EN 16620:2015

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)

General Information

• Status: Published
• Publication Date: 21-Apr-2015
• Withdrawal Date: 30-Oct-2015
• ICS: 67.140.20 - Coffee and coffee substitutes
• Technical Committee: CEN/TC 275 - Food analysis - Horizontal methods
• Drafting Committee: CEN/TC 275/WG 13 - Neoformed contaminants
• Current Stage: 9093 - Decision to confirm - Review Enquiry
• Start Date: 21-Mar-2021
• Completion Date: 24-Dec-2025
• Directive: 882/2004 - Regulation (EC) No 882/2004 of the European Parliament and of the Council of 29 April 2004 onofficial controls performed to ensure the verification of compliance with feed and food law, animal health and animal welfare rules
• Mandate: M/463 - Mandate for Standardisation addressed to CEN for the methods of analysis for food contaminants
• Ref Project: SIST EN 16620:2015 - Food analysis - Determination of furan in coffee and coffee products by headspace gas chromatography and mass spectrometry (HS GC-MS)

Overview

EN 16620:2015 (CEN) specifies a validated laboratory method for the determination of furan in coffee and coffee products using headspace gas chromatography coupled to mass spectrometry (HS‑GC‑MS). The method covers roasted ground coffee and processed coffee extracts (spray‑dried, agglomerated, freeze‑dried) and was validated in an interlaboratory study across naturally contaminated samples with reported concentrations from 264 µg/kg to 2 840 µg/kg.

Key topics and technical requirements

• Analytical principle: headspace sampling of hydrated coffee samples followed by GC‑MS analysis. Quantification uses standard addition with d4‑furan as internal standard.
• Sample prep: weigh 0.5–5 g (normally 1 g) into 20 ml headspace vials, add water (typically 5 ml), adjust pH to ~10 with KOH to limit artifact formation, and add internal standard.
• Incubation: 50 °C for 30 minutes prior to headspace sampling.
• Instrumentation: capillary GC with headspace autosampler and mass spectrometer capable of single ion monitoring (SIM). Recommended analytical ions: furan m/z 68 (quantifier) / 39 (qualifier) and d4‑furan m/z 72. Example suitable columns (documented): DB‑5 (60 m) or HP Plot Q (PLOT) coupled to HP‑5MS.
• Calibration and calculation: multipoint standard addition (minimum 7 points recommended) with area ratio (furan/d4‑furan) to derive sample concentration using linear regression (intercept/slope).
• Reagents & standards: high‑purity furan and d4‑furan stock and working solutions prepared in methanol/water; use solvent and water grade per EN ISO 3696.
• Precision & validation: method precision established by interlaboratory study (see Annex B of the standard). Results reported with three significant digits.

Practical applications and users

• Routine monitoring of furan in coffee for food safety, quality control, and regulatory compliance.
• Risk assessment and exposure studies in food safety agencies and research laboratories.
• Quality assurance in coffee manufacturing, processing (spray‑dry, freeze‑dry), and product development to track formation of volatile contaminants.
• Instrument vendors and laboratory method developers for implementation, method transfer and training.

Typical users: accredited food testing laboratories, national reference laboratories, coffee industry QA teams, regulatory authorities, and academic researchers.

Related standards

• EN ISO 3696:1995 - Water for analytical laboratory use (referenced for water quality).
• Prepared by CEN/TC 275 (Food analysis – Horizontal methods).

Keywords: EN 16620:2015, furan in coffee, HS‑GC‑MS, headspace gas chromatography mass spectrometry, food analysis, coffee products, spray‑dried coffee, standard addition, d4‑furan.

Standards Content (Sample)

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
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

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
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

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

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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