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<\/i>]anthracene (BaA), benzo[ a<\/i>]pyrene (BaP), benzo[ b<\/i>]fluoranthene (BbF) and chrysene (CHR). The method allows their quantification in the presence of the other 12 EU priority PAHs (benzo[ j<\/i>]fluoranthene (BjF), cyclopenta[ cd<\/i>]pyrene (CPP), benzo[ k<\/i>]fluoranthene (BkF), dibenz[ a,h<\/i>]anthracene (DhA), benzo[ c<\/i>]fluorene (BcL), dibenzo[ a,e<\/i>]pyrene (DeP), benzo[ ghi<\/i>]perylene (BgP), dibenzo[ a,h<\/i>]pyrene (DhP), dibenzo[ a,i<\/i>]pyrene (DiP), dibenzo[ a,l<\/i>]pyrene (DlP), indeno[1,2,3- cd<\/i>]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).<\/p>\n
This method complies with the performance characteristics specified in Commission Regulation (EU) No 836\/2011 (see [1]<\/span>). In particular the specifications for the limit of detection (LOD) and of the limit of quantification (LOQ) (0,30 \u00b5g\/kg and 0,90 \u00b5g\/kg respectively) were met.<\/p>\n The method has been validated in an interlaboratory study via the analysis of both naturally contaminated and spiked samples, ranging from 0,5 \u00b5g\/kg to 11,9 \u00b5g\/kg. However, linearity of the instrument response was proven for the concentration range 0,5 \u00b5g\/kg to 20 \u00b5g\/kg.<\/p>\n For the determination of PAHs in edible fats and oils, two other standards are also available, EN ISO 22959<\/span> <\/span> and EN ISO 15753<\/span> <\/span>, for more information see [2]<\/span> and [3]<\/span>.<\/p>\n Food analysis. Determination of benzo[a]pyrene, benz[a]anthracene, chrysene and benzo[b]fluoranthene in foodstuffs by gas chromatography mass spectrometry (GC-MS)<\/b><\/p>\nPDF Catalog<\/h4>\n
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\n PDF Pages<\/th>\n PDF Title<\/th>\n<\/tr>\n \n 4<\/td>\n Contents Page <\/td>\n<\/tr>\n \n 5<\/td>\n Foreword <\/td>\n<\/tr>\n \n 6<\/td>\n 1 Scope
2 Normative references
3 Principle <\/td>\n<\/tr>\n\n 7<\/td>\n 4 Reagents <\/td>\n<\/tr>\n \n 9<\/td>\n Table 1 \u2014 Names and structures of the native PAHs <\/td>\n<\/tr>\n \n 10<\/td>\n Table 2 \u2014 Names and structures of 13C labelled PAHs
Table 3 \u2014 Correspondence stable isotope labelled PAHs and native PAHs
Table 4 \u2014 Name and structure of the injection standard <\/td>\n<\/tr>\n\n 11<\/td>\n 5 Standard preparation
5.1 General
5.2 Injection standard solution
5.3 PAH stock solutions
5.4 Mixed PAH stock solutions <\/td>\n<\/tr>\n\n 12<\/td>\n 5.5 Labelled PAH stock solution
5.6 Process solution
5.7 Intermediate solutions <\/td>\n<\/tr>\n\n 13<\/td>\n Table 5 \u2014 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 \u2014 Indicative compositions of the PAH calibration solutions <\/td>\n<\/tr>\n\n 14<\/td>\n 5.9 Standard solution for assessment of chromatographic selectivity
6 Apparatus <\/td>\n<\/tr>\n\n 17<\/td>\n 7 Procedure
7.1 Sample treatment
7.2 Test portion preparation
7.3 Sample extraction by PLE and preparation for SEC <\/td>\n<\/tr>\n\n 18<\/td>\n 7.4 Soxhlet extract as alternative to PLE
7.5 SEC cleanup <\/td>\n<\/tr>\n\n 19<\/td>\n 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 <\/td>\n<\/tr>\n\n 20<\/td>\n 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 <\/td>\n<\/tr>\n\n 21<\/td>\n 8.1.6 Transfer line conditions
8.1.7 Mass spectrometer conditions
8.1.8 Mass spectrometer acquisition parameters and peak identification
Table 7 \u2014 Acquisition programme in SIM <\/td>\n<\/tr>\n\n 22<\/td>\n Table 8 \u2014 Indicative retention times and ions for identification and quantification of the 4 target PAHs in SIM
8.2 Calibration graph <\/td>\n<\/tr>\n\n 23<\/td>\n 8.3 Sample analysis <\/td>\n<\/tr>\n \n 24<\/td>\n 9 Calculation and reporting
9.1 Calculation
9.2 Reporting
10 Quality control
10.1 General <\/td>\n<\/tr>\n\n 25<\/td>\n 10.2 Recovery <\/td>\n<\/tr>\n \n 26<\/td>\n 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 <\/td>\n<\/tr>\n\n 27<\/td>\n 11.2 Repeatability <\/td>\n<\/tr>\n \n 28<\/td>\n 11.3 Reproducibility
The values for benzo[a]pyrene are: <\/td>\n<\/tr>\n\n 29<\/td>\n 12 Test report <\/td>\n<\/tr>\n \n 30<\/td>\n Annex A (informative) Typical chromatograms
Figure A.1 \u2014 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 \u2014 Extracts from chromatograms of PAH standard solutions in toluene <\/td>\n<\/tr>\n\n 31<\/td>\n Table A.1 \u2014 Identification of chromatographic peaks <\/td>\n<\/tr>\n \n 32<\/td>\n Annex B (informative) Precision data <\/td>\n<\/tr>\n \n 33<\/td>\n \u200bTable B.1 \u2014 Statistical evaluation of interlaboratory study results for benz[a]anthracene in different food <\/td>\n<\/tr>\n \n 34<\/td>\n Table B.2 \u2014 Statistical evaluation of interlaboratory study results for benzo[a]pyrene in different food <\/td>\n<\/tr>\n \n 35<\/td>\n Table B.3 \u2014 Statistical evaluation of interlaboratory study results for benzo[b]fluoranthene in different food <\/td>\n<\/tr>\n \n 36<\/td>\n Table B.4 \u2014 Statistical evaluation of interlaboratory study results for chrysene in different food <\/td>\n<\/tr>\n \n 37<\/td>\n Annex C (informative) Precision data from single laboratory validation
Table C.1 \u2014 Results from single laboratory validation for BaA and BaP <\/td>\n<\/tr>\n\n 38<\/td>\n Table C.2 \u2014 Results from single laboratory validation for BbF and CHR <\/td>\n<\/tr>\n \n 39<\/td>\n Bibliography <\/td>\n<\/tr>\n<\/table>\n","protected":false},"excerpt":{"rendered":" \n\n
\n Published By<\/td>\n Publication Date<\/td>\n Number of Pages<\/td>\n<\/tr>\n \n BSI<\/b><\/a><\/td>\n 2015<\/td>\n 42<\/td>\n<\/tr>\n<\/tbody>\n<\/table>\n","protected":false},"featured_media":338144,"template":"","meta":{"rank_math_lock_modified_date":false,"ep_exclude_from_search":false},"product_cat":[2641],"product_tag":[],"class_list":{"0":"post-338137","1":"product","2":"type-product","3":"status-publish","4":"has-post-thumbnail","6":"product_cat-bsi","8":"first","9":"instock","10":"sold-individually","11":"shipping-taxable","12":"purchasable","13":"product-type-simple"},"_links":{"self":[{"href":"https:\/\/pdfstandards.shop\/wp-json\/wp\/v2\/product\/338137","targetHints":{"allow":["GET"]}}],"collection":[{"href":"https:\/\/pdfstandards.shop\/wp-json\/wp\/v2\/product"}],"about":[{"href":"https:\/\/pdfstandards.shop\/wp-json\/wp\/v2\/types\/product"}],"wp:featuredmedia":[{"embeddable":true,"href":"https:\/\/pdfstandards.shop\/wp-json\/wp\/v2\/media\/338144"}],"wp:attachment":[{"href":"https:\/\/pdfstandards.shop\/wp-json\/wp\/v2\/media?parent=338137"}],"wp:term":[{"taxonomy":"product_cat","embeddable":true,"href":"https:\/\/pdfstandards.shop\/wp-json\/wp\/v2\/product_cat?post=338137"},{"taxonomy":"product_tag","embeddable":true,"href":"https:\/\/pdfstandards.shop\/wp-json\/wp\/v2\/product_tag?post=338137"}],"curies":[{"name":"wp","href":"https:\/\/api.w.org\/{rel}","templated":true}]}}