Food analysis - Determination of furan in coffee and coffee products by headspace gas chromatography and mass spectrometry (HS GC-MS)

This European Standard specifies a method for the determination of furan in coffee and coffee products with headspace-gas chromatography-mass spectrometry (HS-GC-MS), see [1] and [2]. Coffee products in the scope of this method are extracts which have been spray-dried, agglomerated or freeze-dried. The method has been validated in an interlaboratory study via the analysis of naturally contaminated samples of spray-dried coffee, freeze-dried coffee and ground roasted coffee ranging from 264 µg/kg to 2 840 µg/kg.

Lebensmittelanalytik - Bestimmung von Furan in Kaffee und Kaffee-Erzeugnissen mit Headspace-Gaschromatographie und Massenspektrometrie (HS GS-MS)

Diese Europäische Norm legt ein Verfahren zur Bestimmung von Furan in Kaffee und Kaffee-Erzeugnissen mittels Headspace-Gaschromatographie/Massenspektrometrie (HS GC MS) fest, siehe [1] und [2]. Kaffee-Erzeugnisse, die in den Anwendungsbereich dieses Verfahrens fallen, sind Extrakte, die sprühgetrocknet, agglomeriert oder gefriergetrocknet wurden. Das Verfahren wurde in einem Ringversuch mit natürlich kontaminierten Proben von sprühgetrocknetem Kaffee, gefriergetrocknetem Kaffee und gemahlenem Röstkaffee im Bereich von 264 µg/kg bis 2 840 µg/kg validiert.

Analyse des produits alimentaires - Dosage du furane dans le café et les produits à base de café par chromatographie en phase gazeuse avec espace de tête couplée à la spectrométrie de masse (HS CG-SM)

La présente Norme européenne spécifie une méthode de dosage du furane dans le café et les produits à base de café par chromatographie en phase gazeuse avec espace de tête couplée à la spectrométrie de masse (ET-CPG-SM), voir 0 et [1]. Les produits à base de café concernés par cette méthode sont des extraits qui ont été séchés par atomisation, agglomérés ou lyophilisés. La méthode a été validée lors d’un essai interlaboratoires impliquant l’analyse d’échantillons naturellement contaminés de café séché par atomisation, de café lyophilisé et de café torréfié, à des teneurs comprises entre 263,8 μg/kg et 2 840,7 μg/kg.

Analize živil - Določevanje furana v kavi in proizvodih iz kave s "headspace" plinsko kromatografijo in masno spektrometrijo (HS GC-MS)

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Status
Published
Publication Date
21-Apr-2015
Current Stage
9093 - Decision to confirm - Review Enquiry
Completion Date
21-Mar-2021

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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Lebensmittelanalytik - Bestimmung von Furan in Kaffee und Kaffee-Erzeugnissen mit Headspace-Gaschromatographie und Massenspektrometrie (HS GC-MS)Analyse des produits alimentaires - Dosage du furane dans le café et les produits à base de café par chromatographie en phase gazeuse avec espace de tête couplée à la spectrométrie de masse (ET-CPG-SM)Food analysis - Determination of furan in coffee and coffee products by headspace gas chromatography and mass spectrometry (HS GC-MS)67.140.20Kava in kavni nadomestkiCoffee and coffee substitutesICS:Ta slovenski standard je istoveten z:EN 16620:2015SIST EN 16620:2015en,fr,de01-julij-2015SIST EN 16620:2015SLOVENSKI

STANDARD
SIST EN 16620:2015
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 16620
April 2015 ICS 67.140.20
English Version

Food analysis - Determination of furan in coffee and coffee products by headspace gas chromatography and mass spectrometry (HS GC-MS)

Analyse des produits alimentaires - Dosage du furane dans le café et les produits à base de café par chromatographie en phase gazeuse avec espace de tête couplée à la spectrométrie de masse (ET-CPG-SM)

Lebensmittelanalytik - Bestimmung von Furan in Kaffee und Kaffee-Erzeugnissen mit Headspace-Gaschromatographie und Massenspektrometrie (HS 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
CEN-CENELEC Management Centre:
Avenue Marnix 17,

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 16620:2015 E SIST EN 16620:2015

EN 16620:2015 (E)

2 Contents Page Foreword ..............................................................................................................................................................3 1 Scope ......................................................................................................................................................4 2 Normative references ............................................................................................................................4 3 Principle ..................................................................................................................................................4 4 Reagents .................................................................................................................................................4 5 Apparatus ...............................................................................................................................................5 6 Procedure ...............................................................................................................................................6 7 Calculation ..............................................................................................................................................9 8 Precision .............................................................................................................................................. 10 9 Test report ........................................................................................................................................... 11 Annex A (informative)

Typical chromatograms ............................................................................................ 12 Annex B (informative)

Precision data ............................................................................................................. 14 Bibliography ..................................................................................................................................................... 15

SIST EN 16620:2015

EN 16620:2015 (E) 3 Foreword This document (EN 16620:2015) 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 October 2015 and conflicting national standards shall be withdrawn at the latest by October 2015. 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. This document has been prepared under a mandate given to CEN by the European Commission and the European Free Trade Association. WARNING — The use of this document can involve hazardous materials, operations and equipment. This document does not purport to address all the safety problems associated with its use. It is the responsibility of the user of this document to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 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, 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 the United Kingdom. SIST EN 16620:2015

EN 16620:2015 (E)

4 1 Scope This European Standard specifies a method for the determination of furan in coffee and coffee products with headspace-gas chromatography-mass spectrometry (HS-GC-MS), see [1] and [2]. Coffee products in the scope of this method are extracts which have been spray-dried, agglomerated or freeze-dried. The method has been validated in an interlaboratory study via the analysis of naturally contaminated samples of spray-dried coffee, freeze-dried coffee and ground roasted coffee ranging from 264 µg/kg to 2 840 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 Coffee and coffee products are weighed into headspace vials, diluted with water and incubated at 50 °C for 30 min. The furan content in the headspace is measured with HS-GC-MS. Quantification is done by using a standard addition curve, taking into account deuterated furan (d4-furan) as internal standard. 4 Reagents Use only reagents of recognized analytical grade and water complying with grade 1 of EN ISO 3696:1995, unless otherwise specified. Solvents shall be of quality for HPLC analysis. 4.1 Furan, (CAS 110-00-9), mass concentration

= 0,936 g/ml. 4.2 d4-Furan, (CAS 6142-90-1),
= 0,991 g/ml. 4.3 Methanol. 4.4 Potassium hydroxide, aqueous solution,
= 250 g/l. 4.5 Stock solutions 4.5.1 Furan stock solution,

approximately 2,50 mg/ml. Place 20 ml of methanol in a headspace vial and seal the vial. Weigh the sealed vial. Using a chilled syringe, transfer 50 µl of furan through the septum of the vial into the methanol. Reweigh the sealed vial. Mix the contents well. The solution is stable for 2 weeks at 4 °C. Pierced headspace vials shall be re-capped. 4.5.2 d4-Furan stock solution,

approximately 2,50 mg/ml. Place 20 ml of methanol in a headspace vial and seal the vial. Weigh the sealed vial. Using a chilled syringe, transfer 50 µl of d4-furan through the septum of the vial into the methanol. Reweigh the sealed vial. Mix the contents well. The solution is stable for 2 weeks at 4 °C. Pierced headspace vials shall be re-capped. SIST EN 16620:2015

EN 16620:2015 (E) 5 4.6 Standard solutions 4.6.1 General The amount of added solutions is calculated by differential weighing considering the densities. The solutions and additional dilutions should be kept cooled when working. Adapt the concentration of standard and internal standard solutions to the expected values in the samples. If necessary, prepare additional dilutions according to the working range. All furan and d4-furan solutions should be prepared in different rooms. Use separate syringes without plastic material. 4.6.2 Furan standard solution 1,

approximately 25 µg/ml. Place 10 ml of water in a headspace vial and seal the vial. Weigh the sealed vial. Using a chilled syringe, transfer 100 µl of furan stock solution (4.5.1) through the septum of the vial into the water. Reweigh the sealed vial. Mix the contents well. Prepare the solution daily. 4.6.3 d4-Furan standard solution 1,

approximately 25 µg/ml. Place 10 ml water in a headspace vial and seal the vial. Weigh the sealed vial. Using a chilled syringe, transfer 100 µl of d4-furan stock solution (4.5.2) through the septum of the vial into the water. Reweigh the sealed vial. Mix the contents well. Prepare the solution daily. 4.6.4 Furan standard solution 2,

approximately 250 ng/ml. Place 10 ml water in a headspace vial and seal the vial. Weigh the sealed vial. Using a chilled syringe, transfer 100 µl of furan standard solution 1 (4.6.2) through the septum of the vial into the water. Reweigh the sealed vial. Mix the contents well. Prepare the solution daily. 4.6.5 d4-Furan standard solution 2,

approximately 250 ng/ml. Place 10 ml water in a headspace vial and seal the vial. Weigh the sealed vial. Using a chilled syringe, transfer 100 µl of d4-furan standard solution 1 (4.6.3) through the septum of the vial into the water. Reweigh the sealed vial. Mix the contents well. Prepare the solution daily. 5 Apparatus Usual laboratory glassware and equipment and, in particular, the following: 5.1 Positive displacement pipette. 5.2 Microlitre syringes. 5.3 Hand crimper and de-crimper. 5.4 Homogenizer or mill. 5.5 Test tube shaker. 5.6 Gas chromatograph for capillary gas chromatography, with split/splitless injector and headspace autosampler. SIST EN 16620:2015

EN 16620:2015 (E)

6 5.6.1 Fused silica capillary column, suitable for analysing volatile organic compounds e.g. non-polar polysiloxane with 5 % phenyl. The following column has been shown to be suitable: J&W DB-5 from Agilent1) length of 60 m, internal diameter (i.d.) of 0,32 mm and film thickness (df) of 1 µm. 5.6.2 PLOT column for separation of very volatile compounds, e.g. HP® Plot Q from Agilent1), length of 15 m, i.d. of 0,32 mm and df of 20 µm coupled to a restriction column HP-5MS from Agilent1), length of 30 m, i.d. of 0,25 mm and df of 0,25 µm. This column is an alternative for the column given under 5.6.1. 5.6.3 Rt®Q-Bond.2) 5.6.4 Carrier gas, helium. 5.6.5 Mass spectrometer with capability of single ion monitoring, coupled to gas chromatograph. 5.7 Headspace vials, 20 ml, with aluminium crim

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