BS EN 16619:2015

$167.15

Food analysis. Determination of benzo[a]pyrene, benz[a]anthracene, chrysene and benzo[b]fluoranthene in foodstuffs by gas chromatography mass spectrometry (GC-MS)

Published By	Publication Date	Number of Pages
BSI	2015	42

Guaranteed Safe Checkout

Category: BSI

If you have any questions, feel free to reach out to our online customer service team by clicking on the bottom right corner. We’re here to assist you 24/7.
Email:[email protected]

Description

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 method 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 standards are also available, EN ISO 22959 and EN ISO 15753 , for more information see [2] and [3].

PDF Catalog

PDF Pages	PDF Title
4	Contents Page
5	Foreword
6	1 Scope 2 Normative references 3 Principle
7	4 Reagents
9	Table 1 — Names and structures of the native PAHs
10	Table 2 — Names and structures of 13C labelled PAHs Table 3 — Correspondence stable isotope labelled PAHs and native PAHs Table 4 — Name and structure of the injection standard
11	5 Standard preparation 5.1 General 5.2 Injection standard solution 5.3 PAH stock solutions 5.4 Mixed PAH stock solutions
12	5.5 Labelled PAH stock solution 5.6 Process solution 5.7 Intermediate solutions
13	Table 5 — Nominal volumes of the mixed PAH stock solution (5.4) to be pipetted in order to prepare 100 ml of each of the listed concentration levels of the intermediate solutions 5.8 Calibration solutions Table 6 — Indicative compositions of the PAH calibration solutions
14	5.9 Standard solution for assessment of chromatographic selectivity 6 Apparatus
17	7 Procedure 7.1 Sample treatment 7.2 Test portion preparation 7.3 Sample extraction by PLE and preparation for SEC
18	7.4 Soxhlet extract as alternative to PLE 7.5 SEC cleanup
19	7.6 Concentration step after SEC cleanup 7.7 Sample preparation for SPE cleanup 7.8 SPE cleanup 7.9 Preparation of the sample for GC-MS analysis 8 GC-MS analysis 8.1 GC-MS operating conditions 8.1.1 General
20	8.1.2 Injection conditions, for PTV injector 8.1.3 Injection conditions, for split-splitless injector 8.1.4 Oven conditions 8.1.5 Column conditions
21	8.1.6 Transfer line conditions 8.1.7 Mass spectrometer conditions 8.1.8 Mass spectrometer acquisition parameters and peak identification Table 7 — Acquisition programme in SIM
22	Table 8 — Indicative retention times and ions for identification and quantification of the 4 target PAHs in SIM 8.2 Calibration graph
23	8.3 Sample analysis
24	9 Calculation and reporting 9.1 Calculation 9.2 Reporting 10 Quality control 10.1 General
25	10.2 Recovery
26	10.3 Chromatographic resolution 10.4 Reference material for method performance check 10.5 Procedural blank 10.6 Integrity check of the standards 11 Precision data 11.1 General
27	11.2 Repeatability
28	11.3 Reproducibility The values for benzo[a]pyrene are:
29	12 Test report
30	Annex A (informative) Typical chromatograms Figure A.1 — Typical GC-MS chromatogram of 15+1 EU PAHs and stable isotope labelled PAHs obtained under the conditions described in Clause 8 and applying PTV injection Figure A.2 — Extracts from chromatograms of PAH standard solutions in toluene
31	Table A.1 — Identification of chromatographic peaks
32	Annex B (informative) Precision data
33	Table B.1 — Statistical evaluation of interlaboratory study results for benz[a]anthracene in different food
34	Table B.2 — Statistical evaluation of interlaboratory study results for benzo[a]pyrene in different food
35	Table B.3 — Statistical evaluation of interlaboratory study results for benzo[b]fluoranthene in different food
36	Table B.4 — Statistical evaluation of interlaboratory study results for chrysene in different food
37	Annex C (informative) Precision data from single laboratory validation Table C.1 — Results from single laboratory validation for BaA and BaP
38	Table C.2 — Results from single laboratory validation for BbF and CHR
39	Bibliography

Additional information

Status	Confirmed
Pages	42
Publication Date	2015-04-30
ISBN	978 0 580 80856 2
Standard Number	BS EN 16619:2015
Title	Food analysis. Determination of benzo[a]pyrene, benz[a]anthracene, chrysene and benzo[b]fluoranthene in foodstuffs by gas chromatography mass spectrometry (GC-MS)
Identical National Standard Of	EN 16619:2015
Descriptors	Determination of content, Agricultural products, Food products, Plant products, Pesticides, Mass spectrometry, Residues (pesticides), Chemical analysis and testing, Liquid chromatography, Food testing
Publisher	BSI
Committee	AW/275
ICS Codes	67.050 - General methods of tests and analysis for food products

Preview PDF


PDF Format	Searchable	Printable	Preview Now

BS EN 16619:2015

PDF Catalog

Related products