This document is applicable to the determination of polychlorinated dibenzo-p-dioxins (PCDDs), polychlorinated dibenzofurans (PCDFs), (together termed \u2018dioxins\u2019 (PCDD\/Fs)) and dioxin-like PCBs and non-dioxin-like PCBs (dl-PCBs and ndl-PCBs) in animal feeding stuffs. Collaborative studies have been carried out. The method is suitable for the determination of dioxins, dl-PCBs and ndl-PCBs at the appropriate MRL in compound feed and ingredients e.g. oil, mineral clay. The method is applicable to samples containing trace level amounts of one or more dioxins, dioxin-like PCBs and non-dioxin-likePCBs. The limit of quantification (LOQ) is<\/p>\n
0,05 pg\/g (OCDD\/ F<\/i> = 0,1 pg\/g) for the relevant individual congeners of dioxins\/furans,<\/p>\n<\/li>\n 0,05 pg\/g for non-ortho PCBs,<\/p>\n<\/li>\n 10 pg\/g for mono-ortho PCBs, and<\/p>\n<\/li>\n 100 pg\/g for non-dioxin-like-PCBs.<\/p>\n<\/li>\n<\/ul>\n For determination of dioxins and dioxin-like PCBs, the procedure can be used as confirmatory method as defined by Commission Regulation (EC) No 152\/2009 for dioxins and dl-PCB in feed [1<\/span>]. Confirmatory methods as described in this standard are high-resolution gas chromatography\/high resolution mass spectrometry (HRGC\/HRMS) methods. If only the analysis of non-dioxin-like PCBs is required, a GC-LRMS method can be used (e.g. EN 15741<\/span><\/span> [2<\/span>]) provided that appropriate analytical performance criteria are met in the relevant range for the matrix of interest.<\/p>\n This document is split into four modules. Each module describes a part of the whole procedure (see Figure 1<\/span> and Figure 2<\/span>) to be followed:<\/p>\n Module A: Description of standards which might be used;<\/p>\n<\/li>\n Module B: Description of extraction procedures;<\/p>\n<\/li>\n Module C: Description of clean-up procedures;<\/p>\n<\/li>\n Module D: GC\/HRMS determination.<\/p>\n<\/li>\n<\/ol>\n Each module describes a part of the whole method as well as, when applicable, alternatives which should be equivalent. Each module has to be regarded as an example. Combining modules and\/or alternatives gives a highly flexible, \u201cperformance based\u201d procedure. It is permitted to modify the method if all performance criteria laid down in Commission Regulation (EC) No 152\/2009 [1<\/span>] are met.<\/p>\n Any deviation of the described method, combination of modules needs to be recorded as part of the QA\/QC procedures of accredited laboratories and should be available on request.<\/p>\n Animal feeding stuffs: Methods of sampling and analysis. Determination of dioxins and dioxin-like PCBs by GC\/HRMS and of indicator PCBs by GC\/HRMS<\/b><\/p>\n\n
PDF Catalog<\/h4>\n
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\n PDF Pages<\/th>\n PDF Title<\/th>\n<\/tr>\n \n 2<\/td>\n undefined <\/td>\n<\/tr>\n \n 8<\/td>\n 1 Scope <\/td>\n<\/tr>\n \n 10<\/td>\n 2 Normative references
3 Terms and definitions <\/td>\n<\/tr>\n\n 11<\/td>\n 4 Principle <\/td>\n<\/tr>\n \n 12<\/td>\n 5 Reagents
5.1 General
5.2 Dioxins, furans, non-ortho PCBs, mono-ortho PCBs and non-dioxin-like PCBs and their labelled analogues
6 Apparatus
7 Sampling <\/td>\n<\/tr>\n\n 13<\/td>\n 8 Preparation of test sample
9 Procedure
9.1 General
9.2 Animal feed stuff sample and oil\/fat sample
9.2.1 10 g animal feed stuff sample (12 % moisture content)
9.2.2 2,5 g oil\/fat sample
10 Extraction
10.1 General <\/td>\n<\/tr>\n\n 14<\/td>\n 10.2 Module BI Extraction using automated Pressurized Fluid Extraction (PFE) system <\/td>\n<\/tr>\n \n 15<\/td>\n 10.3 Module BII: Manual extraction procedure <\/td>\n<\/tr>\n \n 16<\/td>\n 11 Clean-up
11.1 General <\/td>\n<\/tr>\n\n 18<\/td>\n 11.2 Module CI: Automated clean-up <\/td>\n<\/tr>\n \n 21<\/td>\n 11.3 Module CII: Manual sample clean-up, removal of fat and group separation <\/td>\n<\/tr>\n \n 24<\/td>\n 11.4 Additional clean-up-steps for fraction A and fraction B of module CII <\/td>\n<\/tr>\n \n 26<\/td>\n 11.5 Module CIII: Removal of matrix, manual sample clean-up and group separation <\/td>\n<\/tr>\n \n 31<\/td>\n 12 Module D: Gas chromatograph-high resolution mass spectrometer (GC-HRMS)
12.1 General
12.2 Reagents and materials
12.3 Procedure <\/td>\n<\/tr>\n\n 33<\/td>\n 13 Calculation and expression of results
13.1 General
13.2 Calibration by Isotope Dilution
13.3 Linearity
13.4 Calibration criteria
13.5 Identification and confirmation <\/td>\n<\/tr>\n\n 34<\/td>\n 13.6 Calculation <\/td>\n<\/tr>\n \n 35<\/td>\n 13.7 Toxic Equivalent (TEQ) values <\/td>\n<\/tr>\n \n 38<\/td>\n 13.8 Recovery
14 Precision <\/td>\n<\/tr>\n\n 40<\/td>\n 15 Test report <\/td>\n<\/tr>\n \n 41<\/td>\n Annex A (informative)Description of PTV injection system
A.1 Large volume injection (100 \u00b5l) \u2013 GC-HRMS Calibration mixtures dioxins and non-ortho PCBs <\/td>\n<\/tr>\n\n 42<\/td>\n A.2 Sample preparation procedure
A.3 PTV injection conditions using 100 \u00b5l injection <\/td>\n<\/tr>\n\n 43<\/td>\n Annex B (informative)Description of standards and concentration of the standard solutions
B.1 CAS Registry numbers for dioxins, furans, non-ortho PCBs, mono-ortho PCBs and non-dioxin-like PCBs and their labelled analogues <\/td>\n<\/tr>\n\n 44<\/td>\n B.2 Standard solutions
B.2.1 13C-1,2,3,4-TCDD (50 \u00b5g\/ml)
B.2.2 13C-1,2,3,6,7,8-HxCDF (50 \u00b5g\/ml)
B.2.3 37Cl4-2,3,7,8 TCDD (50 \u00b5g\/ml)
B.2.4 Mixture 13C-PCDD (1 \u00b5g\/ml)
B.2.5 Mixture 13C-PCDF (1 \u00b5g\/ml)
B.2.6 Mixture TCDD-HpCDD (5 \u00b5g\/ml)
B.2.7 Mixture TCDF-HpCDF (5 \u00b5g\/ml)
B.2.8 OCDD (10 \u00b5g\/ml) <\/td>\n<\/tr>\n\n 45<\/td>\n B.2.9 OCDF (50 \u00b5g\/ml)
B.2.10 OCDF standard (5 \u00b5g\/ml)
B.2.11 Mixture 13C-non-ortho PCBs (1 \u00b5g\/ml)
B.2.12 Mixture 13C-mono-ortho PCBs (1 \u00b5g\/ml)
B.2.13 Mixture 13C-non-dioxin-like PCBs (5 \u00b5g\/ml)
B.2.14 Mixture non-ortho PCBs (10 \u00b5g\/ml)
B.2.15 Mixture mono-ortho PCBs (10 \u00b5g\/ml)
B.2.16 Commercially available mixture non-dioxin-like PCBs (10 \u00b5g\/ml)
B.2.17 Recovery standard DIOX-RS-100 (100 pg\/\u00b5l 13C-1,2,3,4-TCDD and 100 pg\/\u00b5l 13C-1,2,3,6,7,8-HxCDF in toluene)
B.2.18 Recovery standard DIOX-RS-1 (1,0 pg\/\u00b5l 13C-1,2,3,4-TCDD, 1,0 pg\/\u00b5l 13C-1,2,3,6,7,8-HxCDF in toluene) <\/td>\n<\/tr>\n\n 46<\/td>\n B.2.19 Recovery standard TCDD-RS-III (100 pg\/\u00b5l 13C-1,2,3,4-TCDD in iso-octane)
B.2.20 Recovery standard TCDD-RS-VI (25 pg\/\u00b5l 13C-1,2,3,4-TCDD in iso-octane)
B.2.21 Clean-up standard CS-50 (50 pg\/\u00b5l 37Cl4-2,3,7,8-TCDD in toluene)
B.2.22 Clean-up standard CS-1 (1,0 pg\/\u00b5l 37Cl4-2,3,7,8-TCDD in toluene)
B.2.23 Mixture non-ortho PCBs (NOP-500) (500 pg\/\u00b5l in toluene)
B.2.24 Mixture PCDD\/F and non-ortho PCBs (DIOXNOP) (20 pg\/\u00b5l in toluene)
B.2.25 Mixture PCDD\/F and non-ortho PCBs (DIOXNOP-1) (2,0 pg\/\u00b5l in toluene)
B.2.26 Mixture mono-ortho PCBs and indicator PCBs (MOPIP-500) (500 pg\/\u00b5l in iso-octane)
B.2.27 Mixture mono-ortho PCBs and indicator PCBs (MOPIP-25) (25 pg\/\u00b5l in iso-octane) <\/td>\n<\/tr>\n\n 47<\/td>\n B.2.28 Mixture mono-ortho PCBs and indicator PCBs (MOPIP-2,5) (2,5 pg\/\u00b5l in iso-octane)
B.2.29 Mixture mono-ortho PCBs and indicator PCBs (MOPIP-,.25) (0,25 pg\/\u00b5l in iso-octane)
B.2.30 Mixture 13C-PCDD\/F and 13C-non-ortho PCBs (13C-DIOXNOP) (50 pg\/\u00b5l in toluene)
B.2.31 Mixture 13C-PCDD\/F and 13C-non-ortho PCBs (13C-DIOXNOP-2) (0,10 pg\/\u00b5l in toluene)
B.2.32 Mixture 13C-mono-ortho PCBs and 13C-indicator PCBs (13C-MOPIP-1) (50 pg\/\u00b5l in iso-octane)
B.2.33 Mixture 13C-mono-ortho PCBs and 13C-indicator PCBs (13C-MOPIP-2) (2,0 pg\/\u00b5l in iso-octane)
B.3 GC-standard solutions
B.3.1 Standard dioxins and non-ortho PCBs mixtures <\/td>\n<\/tr>\n\n 48<\/td>\n B.3.2 Preparation mono-ortho PCBs standard mixtures. <\/td>\n<\/tr>\n \n 50<\/td>\n Annex C (informative)Example of automated procedure <\/td>\n<\/tr>\n \n 52<\/td>\n Annex D (informative)Mass spectrometer (MS) <\/td>\n<\/tr>\n \n 56<\/td>\n Annex E (informative)Use of additional clean-up after fractionation using a small multi-layer silica column
E.1 Preparation of the silica mixtures
E.2 Preparation of the small multi-layer column <\/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 2020<\/td>\n 58<\/td>\n<\/tr>\n<\/tbody>\n<\/table>\n","protected":false},"featured_media":335795,"template":"","meta":{"rank_math_lock_modified_date":false,"ep_exclude_from_search":false},"product_cat":[2641],"product_tag":[],"class_list":{"0":"post-335789","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\/335789","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\/335795"}],"wp:attachment":[{"href":"https:\/\/pdfstandards.shop\/wp-json\/wp\/v2\/media?parent=335789"}],"wp:term":[{"taxonomy":"product_cat","embeddable":true,"href":"https:\/\/pdfstandards.shop\/wp-json\/wp\/v2\/product_cat?post=335789"},{"taxonomy":"product_tag","embeddable":true,"href":"https:\/\/pdfstandards.shop\/wp-json\/wp\/v2\/product_tag?post=335789"}],"curies":[{"name":"wp","href":"https:\/\/api.w.org\/{rel}","templated":true}]}}