CEN/TC 275/WG 13 - Neoformed contaminants

ISO 18862:2016 specifies methods for the determination of acrylamide in coffee and coffee products by extraction with water, clean-up by solid-phase extraction and determination by HPLC-MS/MS and GC-MS. It was validated in a method validation study on roasted coffee, soluble coffee, coffee substitutes and coffee products with ranges from 53 μg/kg to 612,1 μg/kg.

This European Standard specifies a method for the determination of melamine and cyanuric acid in foodstuffs with liquid chromatography in combination with tandem mass spectrometry. The method has been validated in an interlaboratory study via the analysis of spiked samples of milk based infant formula, soy based infant formula, milk powder, whole milk, soy drink and milk chocolate ranging from 0,71 mg/kg to 1,43 mg/kg for melamine and 0,57 mg/kg to 1,45 mg/kg for cyanuric acid. The limits of quantification (LOQ) for melamine and cyanuric acid in food are 0,05 mg/kg and 0,25 mg/kg, respectively. The upper limit of the working range is up to 10 mg/kg for melamine and up to 25 mg/kg for cyanuric acid.

This European Standard specifies a gas chromatographic method using mass spectrometric detection for the determination of ethyl carbamate (EC) in stone fruit spirits, fruit marc spirits and other spirit drinks.
The method has been validated in an interlaboratory study for stone fruit spirits and fruit liqueurs, at levels ranging from 0,253 mg/l to 1,11 mg/l. However, linearity of the instrument response was proven for the concentration ranges 0,10 mg/l to 4,0 mg/l (simplified method) and 0,025 mg/l to 3,0 mg/l (procedure including sample clean-up), respectively.

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.

This Technical Specification specifies a method for the determination of acrylamide in cereal-based products, potato-based products and coffee by gas-chromatography mass spectrometry (GC-MS).
The method has been single-laboratory validated via the analysis of spiked samples (French fries (uncooked), bread, water biscuit, infant cereal, biscuit, green coffee, roast coffee and instant coffee), ranging from 30 μg/kg to 1 500 μg/kg acrylamide.
The results from the single laboratory validation were obtained by a laboratory with significant experience in acrylamide analysis. In addition, this method has also been studied by inter laboratory trial via the analysis of samples containing incurred acrylamide, ranging from approximately 200 μg/kg to 2 000 μg/kg. Critical points of the method are identified in 7.5 and Clause 8.

This European Standard specifies a method for the determination of acrylamide in bakery ware such as bread, toasted bread, crisp bread, butter cookies, and biscuits, as well as potato products such as potato chips, potato crisps, and potato pan cake and roasted coffee, by liquid chromatography in combination with electrospray ionization and tandem mass spectrometry (LC-ESI-MS/MS). This method has been validated in an interlaboratory study via the analysis of both naturally contaminated and spiked samples, ranging from 14,3 µg/kg to 9 083 µg/kg. It was developed at the Swedish National Food Administration and validated in a study organized by the Directorate General Joint Research Centre (DG JRC), Swedish National Food Administration and the Nordic Committee on Food Analysis (NMKL), see [1] and [2].
The limit of quantification (LOQ) depends on the type of instrument used and on the actual performance of the instrument. The majority of the laboratories participating in the validation study were able to determine acrylamide in a butter cookie sample at a level of 14,3 µg/kg. Thus, the validation by interlaboratory study showed that LOQ can be expected to be in the range between below 15 µg/kg and 30 µg/kg.

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.

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].

This Technical Specification specifies a method for the determination of benzo[a]pyrene (BaP) plus benz[a]anthracene (BaA), benzo[b]fluoranthene (BbF) and chrysene (CHR) in several food matrices. The method is based on size exclusion chromatography (SEC) cleanup, followed by quantification with high performance liquid chromatography (HPLC) with programmable fluorescence detection. This method has been in-house validated via the analysis of spiked samples of edible olive oil, fresh mussels, smoked fish, smoked meat products, processed cereal-based foods for young children, infant formulae, chocolate and food supplements (isoflavones) at levels ranging from 0,25 μg/kg to 1,00 μg/kg and from 4,95 μg/kg to 23,53 µg/kg, depending on the Polycyclic Aromatic Hydrocarbon (PAH) or the matrix. This method complies with the performance characteristics specified for BaP, BaA, BbF and CHR in current legislation [3].
The method has been shown to be applicable to a variety of additional matrices as meat products, fresh fish, paprika, roasted coffee, bread, herbs, breakfast cereals, beer, sunflower oil, olives and fried tomato, with a limit of quantification below 0,5 µg/kg.
In addition, the method was tested in-house and shown to be applicable also for the quantification of the other 12 PAHs of the 15+1 EU priority PAHs set (benzo[c]fluorene (BcL), benzo[j]fluoranthene (BjF), benzo[k]fluoranthene (BkF), cyclopenta[cd]pyrene (CPP), dibenz[a,h]anthracene (DhA), 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 all matrices listed above and at similar level ranges, except for CPP, where a UV detection had to be used with limits of quantification above 8 µg/kg.
For the determination of PAHs in edible fats and oils, two other standards are also available, EN ISO 22959 and EN ISO 15753 (see [1] and [2]).

This draft European Standard specifies a gas chromatographic method using mass spectrometric detection for the determination of 3-monochloropropane-1,2-diol (3-MCPD) in hydrolysed vegetable proteins. The method has been validated in interlaboratory studies for malt extract, soup powder, bread crumbs, salami sausage, cheese alternative and hydrolysed vegetable protein [1], [2].

ISO 18862:2016 specifies methods for the determination of acrylamide in coffee and coffee products by extraction with water, clean-up by solid-phase extraction and determination by HPLC-MS/MS and GC-MS. It was validated in a method validation study on roasted coffee, soluble coffee, coffee substitutes and coffee products with ranges from 53 μg/kg to 612,1 μg/kg.

This standard specifies methods for the determination of acrylamide in coffee and coffee products by extraction with water, clean-up by solid-phase extraction and determination by HPLC-MS/MS and GC-MS. It was validated in a method validation study on roasted coffee, soluble coffee, coffee substitutes and coffee products with ranges from 53 μg/kg to 612,1 μg/kg.

This European Standard specifies a highly efficient method for the determination of saturated and aromatic hydrocarbons (from C10 to C50) in vegetable fats and oils and foodstuff on basis of vegetable oils for which it has been interlaboratory validated, with online-HPLC-GC-FID [1], [2] and [3]. This standard is not intended to be applied to other matrices.
The method can be used for the analysis of mineral oil saturated hydrocarbons (MOSH) and/or mineral oil aromatic hydrocarbons (MOAH).
The method has been tested in an interlaboratory study via the analysis of both naturally contaminated and spiked vegetable oil samples and mayonnaise and margarine samples, ranging from 4 mg/kg to 197 mg/kg for MOSH, and from 2 mg/kg to 51 mg/kg for MOAH.
According to the results of the interlaboratory studies, the method has been proven suitable for MOSH- and MOAH mass concentrations each above 10 mg/kg.
In case of suspected interferences from natural sources, the mineral origin of the MOSH and MOAH fraction can be verified by examination of the pattern by GC-MS.