgelegt.
Das Verfahren wurde in einem Ringversuch sowohl an natürlich kontaminierten als auch an angereicherten Proben (Vormischung, Sojabohnenmehl, Sonnenblumenkerne, Hühnerfutter, Schweinefutter, Pflanzenöl) in Bereichen von 3 mg/kg bis 286 mg/kg für MOSH und von 1 mg/kg bis 16 mg/kg für MOAH getestet.
Nach den Ringversuchsergebnissen hat sich das Verfahren bei Massenkonzentrationen an MOSH und MOAH von jeweils über 10 mg/kg als geeignet erwiesen. Das Verfahren wurde jedoch während der gemeinsamen Studie für die Probe einer Vormischung wegen zu geringer MOSH und MOAH Konzentrationen nicht vollständig validiert. Außerdem wurde das Verfahren während der gemeinsamen Studie für die Sonnenblumenkern-Probe wegen einer zu geringen MOAH Konzentration nicht vollständig validiert.
ANMERKUNG 2 Die Schlussfolgerungen in Bezug auf MOAH basieren auf 4 Analyt /Matrix Kombinationen, während das IUPAC-Protokoll [4] mindestens 5 erwartet.
Wenn Störungen durch natürliche Quellen vermutet werden, kann die fossile Herkunft der MOSH- und MOAH-Fraktion durch Untersuchung des chromatographischen Profils mit GC-MS verifiziert werden.
Für die Bestimmung von MOSH und MOAH in essbaren Fetten und Ölen steht auch eine andere Norm zur Verfügung: EN 16995. Weitere Informationen siehe [5].
In Anhang C wird ein manuelles Alternativverfahren zur Online-HPLC-GC-FID-Analyse vorgeschlagen, das als Screening-Verfahren für die Bestimmung von MOSH verwendet werden kann.
Aliments pour animaux : Méthodes d’échantillonnage et d’analyse - Détermination des hydrocarbures saturés d’huile minérale (MOSH) et des hydrocarbures aromatiques d’huile minérale (MOAH) par analyse CLHP CG-FID en ligne
Le présent document décrit une méthode de détermination des hydrocarbures saturés et aromatiques (de C10 à C50) présents dans les aliments composés pour animaux. La méthode a fait l’objet d’une validation interlaboratoires par une analyse CLHP CG FID en ligne ; voir [1], [2] et [3]. La présente méthode n’est pas destinée à être appliquée à d’autres matrices.
La méthode peut être employée pour l’analyse des hydrocarbures saturés d’huile minérale (MOSH) et/ou des hydrocarbures aromatiques d’huile minérale (MOAH).
La méthode est applicable aux matières premières pour aliments des animaux, notamment les huiles végétales et autres matières riches en matière grasse, aux aliments composés et aux prémélanges. Elle n’est pas applicable aux additifs et aux distillats de désodorisation.
NOTE 1 Cette méthode n’a pas été conçue pour les matrices encapsulées.
Cette méthode a été soumise à essai lors d’une étude interlaboratoires en procédant à l’analyse d’échantillons naturellement contaminés et dopés (prémélange, farine de soja, graines de tournesol, aliments pour volailles, aliments pour porcs, huile végétale) à des teneurs comprises entre 3 mg/kg et 286 mg/kg pour les MOSH et entre 1 mg/kg et 16 mg/kg pour les MOAH.
D’après les résultats de l’étude interlaboratoires, il a été démontré que la méthode est adaptée pour les concentrations massiques des MOSH et des MOAH, au dessus de 10 mg/kg chacune. Toutefois, la méthode n’a pas été entièrement validée lors de l’étude interlaboratoires pour l’échantillon de prémélange en raison des concentrations trop faibles des MOSH et MOAH. La méthode n’a pas non plus été entièrement validée lors de l’étude interlaboratoires pour l’échantillon de graines de tournesol en raison de la concentration trop faible des MOAH.
NOTE 2 Les conclusions concernant les MOAH se fondent sur quatre combinaisons analytes/matrice, alors que le protocole IUPAC [4] prévoit un minimum de cinq combinaisons.
En cas de suspicion d’interférences dues à des sources naturelles, l’origine fossile de la fraction des MOSH et des MOAH peut être vérifiée par un examen du profil par CG SM.
Une autre norme CEN est également disponible dans le cadre de la détermination des MOSH et MOAH dans les huiles et graisses alimentaires : l’EN 16995. Pour plus d’informations, voir [5].
L’Annexe C propose une méthode manuelle alternative pour l’analyse CLHP CG FID en ligne qui peut être utilisée en tant que méthode de criblage pour la détermination des MOSH.
Krma: metode vzorčenja in analize - Določevanje nasičenih ogljikovodikov iz mineralnih olj (MOSH) in aromatskih ogljikovodikov iz mineralnih olj (MOAH) z analizo on-line HPLC-GC-FID
Ta dokument določa metodo za določevanje nasičenih in aromatskih ogljikovodikov (od C10 do C50) v krmi. Metoda je bila potrjena v medlaboratorijski študiji z analizo on-line HPLC-GC-FID – glej točke [1], [2] in [3]. Ta metoda ni namenjena za uporabo pri drugih matrikah.
Metodo je mogoče uporabiti za analizo nasičenih ogljikovodikov iz mineralnih olj (MOSH) in/ali aromatskih ogljikovodikov iz mineralnih olj (MOAH).
Metoda se uporablja za sestavine krme, zlasti rastlinska olja in druge sestavine krme, bogate z maščobami, krmne mešanice in premikse. Ne uporablja se za aditive ali deodestilate.
Ta metoda je bila preskušena v medlaboratorijski študiji z analizo naravno kontaminiranih in primešanih vzorcev (premiks, sojina moka, sončnična semena, krma za perutnino, krma za prašiče, rastlinsko olje) v razponu 3–286 mg/kg za nasičene ogljikovodike iz mineralnih olj in 1–16 mg/kg za aromatske ogljikovodike iz mineralnih olj.
Glede na rezultate medlaboratorijske študije je metoda dokazano primerna za masne koncentracije nasičenih ogljikovodikov iz mineralnih olj in aromatskih ogljikovodikov iz mineralnih olj nad 10 mg/kg. Vendar pa metoda med sodelovalno študijo za vzorec premiksa ni bila v celoti potrjena zaradi prenizkih koncentracij nasičenih ogljikovodikov iz mineralnih olj in aromatskih ogljikovodikov iz mineralnih olj. Metoda tudi ni bila v celoti potrjena med sodelovalno študijo za vzorec sončničnih semen zaradi prenizke koncentracije aromatskih ogljikovodikov iz mineralnih olj.
OPOMBA: Ugotovitve glede aromatskih ogljikovodikov iz mineralnih olj temeljijo na štirih kombinacijah analit/matrika, medtem ko se v skladu s protokolom UPAC [4] pričakuje najmanj pet kombinacij.
V primeru domnevnih motenj iz naravnih virov je mogoče fosilni izvor deleža nasičenih ogljikovodikov iz mineralnih olj in aromatskih ogljikovodikov iz mineralnih olj potrditi s pregledom vzorca z metodo GC-MS.
Za določevanje nasičenih ogljikovodikov iz mineralnih olj in aromatskih ogljikovodikov iz mineralnih olj v jedilnih maščobah in oljih je na voljo dodaten standard CEN: EN 16995. Za več informacij glej točko [5].
V dodatku C je predlagana alternativna metoda analizi on-line HPLC-GC-FID, ki jo je mogoče uporabiti kot presejalno metodo.
General Information
Standards Content (Sample)
SLOVENSKI STANDARD
01-januar-2022
Krma: metode vzorčenja in analize - Določevanje nasičenih ogljikovodikov iz
mineralnih olj (MOSH) in aromatskih ogljikovodikov iz mineralnih olj (MOAH) z
analizo on-line HPLC-GC-FID
Animal feeding stuffs: Methods of sampling and analysis - Determination of mineral oil
saturated hydrocarbons (MOSH) and mineral oil aromatic hydrocarbons (MOAH) with
on-line HPLC-GC-FID analysis
Futtermittel: Probenahme- und Untersuchungsverfahren - Bestimmung von
mineralölgesättigten Kohlenwasserstoffen (MOSH) und mineralölaromatischen
Kohlenwasserstoffen (MOAH) mit Online-Analyse durch HPLC-GC-FID
Aliments pour animaux : Méthodes d’échantillonnage et d’analyse - Détermination des
hydrocarbures saturés d’huile minérale (MOSH) et des hydrocarbures aromatiques
d’huile minérale (MOAH) par analyse CLHP CG-FID en ligne
Ta slovenski standard je istoveten z: EN 17517:2021
ICS:
65.120 Krmila Animal feeding stuffs
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
EN 17517
EUROPEAN STANDARD
NORME EUROPÉENNE
October 2021
EUROPÄISCHE NORM
ICS 65.120
English Version
Animal feeding stuffs: Methods of sampling and analysis -
Determination of mineral oil saturated hydrocarbons
(MOSH) and mineral oil aromatic hydrocarbons (MOAH)
with on-line HPLC-GC-FID analysis
Aliments pour animaux : Méthodes d'échantillonnage Futtermittel: Probenahme und
et d'analyse - Détermination des hydrocarbures Untersuchungsverfahren - Bestimmung von
saturés d'huile minérale (MOSH) et des hydrocarbures mineralölgesättigten Kohlenwasserstoffen (MOSH) und
aromatiques d'huile minérale (MOAH) par analyse mineralölaromatischen Kohlenwasserstoffen (MOAH)
CLHP CG-FID en ligne mit Online Analyse durch HPLC GC FID
This European Standard was approved by CEN on 2 August 2021.
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-CENELEC 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-CENELEC Management
Centre has the same status as the official versions.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,
Poland, Portugal, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and
United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2021 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 17517:2021 E
worldwide for CEN national Members.
Contents Page
European foreword . 3
Introduction . 4
1 Scope . 5
2 Normative references . 5
3 Terms and definitions . 5
4 Principle . 6
5 Reagents . 6
6 Apparatus . 9
7 Sampling . 10
8 Preparation of the test sample . 10
9 Preparation of the analytical sample . 10
9.1 Fat extraction from feed sample . 10
9.2 Procedure for fats and fat extracts . 11
9.3 Blank . 11
10 Liquid chromatography and gas chromatography . 12
10.1 Liquid chromatography setup . 12
10.2 Working conditions for HPLC . 12
10.3 HPLC-GC-interface . 13
10.4 Gas chromatography setup . 14
10.5 Working conditions for GC . 14
10.6 Solvent vapor exit . 15
10.7 Peak identification . 15
10.8 Performance of the HPLC-GC system. 15
10.9 Quantitative determination of hydrocarbons attributed to mineral oil origin . 16
11 Precision . 17
11.1 Interlaboratory test . 17
11.2 Repeatability . 17
11.3 Reproducibility . 17
12 Test report . 17
Annex A (informative) Examples of chromatograms . 19
Annex B (informative) Precision data. 25
Annex C (informative) Determination of saturated hydrocarbons of mineral oil - Manual
alternative method to on line HPLC-GC-FID analysis . 28
Bibliography . 40
European foreword
This document (EN 17517:2021) has been prepared by Technical Committee CEN/TC 327 “Animal
feeding stuffs - Methods of sampling and analysis”, the secretariat of which is held by NEN.
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 April 2022, and conflicting national standards shall be
withdrawn at the latest by April 2022.
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CEN shall not be held responsible for identifying any or all such patent rights.
This document has been prepared under a standardization request given to CEN by the European
Commission and the European Free Trade Association.
Any feedback and questions on this document should be directed to the users’ national standards body.
A complete listing of these bodies can be found on the CEN website.
According to the CEN-CENELEC Internal Regulations, the national standards organisations of the
following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia,
Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland,
Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Republic of North
Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United
Kingdom.
Introduction
WARNING — The method described in this document implies the use of reagents that pose a hazard to
health. This document does not claim to address all associated safety problems. It is the responsibility of
the user of this document to take appropriate measures for the health and safety protection of the
personnel prior to use of the standard and to ensure that regulatory and legal requirements are complied
with.
1 Scope
This document specifies a method for the determination of saturated and aromatic hydrocarbons (from
C10 to C50) in feed. The method has been interlaboratory validated with on-line-HPLC-GC-FID – see [1],
[2] and [3]. This method is not intended to be applied to other matrices.
The method can be used for the analysis of mineral oil saturated hydrocarbons (MOSH) and/or mineral
oil aromatic hydrocarbons (MOAH).
The method is applicable for feed materials, in particular vegetable oils and other fat rich feed materials,
compound feeds and pre-mixtures. It is not applicable to additives or deodistillates.
NOTE 1 The method was not designed for encapsulated matrices.
The method has been tested in an interlaboratory study via the analysis of both naturally contaminated
and spiked samples (pre-mixture, soybean meal, sunflower seeds, chicken feed, pig feed, vegetable oil)
ranging from 3 mg/kg to 286 mg/kg for MOSH and from 1 mg/kg to 16 mg/kg for MOAH.
According to the results of the interlaboratory study, the method has been proven suitable for MOSH and
MOAH mass concentrations, each above 10 mg/kg. However, the method was not fully validated during
the collaborative study for the premixture sample due to too low concentrations of MOSH and MOAH. The
method was also not fully validated during the collaborative study for the sunflower seeds sample due to
a too low concentration of MOAH.
NOTE 2 The conclusions regarding MOAH are based on 4 analyte / matrix combinations while the IUPAC
protocol [4] expects this to be a minimum of 5.
In case of suspected interferences from natural sources, the fossil origin of the MOSH and MOAH fraction
can be verified by examination of the pattern by GC-MS.
For the determination of MOSH and MOAH in edible fats and oils, another CEN standard is also available:
EN 16995. For more information see [5].
Annex C proposes a manual alternative method to on-line HPLC-GC-FID analysis that can be used as a
screening method for the determination of MOSH.
2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements 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.
EN ISO 6498, Animal feeding stuffs - Guidelines for sample preparation (ISO 6498)
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https://www.iso.org/obp
— IEC Electropedia: available at https://www.electropedia.org/
3.1
mineral oil saturated hydrocarbons
MOSH
paraffinic (open-chain, usually branched) and naphthenic (cyclic, alkylated) hydrocarbons
3.2
mineral oil aromatic hydrocarbons
MOAH
aromatic mainly alkylated hydrocarbons
3.3
unresolved complex mixture
UCM
complex mixture of saturated or aromatic hydrocarbons not resolved by gas chromatography such as
branched paraffins, alkylated naphthenes and alkylated aromatics
4 Principle
The fatty material is extracted from the commodity using organic solvent. After concentration of part of
the solvent, the extract is submitted to an epoxidation step. The fractions of MOSH and MOAH are isolated
and separated by an HPLC-GC-FID system. MOSH and MOAH fractions are separated on a silica gel column
using an n-hexane/dichloromethane gradient and each transferred as 450 µl fractions to GC using the Y-
interface [6], while triglycerides are kept on the HPLC column. Solvent vapours are discharged via a
solvent vapour exit located between the uncoate
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.