EN 16215:2012
(Main)Animal feeding stuffs - Determination of dioxins and dioxin-like PCBs by GC/HRMS and of indicator PCBs by GC/HRMS
Animal feeding stuffs - Determination of dioxins and dioxin-like PCBs by GC/HRMS and of indicator PCBs by GC/HRMS
This European Standard is applicable to the determination of polychlorinated dibenzo-p-dioxins (PCDDs), polychlorinated dibenzofurans (PCDFs), (together termed ‘dioxins’ (PCDD/Fs)) and dioxin-like PCBs and non dioxin-like PCBs (dl-PCBs and ndl-PCBs) in animal feeding stuffs. Collaborative studies have been carried out. The method is suitable for the determination of dioxins, dl-PCBs and ndl-PCBs at the appropriate MRL in compound feed and ingredients e.g. oil, mineral clay. The method is applicable to samples containing residues of one or more of the following dioxins, dioxin-like PCBs and indicator PCBs. The limit of quantification (LOQ) for the relevant individual congeners of dioxins/furans is 0,05 pg/g (OCDD/F = 0,1 pg/g), of non-ortho PCBs 0,05 pg/g, of mono-ortho PCBs 10 pg/g and of indicator PCBs 100 pg/g.
For determination of dioxins and dioxin-like PCBs, the procedure can be used as confirmatory method as defined by Commission Regulation (EC) No 152/2009 for dioxins and dl-PCB in feed [1]. Confirmatory methods are high-resolution gas chromatography/high resolution mass spectrometry (HRGC/HRMS) methods. If only the analysis of indicator PCBs is required, a GC-LRMS method can be used (e.g. EN 15741 Animal feeding stuffs - Determination of OC-pesticides and PCBs by GC/MS [7] and EN 15742 Animal feeding stuffs - Determination of OC-pesticides and PCBs by GC/ECD [8]) provided that appropriate analytical performance criteria are met in the relevant range for the matrix of interest.
This European Standard is split into four modules each describing a part of the whole procedure (see Figure 1 and Figure 2) to be followed:
a) Module A: Description of standards which might be used;
b) Module B: Description of extraction procedures;
c) Module C: Description of clean up procedures;
d) Module D: GC/HRMS determination.
Each module describes a part of the whole method as well as, when applicable, alternatives which should be equivalent. Each module has to be regarded as an example. Combining modules and/or alternatives gives a highly flexible procedure which is "performance based". It is permitted to modify the method if all performance criteria laid down in Commission Regulation (EC) No 152/2009 [1] are met.
Any deviation of the described method, combination of modules needs to be recorded as part of the QA/QC procedures of accredited laboratories and should be available on request.
Futtermittel - Bestimmung von Dioxinen und dioxin-ähnlichen PCBs mittels GC/HRMS und von Indikator-PCBs mittels GC/HRMS
Diese Europäische Norm ist anwendbar für die Bestimmung von polychlorierten Dibenzo-p-dioxinen (PCDD), polychlorierten Dibenzofuranen (PCDF) [zusammen als „Dioxine“ bezeichnet (PCDD/F)] und dioxin-ähnlicher PCBs und nicht dioxin ähnlicher PCBs (dl-PCB und ndl-PCB) in Futtermitteln. Ringversuche wurden durchgeführt. Das Ver¬fahren ist für die Bestimmung von Dioxinen, dl-PCBs und ndl-PCBs bei der entsprechenden MRL in Mischfutter und Inhaltsstoffen, z. B. Öl, Tonmineral, geeignet. Das Verfahren ist auf Proben anwendbar, die Rückstände von einem oder mehreren der folgenden Dioxine, dioxin-ähnlichen PCBs und Indikator-PCBs enthalten. Die Bestimmungsgrenze (LOQ) beträgt für die relevanten einzelnen Kongeneren der Dioxine/Furane 0,05 pg/g (OCDD/F 0,1 pg/g), für non-ortho PCBs 0,05 pg/g, für mono-ortho PCBs 10 pg/g und 100 pg/g für Indikator PCBs.
Für die Bestimmung von Dioxinen und dioxin-ähnlichen PCB kann das Verfahren, wie in der Kommissions-Verordnung (EG) Nr. 152/2009 für Dioxine und dl-PCB in Futtermitteln [6] festgelegt, als Bestätigungs-verfahren angewendet werden. Die Bestätigungsverfahren sind Verfahren mit hochauflösender Gaschromatographie/hochauf¬lösender Massenspektrometrie (HRGC/HRMS). Ist nur die Analyse der Indikator-PCBs erforderlich, kann ein GC/LRMS Verfahren (z. B. EN 15741, Futtermittel — Bestimmung der OC-Pestizide und PCBs mittels GC/MS-Verfahren [1] und EN 15742, Futtermittel — Bestimmung der OC-Pestizide und PCBs mittels GC/ECD Verfahren [2]) angewendet werden, vorausgesetzt, dass für die zu untersuchende Matrix im relevanten Bereich die entsprechenden analytischen Leistungskriterien erfüllt werden.
Diese Europäische Norm ist in vier Module aufgeteilt, die jeweils einen Teil des gesamten Verfahrens (siehe Bild 1 und Bild 2) wie folgt beschreiben:
a) Modul A: Beschreibung der Normen, die angewendet werden können;
b) Modul B: Beschreibung der Extraktionsverfahren;
c) Modul C: Beschreibung der Reinigungsverfahren;
d) Modul D: GC/HRMS Bestimmung.
Jedes Modul beschreibt einen Teil des gesamten Verfahrens sowie, falls anwendbar, Alternativen, die gleich-wertig sein sollten. Jedes Modul muss als ein Beispiel betrachtet werden. Kombinierbare Module und/oder Alternativen ergeben ein hochflexibles Verfahren, das „leistungsbezogen“ ist. Es ist zulässig, das Verfahren zu verändern, wenn sämtliche Leistungskriterien entsprechend der Kommissions-Verordnung (EG) Nr. 152/2009 [6] erfüllt werden.
Jede Abweichung vom beschriebenen Verfahren und die Kombination der Module müssen als Teil der QA/QC Verfahren von anerkannten Laboratorien aufgezeichnet werden und sollten auf Anfrage verfügbar sein.
Aliments des animaux - Dosage des dioxines, des PCB de type dioxine et des PCB indicateurs par GC/HRMS
La présente Norme européenne concerne le dosage des dibenzo-p-dioxines polychlorés (PCDD), des dibenzofuranes polychlorés (PCDF) (conjointement appelés 'dioxines' (PCDD/F)) ainsi que des PCB de type dioxine et des PCB autres que ceux de type dioxine (dl-PCB et ndl-PCB) dans les aliments des animaux. Des études comparatives ont été menées. La méthode convient au dosage des dioxines, des dl-PCB et des ndl-PCB à la LMR appropriée dans les aliments et les ingrédients composés tels que l'huile et l'argile minérale. La méthode est applicable aux échantillons contenant des résidus de dioxines, PCB de type dioxine et/ou PCB indicateurs. La limite de quantification (LOQ) est de 0,05 pg/g (OCDD/F = 0,1 pg/g) pour les congénères individuels concernés des dioxines/furanes, de 0,05 pg/g pour les PCB non-ortho, de 10 pg/g pour les PCB mono-ortho et de 100 pg/g pour les PCB indicateurs.
Pour le dosage des dioxines et des PCB de type dioxine, le mode opératoire peut être utilisé comme méthode de confirmation, conformément aux définitions du Réglement (CE) n° 152/2009 de la Commission relatif aux dioxines et aux dl-PCB dans les aliments [6]. Les méthodes de confirmation sont les méthodes de chromatographie en phase gazeuse haute résolution/spectrométrie de masse haute résolution (HRGC/HRMS). Si seule l'analyse des PCB indicateurs est requise, une méthode GC-LRMS peut être utilisée (par exemple, EN 15741, Aliments des animaux - Détermination des pesticides organochlorés (OC) et des polychlorobiphényles (PCB) par GC/MS [1] et EN 15742, Aliments des animaux - Détermination des pesticides organochlorés (OC) et des polychlorobiphényles (PCB) par GC/ECD [2] à condition que les critères de performance analytique appropriés soient atteints dans la gamme de concentration correspondant aux aliments concernés.
La présente Norme européenne se divise en quatre modules, chacun décrivant une partie de l'ensemble du mode opératoire (voir les Figures 1 et 2) à respecter :
a) Module A : Description des normes susceptibles d'être utilisées ;
b) Module B : Description des modes opératoires d'extraction ;
c) Module C : Description des modes opératoires de purification ;
d) Module D : Dosage par GC/HRMS.
Chaque module décrit une partie de l'ensemble de la méthode ainsi que, le cas échéant, des alternatives équivalentes. Chaque module doit être considéré comme un exemple. La combinaison des modules et/ou alternatives donne un mode opératoire très souple qui est « basé sur les performances ». Il est possible de modifier la méthode si tous les critères de performance énoncés dans le Règlement (CE) n° 152/2009 de la Commission [6] sont remplis.
En cas d'écart par rapport à la méthode décrite, la combinaison de modules doit être enregistrée dans le cadre des procédures AQ/CQ des laboratoires accrédités et il convient que cette combinaison soit disponible sur demande.
Krma - Določevanje dioksinov in dioksinu podobnih PCB z GC/HRMS in indikatorjev PCB z GC/HRMS
Ta evropski standard se uporablja za določevanje polikloriranih dibenzo-p-dioksinov (PCDD), polikloriranih dibenzofuranov (PCDF) (s skupnim imenom »dioksini« (PCDD/F)) ter dioksinom podobnih polikloriranih bifenilov in dioksinom nepodobnih polikloriranih bifenilov (dl-PCBs in ndl-PCBs) v živalski krmi. Izvedene so bile medlaboratorijske študije. Metoda je primerna za določevanje dioksinov, dioksinom podobnih polikloriranih bifenilov in dioksinom nepodobnih polikloriranih bifenilov v krmi in sestavinah, na primer olju ter mineralni glini, pri ustrezni mejni vrednosti ostankov. Metoda se uporablja za vzorce, ki vsebujejo ostanke enega ali več naslednjih dioksinov, dioksinom podobnih polikloriranih bifenilov ter indikatorskih polikloriranih bifenilov. Meja kvantifikacije (LOQ) za ustrezne posamezne analoge dioksinov/furanov je 0,05 pg/g (OCDD/F = 0,1 pg/g), za neorto poliklorirane bifenile 0,05 pg/g, za monoorto poliklorirane bifenile 10 pg/g, za indikatorske poliklorirane bifenile pa 100 pg/g.
General Information
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Standards Content (Sample)
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.QFuttermittel - Bestimmung von Dioxinen und dioxin-ähnlichen PCBs mittels GC/HRMS und von Indikator-PCBs mittels GC/HRMSAnimal feed - Determination of dioxins and dioxin-like PCBs by GC/HRMS and of indicator PCBs by GC/HRMS65.120KrmilaAnimal feeding stuffsICS:Ta slovenski standard je istoveten z:EN 16215:2012SIST EN 16215:2012en,fr,de01-september-2012SIST EN 16215:2012SLOVENSKI
STANDARD
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 16215
April 2012 ICS 65.120 English Version
Animal feeding stuffs - Determination of dioxins and dioxin-like PCBs by GC/HRMS and of indicator PCBs by GC/HRMS
Aliments des animaux - Dosage des dioxines, des PCB de type dioxine et des PCB indicateurs par GC/HRMS
Futtermittel - Bestimmung von Dioxinen und dioxin-ähnlichen PCBs mittels GC/HRMS und von Indikator-PCBs mittels GC/HRMS This European Standard was approved by CEN on 9 March 2012.
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, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre:
Avenue Marnix 17,
B-1000 Brussels © 2012 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 16215:2012: ESIST EN 16215:2012
Description of PTV injection system .37Annex B (informative)
Description of standards and concentration of the standard solutions .39Annex C (informative)
Example of automated procedure .46Annex D (informative)
Mass spectrometer (MS) .48Annex E (informative)
Use of additional clean up after fractionation using a small multi-layer silica column .52Bibliography .53 SIST EN 16215:2012
GC/HRMS determination. Each module describes a part of the whole method as well as, when applicable, alternatives which should be equivalent. Each module has to be regarded as an example. Combining modules and/or alternatives gives a highly flexible procedure which is "performance based". It is permitted to modify the method if all performance criteria laid down in Commission Regulation (EC) No 152/2009 [6] are met. Any deviation of the described method, combination of modules needs to be recorded as part of the QA/QC procedures of accredited laboratories and should be available on request.
= optional Figure 1 — Flow scheme for the determination of Dioxins, dl-PCBs and Indicator PCBs in feed SIST EN 16215:2012
= optional Figure 2 — Flow scheme for the determination of Dioxins, dl-PCBs and Indicator PCBs in oil / fat 2 Normative references The following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. prEN ISO 6498, Animal feeding stuffs
Guidelines for sample preparation (ISO/DIS 6498) 3 Terms and definitions For the purposes of this document, the following terms and definitions apply. 3.1 limit of detection smallest measured content, from which it is possible to deduce the presence of the analyte with reasonable statistical certainty Note 1 to entry: The limit of detection is numerically equal to three times the standard deviation of the mean of blank determinations (n > 10). SIST EN 16215:2012
Quantification is based on isotope dilution. If only indicator PCBs are required, they can be determined with GC-LRMS (e.g. according to EN 15741 Animal feeding stuffs - Determination of OC-pesticides and PCBs by GC/MS [1] and EN 15742 Animal feeding stuffs - Determination of OC-pesticides and PCBs by GC/ECD [2])
Preconditions of combining modules for extraction and clean-up are: a) for each extraction module an equal sample intake of 10 g for feed or feed ingredients with a fat content ≤ 25 % or 2,5 g fat or oil is required; b) in order to achieve the required LOQ for dioxins a final volume of 10 µl in combination with an injection volume of 2 µl is required. If a different injection volume is applied, the final volume has to be adjusted directly proportional. NOTE In case more sensitivity is necessary or less volume reduction is wanted, injection of a larger volume by PTV (an example is described in Annex A) or higher sample intake is possible (see also 9.2.2 NOTE). 5 Reagents Use only reagents of recognized analytical grade and with purity suitable for dioxin and PCB residue analysis. Check the purity of the reagents and reference materials (e.g. standard solutions) by performing a blank test under the same conditions as used in the method. The chromatogram should not show any interfering impurity at the retention time of compounds of interest. SIST EN 16215:2012
6.1 Evaporator, suitable for volumes up to 200 ml and inlet for nitrogen gas. 6.2 Evaporator tubes, endpoint about 0,5 ml. 6.3 Homogeniser 6.4 Pasteur pipette, borosilicate glass, 150 mm. 6.5 Vortexmixer 6.6 Measuring cylinder, borosilicate glass, 100 ml, 2 ml graduations with a precision of ± 0,5 ml. 6.7 Measuring cylinder, borosilicate glass, glass-stoppered, 25 ml, 1 ml graduation with a precision of ± 0,5 ml graduation and 50 ml, 2 ml graduation
with a precision of ± 0,5 ml graduation. 7 Sampling The sample should be truly represe
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