EN 16619:2015
(Main)Food analysis - Determination of benzo[a]pyrene, benz[a]anthracene, chrysene and benzo[b]fluoranthene in foodstuffs by gas chromatography mass spectrometry (GC-MS)
Food analysis - Determination of benzo[a]pyrene, benz[a]anthracene, chrysene and benzo[b]fluoranthene in foodstuffs by gas chromatography mass spectrometry (GC-MS)
This European Standard specifies a method for the determination of 4 of the 16 EU priority polycyclic aromatic hydrocarbons (PAHs), identified as target PAHs. They are benz[a]anthracene (BaA), benzo[a]pyrene (BaP), benzo[b]fluoranthene (BbF) and chrysene (CHR). The method allows their quantification in the presence of the other 12 EU priority PAHs (benzo[j]fluoranthene (BjF), cyclopenta[cd]pyrene (CPP), benzo[k]fluoranthene (BkF), dibenz[a,h]anthracene (DhA), benzo[c]fluorene (BcL), dibenzo[a,e]pyrene (DeP), benzo[ghi]perylene (BgP), dibenzo[a,h]pyrene (DhP), dibenzo[a,i]pyrene (DiP), dibenzo[a,l]pyrene (DlP), indeno[1,2,3-cd]pyrene (IcP), 5-methylchrysene (5MC)) in extruded wheat flour, smoked fish, dry infant formula, sausage meat, freeze-dried mussels, edible oil and wheat flour, by gas-chromatography mass-spectrometry (GC-MS). The extraction of PAHs from solid samples is performed by pressurized liquid extraction (PLE). Soxhlet extraction was applied by some participants in the validation study by collaborative trial as alternative to PLE. The sample cleanup is performed by applying the following techniques in the reported sequence: size exclusion chromatography (SEC), and solid phase extraction (SPE).
This method complies with the performance characteristics specified in Commission Regulation (EU) No 836/2011 (see [1]). In particular the specifications for the limit of detection (LOD) and of the limit of quantification (LOQ) (0,30 µg/kg and 0,90 µg/kg respectively) were met.
The method has been validated in an interlaboratory study via the analysis of both naturally contaminated and spiked samples, ranging from 0,5 µg/kg to 11,9 µg/kg. However, linearity of the instrument response was proven for the concentration range 0,5 µg/kg to 20 µg/kg.
For the determination of PAHs in edible fats and oils, two other CEN standards are also available, EN ISO 22959 and EN ISO 15753, for more information see [2] and [3].
Lebensmittelanalytik - Bestimmung von Benzo[a]pyren, Benz[a]anthracen, Chrysen und Benzo[b]fluoranthen in Lebensmitteln mit Gaschromatographie und Massenspektrometrie (GC-MS)
Diese Europäische Norm legt ein Verfahren zur Bestimmung von 4 der 16 von der EU als prioritär eingestuften polyzyklischen aromatischen Kohlenwasserstoffe (PAK) fest, die als Ziel PAK bezeichnet werden. Diese Verbindungen sind Benz[a]anthracen (BaA), Benzo[a]pyren (BaP), Benzo[b]fluoranthen (BbF) und Chrysen (CHR). Das Verfahren ermöglicht deren quantitative Bestimmung in Gegenwart der anderen 12 von der EU als prioritär eingestuften PAK (Benzo[j]fluoranthen (BjF), Cyclopenta[cd]pyren (CPP), Benzo[k]fluoranthen (BkF), Dibenz[a,h]anthracen (DhA), Benzo[c]fluoren (BcL), Dibenzo[a,e]pyren (DeP), Benzo[ghi]perylen (BgP), Dibenzo[a,h]pyren (DhP), Dibenzo[a,i]pyren (DiP), Dibenzo[a,l]pyren (DlP), Indeno[1,2,3 cd]pyren (IcP), 5 Methylchrysen (5MC)) in extrudiertem Weizenmehl, geräuchertem Fisch, pulverförmiger Babynahrung, Wurstbrät, gefriergetrockneten Muscheln, Speiseöl und Weizenmehl mittels Gaschromatographie-Massenspektrometrie (GC MS). Die Extraktion von PAK aus festen Proben erfolgt durch beschleunigte Lösemittelextraktion (en: pressurized liquid extraction, PLE). Als Alternative zur PLE wurde von einigen Teilnehmern der Methodenvalidierungsstudie durch einen Ringversuch (im Folgenden: Ringversuch) die Soxhlet-Extraktion angewendet. Die Probe wird mit einer der folgenden Techniken in der angegebenen Reihenfolge gereinigt: Größenausschlusschromatographie (en: size exclusion chromatography, SEC) und Festphasenextraktion (en: solid phase extraction, SPE).
Dieses Verfahren entspricht den in der Verordnung (EU) Nr. 836/2011 der Kommission (siehe [1]) festgelegten Leistungskenngrößen. Insbesondere die Festlegungen für die Nachweisgrenze (en: limit of detection, LOD) und die Bestimmungsgrenze (en: limit of quantification, LOQ) (0,30 µg/kg bzw. 0,90 µg/kg) wurden erfüllt.
Das Verfahren wurde in einem Ringversuch durch die Analyse sowohl natürlich kontaminierter als auch aufgestockter Proben im Bereich von 0,5 µg/kg bis 11,9 µg/kg validiert. Die Linearität des Ansprechverhaltens des Gerätes wurde jedoch für den Konzentrationsbereich von 0,5 µg/kg bis 20 µg/kg nachgewiesen.
Zur Bestimmung von PAK in Speisefetten und ölen stehen auch zwei andere Normen zur Verfügung, EN ISO 22959 und EN ISO 15753, hinsichtlich weiterführender Informationen siehe [2] und [3].
Analyse des produits alimentaires - Dosage du benzo(a)pyrène, benzo(a)anthracène, chrysène et benzo(b)fluoranthène dans les denrées alimentaires par chromatographie en phase gazeuse couplée à la spectrométrie de masse (CG-SM)
La présente Norme européenne spécifie une méthode de dosage de 4 des 16 hydrocarbures aromatiques polycycliques (HAP) prioritaires de l'UE, identifiés comme HAP cibles : le benzo[a]anthracène (BaA), le benzo[a]pyrène (BaP), le benzo[b]fluoranthène (BbF) et le chrysène (CHR). La méthode permet de quantifier la présence des 12 autres HAP prioritaires de l'UE (benzo[j]fluoranthène (BjF), cyclopenta[cd]pyrène (CPP), benzo[k]fluoranthène (BkF), dibenz[a,h]anthracène (DhA), benzo[c]fluorène (BcL), dibenzo[a,e]pyrène (DeP), benzo[ghi]pérylène (BgP), dibenzo[a,h]pyrène (DhP), dibenzo[a,i]pyrène (DiP), dibenzo[a,l]pyrène (DlP), indéno[1,2,3-cd]pyrène (IcP), 5-méthylchrysène (5MC)) dans la farine de blé extrudée, le poisson fumé, les laits infantiles en poudre, la chair à saucisse, les moules lyophilisées, les huiles alimentaires et la farine de blé, par chromatographie en phase gazeuse couplée à la spectrométrie de masse (CG-SM). Pour les échantillons solides, l'extraction des HAP est effectuée par extraction liquide sous pression (PLE). L’extraction Soxhlet a été appliquée par certains participants lors de l’étude de validation par l’essai interlaboratoires pour remplacer la PLE. La purification de l'échantillon est effectuée en appliquant les techniques suivantes dans l'ordre indiqué : chromatographie d'exclusion stérique (SEC) et extraction en phase solide (SPE).
Cette méthode est conforme aux caractéristiques de performance spécifiées dans le Règlement (UE) n° 836/2011 de la Commission (voir [1]). En particulier, les exigences relatives à la limite de détection (LOD) et à la limite de quantification (LOQ) (0,30 µg/kg et 0,90 µg/kg respectivement) ont été remplies.
La méthode a été validée lors d'un essai interlaboratoires impliquant l’analyse d’échantillons naturellement contaminés et d’échantillons enrichis, sur un intervalle de concentrations de 0,5 µg/kg à 11,9 µg/kg. Toutefois, la linéarité de la réponse de l'instrument a été démontrée pour la gamme de concentrations de 0,5 µg/kg à 20 µg/kg.
Pour doser les HAP dans les corps gras alimentaires, deux autres normes CEN sont également disponibles, l'EN ISO 22959 et l'EN ISO 15753, pour plus d'informations voir [2] et [3].
Analize živil - Določevanje benzo(a)pirena, benz(a)antracena, krizena in benzo(b)fluorantena v živilih s plinsko kromatografijo z masno spektrometrijo (GS-MS)
General Information
Standards Content (Sample)
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Lebensmittelanalytik - Bestimmung von Benzo[a]pyren, Benz[a]anthracen, Chrysen und Benzo[b]fluoranthen in Lebensmitteln mit Gaschromatographie und Massenspektrometrie (GC-MS)Analyse des produits alimentaires
- Dosage du benzo(a)pyrène, benzo(a)anthracène, chrysène et benzo(b)fluoranthène dans les denrées alimentaires par chromatographie en phase gazeuse couplée à la spectrométrie de masse (CG-SM)Food analysis - Determination of benzo[a]pyrene, benz[a]anthracene, chrysene and benzo[b]fluoranthene in foodstuffs by gas chromatography mass spectrometry (GC-MS)67.050Splošne preskusne in analizne metode za živilske proizvodeGeneral methods of tests and analysis for food productsICS:Ta slovenski standard je istoveten z:EN 16619:2015SIST EN 16619:2015en,fr,de01-julij-2015SIST EN 16619:2015SLOVENSKI
STANDARD
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 16619
April 2015 ICS 67.050 English Version
Food analysis - Determination of benzo[a]pyrene, benz[a]anthracene, chrysene and benzo[b]fluoranthene in foodstuffs by gas chromatography mass spectrometry (GC-MS) Analyse des produits alimentaires
- Dosage du benzo(a)pyrène, benzo(a)anthracène, chrysène et benzo(b)fluoranthène dans les denrées alimentaires par chromatographie en phase gazeuse couplée à la spectrométrie de masse (CG-SM)
Lebensmittelanalytik - Bestimmung von Benzo[a]pyren, Benz[a]anthracen, Chrysen und Benzo[b]fluoranthen in Lebensmitteln mit Gaschromatographie und Massenspektrometrie (GC-MS) This European Standard was approved by CEN on 7 February 2015.
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, Former Yugoslav Republic of Macedonia, 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
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B-1000 Brussels © 2015 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 16619:2015 ESIST EN 16619:2015
Typical chromatograms . 28 Annex B (informative)
Precision data . 30 Annex C (informative)
Precision data from single laboratory validation . 35 Bibliography . 37
SEC fraction. The SEC fraction is evaporated to about 200 µl, and cleaned up by SPE on silica, using cyclohexane as eluent. The cleaned up sample extract is evaporated again to about 200 µl. Finally, an injection standard solution is added to the sample prior to measurement by GC-MS. The injection is performed with a PTV, or split/splitless injection port. The chromatographic separation is obtained on a mid-polar capillary column with high selectivity for PAHs. The analytes are ionised by electron ionization (EI) at 70 eV. The target PAHs are recorded in Single Ion Monitoring (SIM) mode, and quantified by comparison with the stable isotope labelled analogues. SIST EN 16619:2015
density (in g/ml); m measured mass of the substance (in g); v volume of the solution (in ml). The density of toluene at 20 °C is 0,8669 g/ml. Comprehensive information on the density of solvents at various temperatures is given in [4]. All solutions and substances are used at room temperature. WARNING 1 — Some PAHs are considered carcinogenic. Persons using this document should be familiar with normal laboratory practices. It is the responsibility of the user of this document to apply practices which are in agreement with applicable occupational safety and health practices. WARNING 2 — Dispose chemical waste according to applicable environmental rules and regulations. WARNING 3 — PAHs are degraded by UV light. Protect PAHs solutions from light (keep in the dark, use aluminium foil or amber glassware). WARNING 4 — Some precaution is needed when using plastics as polypropylene or PTFE because the analytes may be absorbed onto these materials. 4.2 Helium purified compressed gas (purity equivalent to 99,995 % or better). 4.3 Nitrogen purified compressed gas (purity equivalent to 99,995 % or better). 4.4 Disodium sulfate, (Na2SO4), anhydrous, granular. 4.5 Poly(acrylic acid), partial sodium salt-graft-poly(ethylene oxide) granular, 90
size. 4.6 Sand, 50 mesh to 70 mesh particle size. 4.7 n-Hexane. SIST EN 16619:2015
Commercial SPE columns made of polypropylene were used in the method validation study by collaborative trial. 4.14 Reference material for quality control A certified reference material, or any other suitable quality control material (e.g left over proficiency test material) may be applied for this purpose. The CITAC/Eurachem Guide to Quality in Analytical Chemistry may be consulted for guidance, see [5]. Analyse this material with every sample batch and use it to control the method performances along time (see 10.4). 4.15 Native reference substances - commercially available neat material or solutions of PAHs The list of native substances analysed with this method is provided in Table 1. The target analytes are given in bold font. Commercially available, preferably certified, standard solutions are preferred due to the higher level of safety in handling. Triphenylene, benzo[j]fluoranthene, and benzo[k]fluoranthene are potentially interfering with the target analytes and are therefore used for evaluation of selectivity. SIST EN 16619:2015
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