SIST EN 16857:2017
(Main)Foodstuffs - Determination of benzene in soft drinks, other beverages and vegetable-based infant foods by headspace gas chromatography mass spectrometry (HS-GC-MS)
Foodstuffs - Determination of benzene in soft drinks, other beverages and vegetable-based infant foods by headspace gas chromatography mass spectrometry (HS-GC-MS)
This European Standard shall specify a method of analysis for the determination of benzene in soft drinks, juices and baby food. The method should preferably make use of the HS GC-MS technique. The method shall be inter-laboratory validated, in accordance with ISO 5725 or with AOAC International Guidelines for collaborative study procedures to validate characteristics of a method of analysis, using test materials consisting of soft drinks, juices and baby food at appropriate levels.
Lebensmittel - Bestimmung von Benzol in Erfrischungsgetränken, anderen Getränken und in Babynahrung auf Gemüsebasis mit Headspace-Gaschromatographie/Massenspektrometrie (HS-GC-MS)
Diese Europäische Norm legt ein Verfahren zur Bestimmung von Benzol in Erfrischungsgetränken, anderen Getränken und in gemüsehaltiger Babynahrung mit Headspace-Gaschromatographie/Massenspektrometrie (HS-GC-MS) fest. Das Verfahren wurde in einem Ringversuch durch die Analyse von aufgestockten Proben von kohlensäurehaltigen Erfrischungsgetränken, kohlensäurefreien (stillen) Frucht¬saftgetränken, kohlensäurehaltigen Fruchtsaftgetränken, Gemüse- und Fruchtsäften mit Karotten, gemüsehaltiger Babynahrung und fleischhaltiger Babynahrung im Bereich von 1,9 µg/kg bis 18,6 µg/kg validiert. Die Linearität des Ansprechverhaltens des Gerätes wurde jedoch für den Konzentrationsbereich von 0,5 µg/kg bis 20 µg/kg nachgewiesen. Die Bestimmungsgrenze (en: LOQ, limit of quantification) hängt von der Art des Gerätes ab, sie kann aber im Allgemeinen im Bereich von 0,5 µg/kg bis 1,0 µg/kg erwartet werden.
Produits alimentaires - Détermination de la teneur en benzène dans les boissons non alcoolisées, les autres boissons et les aliments pour nourrissons à base de légumes par chromatographie en phase gazeuse avec espace de tête couplée à la spectrométrie de masse (ET CG-SM)
La présente Norme européenne spécifie une méthode de détermination de la teneur en benzène dans les boissons non alcoolisées, les autres boissons et les aliments pour nourrissons à base de légumes, par chromatographie en phase gazeuse avec espace de tête couplée à la spectrométrie de masse (ET CG-SM). La méthode a été validée lors d’un essai interlaboratoires par l’analyse d’échantillons dopés de boissons non alcoolisées gazeuses, de boissons à base de fruits non gazeuses, de boissons à base de fruits gazeuses, de jus de fruits et de légumes contenant de la carotte, d’aliments pour nourrissons à base de légumes et d’aliments pour nourrissons contenant de la viande, à une concentration comprise entre 1,9 µg/kg et 18,6 µg/kg. Toutefois, la linéarité de la réponse de l’instrument a été atteinte pour la gamme de concentrations de 0,5 µg/kg à 20 µg/kg. Bien que la limite de quantification (LOQ) dépende de l’instrument, elle peut généralement se situer entre 0,5 µg/kg et 1,0 µg/kg.
Živila - Ugotavljanje benzena v brezalkoholnih pijačah, drugih pijačah in hrani za dojenčke na osnovi zelenjave s "headspace" plinsko kromatografijo z masno spektrometrijo (HS-GC-MS)
Ta evropski standard določa analizno metodo za določanje benzena v brezalkoholnih pijačah, sokovih in hrani za dojenčke. Priporočljivo je, da se pri metodi prednostno uporabi »headspace« plinsko kromatografijo z masno spektrometrijo. Metodo je treba medlaboratorijsko potrditi v skladu s standardom ISO 5725 ali z mednarodnimi smernicami AOAC za skupne študijske postopke za preverjanje značilnosti analizne metode z uporabo preskusnih materialov, ki vsebujejo brezalkoholne pijače, sokove in hrano za dojenčke v ustreznih ravneh.
General Information
Standards Content (Sample)
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Lebensmittel - Bestimmung von Benzol in Erfrischungsgetränken, anderen Getränken und in Babynahrung auf Gemüsebasis mit Headspace-Gaschromatographie/Massenspektrometrie (HS-GC-MS)Produits alimentaires - Détermination de la teneur en benzène dans les boissons non alcoolisées, les autres boissons et les aliments pour nourrissons à base de légumes par chromatographie en phase gazeuse avec espace de tête couplée à la spectrométrie de masse (ET CG-SM)Foodstuffs - Determination of benzene in soft drinks, other beverages and vegetable-based infant foods by headspace gas chromatography mass spectrometry (HS-GC-MS)71.040.50Fizikalnokemijske analitske metodePhysicochemical methods of analysis67.230Predpakirana in pripravljena hranaPrepackaged and prepared foods67.160.20Non-alcoholic beveragesICS:Ta slovenski standard je istoveten z:EN 16857:2017SIST EN 16857:2017en,fr,de01-julij-2017SIST EN 16857:2017SLOVENSKI
STANDARD
SIST EN 16857:2017
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 16857
May
t r s y ICS
x yä s x rä t râ
x yä t u r English Version
Foodstuffs æ Determination of benzene in soft drinksá other beverages and vegetableæbased infant foods by headspace Produits alimentaires æ Détermination de la teneur en benzène dans les boissons non alcooliséesá les autres boissons et les aliments pour nourrissons à base de légumes par chromatographie en phase gazeuse avec
Lebensmittel æ Bestimmung von Benzol in Erfrischungsgetränkená anderen Getränken und in Babynahrung auf Gemüsebasis mit HeadspaceæThis European Standard was approved by CEN on
t r February
t r s yä
egulations which stipulate the conditions for giving this European Standard the status of a national standard without any alterationä Upætoædate lists and bibliographical references concerning such national standards may be obtained on application to the CENæCENELEC Management Centre or to any CEN memberä
translation under the responsibility of a CEN member into its own language and notified to the CENæCENELEC Management Centre has the same status as the official versionsä
CEN members are the national standards bodies of Austriaá Belgiumá Bulgariaá Croatiaá Cyprusá Czech Republicá Denmarká Estoniaá Finlandá Former Yugoslav Republic of Macedoniaá Franceá Germanyá Greeceá Hungaryá Icelandá Irelandá Italyá Latviaá Lithuaniaá Luxembourgá Maltaá Netherlandsá Norwayá Polandá Portugalá Romaniaá Serbiaá Slovakiaá Sloveniaá Spainá Swedená Switzerlandá Turkey and United Kingdomä
EUROPEAN COMMITTEE FOR STANDARDIZATION COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre:
Avenue Marnix 17,
B-1000 Brussels
9
t r s y CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Membersä Refä Noä EN
s x z w yã t r s y ESIST EN 16857:2017
EN 16857:2017 (E) 2 Contents Page European foreword . 3 1 Scope . 4 2 Normative references . 4 3 Principle . 4 4 Reagents . 4 5 Apparatus . 6 6 Procedure. 8 7 HS-GC-MS analysis . 8 8 Calculation . 11 9 Precision data . 11 10 Test report . 12 Annex A (informative)
Typical chromatograms . 13 Annex B (informative)
Precision data . 14 Bibliography . 15
SIST EN 16857:2017
EN 16857:2017 (E) 3 European foreword This document (EN 16857:2017) has been prepared by Technical Committee CEN/TC 275 “Food analysis - Horizontal methods”, the secretariat of which is held by DIN. 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 2017, and conflicting national standards shall be withdrawn at the latest by November 2017. 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 mandate given to CEN by the European Commission and the Europan Free Trade Association. WARNING — The use of this standard can involve hazardous materials, operations and equipment. This standard does not purport to address all the safety problems associated with its use. It is the responsibility of the user of this standard to take appropriate measures for ensuring the safety and health of the personnel prior to application of the standard and to fulfil statutory requirements for this purpose. Benzene has been classified by IARC as carcinogenic to humans (see [1]). 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, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. SIST EN 16857:2017
EN 16857:2017 (E) 4 1 Scope This European Standard specifies a method for the determination of benzene in soft drinks, other beverages and vegetable-based infant foods, by headspace gas chromatography mass spectrometry (HS-GC-MS). The method has been validated in an interlaboratory study via the analysis of spiked samples of carbonated soft drink, still fruit-based drink, carbonated fruit-based drink, vegetable and fruit juice containing carrot, infant food vegetable based and infant food containing meat, ranging from 1,9 µg/kg to 18,6 µg/kg. However, linearity of the instrument response was proven for the concentration range from 0,5 µg/kg to 20 µg/kg. The limit of quantification (LOQ) depends on the instrument but can generally be expected to be in the range from 0,5 µg/kg to 1,0 µg/kg. 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. EN ISO 3696:1995, Water for analytical laboratory use - Specification and test methods (ISO 3696:1987) 3 Principle The sample is homogenized, a test portion is heated in a closed system with isotopically-labelled benzene added as internal standard. A portion of the headspace is injected into a GC-MS system for identification and quantification. The injection is performed with a split-splitless injection port. The chromatographic separation is obtained on a mid-polarity capillary GC column. The benzene is ionized at 70 eV, recorded in selected ion monitoring (SIM) mode, and quantified by comparison with the stable isotope labelled analogue. 4 Reagents Use only reagents of recognized analytical grade and water complying with grade 1 of EN ISO 3696:1995, unless otherwise specified. Prepare standard solutions preferably gravimetrically. Use an analytical balance (5.1) for the preparation of both native and stable isotope labelled benzene standard solutions. 4.1 Benzene, C6H6, purity is
· 99,0 % (CAS 71-43-2). While not necessary, it is recommended to store at 4 °C to 6 °C to prevent evaporation. Bring to room temperature before use. 4.2 Benzene-d6, purity is
· 99, 6 atom % D (CAS 1076-43-3). While not necessary, it is recommended to store at 4 °C to 6 °C to prevent evaporation. Bring to room temperature before use. 4.3 Helium purified compressed gas, purity equivalent to 99,995 % or better. 4.4 Methanol, suitable for headspace GC analysis (CAS 67-56-1). 4.5 Preparation of stock and standard solutions 4.5.1 General Prepare all standard solutions preferably gravimetrically. Record the tare masses of all recipients and the masses after each preparation step and use for calculation of the mass concentrations of standard solutions. SIST EN 16857:2017
EN 16857:2017 (E) 5 Volumetric preparation of standard solutions may also be applied provided that the volumetric glassware used complies with EN ISO 1042 (see [2]). 4.5.2 Benzene stock solution, mass concentration
approximately 2,20 mg/ml Pipette 20 ml ± 0,1 ml of methanol into a 20 ml headspace vial (5.17) and seal the vial with a crimp cap. Weigh the sealed vial to the nearest 0,1 mg and record the weight as W1. Using a microsyringe, transfer 50 µl of benzene (4.1) through the septum of the vial containing the methanol and shake vigorously or vortex to mix. Reweigh the sealed vial and record the weight (W2) to the nearest 0,1 mg. Subtract W1 from W2 to determine the weight of benzene transferred (W3). Calculate the mass concentration of stock solution from W3 divided by the total volume (20,05 ml). Alternatively, commercially available certified standard solutions may be used if available. Store the benzene stock solution at 4 °C to 6 °C but allow it to attain ambient temperature before use. Discard after 2 weeks. Once the septum on the stock solution has been pierced, the cap shall be replaced. 4.5.3 Benzene intermediate standard solution,
approximately 54 µg/ml Using a microsyringe, transfer 500 µl of benzene stock solution (4.5.2) to a sealed headspace vial containing 20 ml ± 0,1 ml of methanol and shake vigorously. Prepare fresh daily. Calculate the exact mass concentration from the stock solution (4.5.2). 4.5.4 Benzene standard solution,
approximately 0,5 µg/ml Using a microsyringe, transfer 200 µl of benzene intermediate standard solution (4.5.3) to a sealed headspace vial containing 20 ml ± 0,1 ml of water and shake vigorously. Prepare fresh daily. Calculate the exact concentration from the stock solution (4.5.2). Use this standard solution to prepare a 6-point calibration from 0,5 µg/kg to 20 µg/kg (see 4.6). 4.5.5 Benzene-d6 internal standard (IS) stock solution,
approximately 2,36 mg/ml Pipette 20 ml ± 0,1 ml of methanol into a 20 ml headspace vial (5.17) and seal the vial with a crimp cap. Weigh the sealed vial to the nearest 0,1 mg and record the weight as W1. Using a microsyringe, transfer 50 µl of benzene-d6 (4.2) through the septum of the vial containing the methanol and shake vigorously or vortex. Reweigh the sealed vial and record the weight (W2) to the nearest 0,1 mg. Subtract W1 from W2 to determine the weight of benzene-d6 transferred (W3). Calculate the mass concentration of IS stock solution from W3 divided by the total volume (20,05 ml). Alternatively, commercially available certified standard solutions may be used if available. Store the benzene-d6 IS stock solution at 4 °C to 6 °C but allow it to attain ambient temperature before use. Discard after 2 weeks. Once the septum on the IS stock solution has been pierced, the cap shall be replaced. 4.5.6 Benzene-d6 internal standard (IS) solution,
approximately 4,2 µg/ml Using a microsyringe, transfer 36 µl of benzene-d6 IS stock solution (4.5.5) to a sealed headspace vial containing 20 ml ± 0,1 ml of water and shake vigorously. Prepare fresh daily. Calculate the exact mass concentration from the benzene-d6 IS stock solution (4.5.5). 4.6 Preparation of the calibration solutions Prepare calibration solutions of approximately 0 µg/kg, 0,5 µg/kg, 1 µg/kg, 2,5 µg/kg, 5 µg/kg, 10 µg/kg and 20 µg/kg benzene and approximately 10 µg/kg IS according to the following scheme. Add 10 g ± 0,05 g of water to each of seven 20 ml headspace vials and transfer using a positive displacement pipette benzene standard solution (4.5.4), IS solution (4.5.6)and water according to the values given in Table 1. To avoid loss of benzene, seal the vials immediately following addition of the entire benzene and benzene-d6 solutions and water. SIST EN 16857:2017
EN 16857:2017 (E) 6 Table 1 — Preparation of calibration solutions Mass of water g Volume of 0,5 µg/ml benzene (4.5.4) µl Volume of 4,2 µg/ml benzene-d6 (4.5.6) µl Volume of water µl Benzene mass concentration µg/kg Benzene d6 mass concentration µg/kg 10 0 25 400 0 10,1 10 10 25 390 0,5 10,1 10 20 25 380 1,0 10,1 10 50 25 350 2,5 10,1 10 100 25 300 5,0 10,1 10 200 25 200 10 10,1 10 400 25 0 20 10,1 5 Apparatus WARNING — All glassware shall be meticulously cleaned (except disposable glassware). Usual laboratory glassware and equipment and, in particular, the following: 5.1 Analytical balance, capable of weighing to the nearest of 0,0 001 g. 5.2 Top pan balance, capable of weighing to the nearest 0,001 g. 5.3 Headspace gas chromatography – mass spectrometry (HS-GC-MS) apparatus, comprising the following: 5.3.1 Headspace sampling and injection system, suitable for incubation temperatures of up to 60 °C and incubation time of 30 min. The headspace sampling needle should be suitable for maintenance at 100 °C and the transfer line at 105 °C. SIST EN 16857:2017
EN 16857:2017 (E) 7 5.3.2 Injection system, split-splitless injector, suitable for temperatures up to 250 °C. A programmed temperature vaporizing (PTV) injector may be used as an alternative to a split/splitless injector. However, split/splitless injection was proven in the method validation st
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