65.120 - Animal feeding stuffs
ICS 65.120 Details
Animal feeding stuffs
Futtermittel
Aliments des animaux
Krmila
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This document describes a method for the determination of individual intact glucosinolates in rapeseed
by high performance liquid chromatography (HPLC) coupled with tandem mass spectrometry
(MS/MS). Progoitrin, gluconapin, glucobrassicanapin, glucobrassicin, nasturtiin, neoglucobrassicin and
4-methoxyglucobrassicin are quantitatively determined. Other glucosinolates such as
4-hydroxyglucobrassicin, glucnapoliferin, glucoalysin, can only be qualitatively detected when
analytical standards become commercially available.
The method has been in-house validated for rapeseeds in the range 0.05-60 mmol/kg for individual
glucosinolates.
- Standard52 pagesEnglish languagesale 10% offe-Library read for1 day
- Draft51 pagesEnglish languagesale 10% offe-Library read for1 day
This document defines a Pulsed Field Gel Electrophoresis (PFGE) methodology for the identification of authorized probiotic Lactobacillus, Pediococcus, Enterococcus and Bacillus strains. The method can be applied to purified colonies obtained from cultured premixtures and feeds, in order to verify the presence of strains used as feed additives in declared concentrations, even against eventual microbial background resulting from nonsterile matrices.
- Standard16 pagesEnglish languagesale 10% offe-Library read for1 day
- Draft16 pagesEnglish languagesale 10% offe-Library read for1 day
This document specifies a Pulsed Field Gel Electrophoresis (PFGE) methodology for the identification of authorized probiotic strains of Lactobacillus, Pediococcus, Enterococcus and Bacillus strains. The method can be applied to purified colonies obtained from cultured premixtures and feeds. The method can be used, even in the presence of a significant microbiological background, to verify the presence of microorganisms (strains and declared concentrations) used as feed additives in animal feeding stuffs.
- Standard16 pagesEnglish languagesale 10% offe-Library read for1 day
- Draft16 pagesEnglish languagesale 10% offe-Library read for1 day
This document specifies a method for the determination of individual intact glucosinolates in feed materials including oilseeds and oilseed products and in compound feeds by high performance liquid chromatography (HPLC) coupled with tandem mass spectrometry (MS/MS).
The method specified in this document has been successfully validated by collaborative trial in the following matrices: rape seed, camelina seed, Brassica oleracea seeds, mixed oilseeds, rape seed flakes, compound feed for bovine, porcine and poultry.
The method is applicable for the quantitative determination of epiprogroitrin, glucoalyssin, glucoarabin, glucobrassicanapin, glucobrassicin, glucocamelinin, glucoerucin, glucoiberin, gluconapin, gluconapoleiferin, gluconasturtiin, glucoraphanin, glucoraphenin, glucotropaeolin, homoglucocamelinin, 4-hydroxyglucobrassicin, 4-methoxyglucobrassicin, neoglucobrassicin, progoitrin, sinalbin and sinigrin.
The concentration ranges tested in the collaborative trial for each individual glucosinolate and for the total glucosinolate content are summarized in Table 1.
[table not represented]
- Standard52 pagesEnglish languagesale 10% offe-Library read for1 day
- Draft51 pagesEnglish languagesale 10% offe-Library read for1 day
This document describes a method for the quantitative determination of pyrrolizidine alkaloids (PA) in complete and supplementary feed and in forages by liquid chromatography tandem mass spectrometry (LC-MS/MS) after solid phase extraction (SPE) clean-up.
The method has been successfully validated in a collaborative trial for the matrices complete feed for horses, supplementary feed for horses, supplementary feed for rodents, hay, alfalfa and grass silage. Validation was carried out for the PA and concentrations ranges listed in Table 1. It was demonstrated that the PA isomeric pairs senecivernine and senecionine as well as senecivernine-N-oxide and senecionine-N-oxide cannot be determined individually due to insufficient chromatographic separation. However, the sums of the individual PA of the isomeric pairs were quantified with sufficient reproducibility. Co-elution of other PA-isomers not included in the scope of the method shall be taken into account. A list of potentially co-eluting isomers is presented in Annex E.
Although the calibration range of the method protocol is specified from 10 μg/kg to 300 μg/kg, the results of the collaborative study showed, that the dilution of sample extracts with blank sample extracts enables for the quantitation of concentrations exceeding the calibration range. Satisfactory reproducibility was achieved when quantifying up to 1428 μg/kg for individual PA and up to 887 μg/kg for the sum of isomeric pairs.
NOTE 1 A second method was part of the method validation collaborative main trial. For this method PA-N-Oxides are reduced by adding zinc powder to the extract of the feed material. The following steps correspond to the first and main method. Quantitative results for each PA except the otonecine type PA senkirkine represent the sum of the free PA base and its corresponding N-oxide.
NOTE 2 Due to insufficient numbers of data for some analyte-matrix combinations statistical evaluation was not valid for standardization. Received data indicated the methods applicability in experienced laboratories with appropriate quality assurance measures. Therefore, the method description is included as an informative annex (Annex D).
- Standard67 pagesEnglish languagesale 10% offe-Library read for1 day
- Draft66 pagesEnglish languagesale 10% offe-Library read for1 day
This document specifies a method for the quantitative determination of pyrrolizidine alkaloids (PA) in the concentration ranges shown in Table 1 in complete and supplementary feed and in forages by liquid chromatography tandem mass spectrometry (LC-MS/MS) after solid phase extraction (SPE) clean-up.
Table 1 - Summary of concentration ranges per PA tested in the collaborative trial
NOTE 1 A second method was part of the method validation collaborative main trial. For this method PA-N-Oxides are reduced by adding zinc powder to the extract of the feed material. The following steps correspond to the first and main method. Quantitative results for each PA except the otonecine type PA senkirkine represent the sum of the free PA base and its corresponding N-oxide.
NOTE 2 Due to insufficient numbers of data for some analyte-matrix combinations statistical evaluation was not valid for standardization. Received data indicated the methods applicability in experienced laboratories with appropriate quality assurance measures. Therefore, the method description is included as an informative annex (Annex D).
- Standard67 pagesEnglish languagesale 10% offe-Library read for1 day
- Draft66 pagesEnglish languagesale 10% offe-Library read for1 day
This document specifies a method for the determination of free gossypol, extractable by acidified acetonitrile/water, in cottonseed, cottonseed products and compound feeds by liquid chromatography with tandem mass spectrometry (LC-MS/MS).
The method described in this document has been successfully validated in the range of 69 mg/kg to 5 950 mg/kg by collaborative trial in the following matrices: cottonseed, cottonseed products (cake/meal, hulls) and compound feeds for bovine, porcine and poultry.
NOTE It is possible to reach quantification limits of approximatively 5 mg/kg in compound feeds. The method might be applicable at lower and at higher concentrations than the concentration range validated in the collaborative trial. However, this needs to be assessed by in-house validation.
- Standard21 pagesEnglish languagesale 10% offe-Library read for1 day
- Draft21 pagesEnglish languagesale 10% offe-Library read for1 day
This document describes product specifications, product characteristics and other relevant information for algae and algae products for food, nutraceutical and animal feed applications. This document is a general overview of available limits, procedures and analytical methods applicable to algae and algae products used for food and feed applications.
This document does not apply to pharmaceutical, cosmetics, fertilizer/biostimulants, chemical and biofuel applications.
- Technical report42 pagesEnglish languagesale 10% offe-Library read for1 day
This document describes product specifications, product characteristics and other relevant information for algae and algae products for food, nutraceutical and animal feed applications. This document is a general overview of available limits, procedures and analytical methods applicable to algae and algae products used for food and feed applications.
This document does not apply to pharmaceutical, cosmetics, fertilizer/biostimulants, chemical and biofuel applications.
- Technical report42 pagesEnglish languagesale 10% offe-Library read for1 day
- Amendment8 pagesEnglish languagesale 10% offe-Library read for1 day
- Draft5 pagesEnglish languagesale 10% offe-Library read for1 day
- Amendment7 pagesEnglish languagesale 10% offe-Library read for1 day
- Draft4 pagesEnglish languagesale 10% offe-Library read for1 day
This analytical procedure specifies a reverse phase high performance liquid chromatographic with UV detection (RP-HPLC-UV) method for the simultaneous determination of four authorized carotenoids in fish compound feed and fish premix, namely astaxanthin (AXN), canthaxanthin (CXN), adonirubin (ADR) and astaxanthin dimethyldisuccinate (AXN DMDS), and of six authorized carotenoids in poultry feed and poultry premix, namely canthaxanthin (CXN); capsanthin (CSN), ethyl ester of beta-apo-8'-carotenoic acid (BACARE), citranaxanthin (CIXN), lutein (LUT) and zeaxanthin (ZEA) at levels ranging from approximately 2 mg/kg to approximately 4 500 mg/kg (depending on the carotenoid). Beta-carotene (BCAR), authorized in compound feed and premixes for all animal species, was also added to the scope. The analytical procedure is fit for the purpose of quantitation of declared carotenoids and labelling confirmation. This document is applicable to feed produced using natural and synthetic feed additives.
Xanthophyll esters like those of lutein, zeaxanthin and capsanthin that might be present in feed materials are not authorized feed additives and therefore not part of the scope of this document.
- Standard49 pagesEnglish languagesale 10% offe-Library read for1 day
- Draft47 pagesEnglish languagesale 10% offe-Library read for1 day
This document specifies general rules for the enumeration of bacilli in feeding stuffs (additives, premixtures and compound feeds including mineral feeds) [4] that contain bacilli as a single microorganism component or in a mixture with other microorganisms. There are different categories of feed samples:
a) Additives containing about 1010 colony forming units (CFU)/g;
b) Premixtures containing about 1011 CFU/kg;
c) Compound feeds, meal or pellets containing about 109 CFU/kg.
- Standard16 pagesEnglish languagesale 10% offe-Library read for1 day
- Draft16 pagesEnglish languagesale 10% offe-Library read for1 day
This document specifies general rules for the enumeration of lactobacilli in feeding stuffs (additives, premixtures and compound feeds excluding mineral feeds) that contain lactobacilli as a single microorganism component or in a mixture with other microorganisms. Applying the method to premixtures and compound feeds with critical amounts of copper demands a special procedure (see A.2). The document is not applicable to mineral feeds, which are defined as complementary feeding stuffs composed mainly of minerals and containing at least 40 % crude ash (Regulation (EC) No 767/2009) [3].
There are different categories of feed samples:
a) Additives containing about 1010 colony forming units (CFU)/g;
b) Premixtures containing about 1011 CFU/kg;
c) Compound feeds, meal or pellets which contain about 109 CFU/kg.
- Standard20 pagesEnglish languagesale 10% offe-Library read for1 day
- Draft18 pagesEnglish languagesale 10% offe-Library read for1 day
This document specifies general rules for the enumeration of enterococci (E. faecium) in feeding stuffs (additives, premixtures and compound feeds excluding mineral feeds) that contain enterococci as a single microorganism component or in a mixture with other microorganisms. Applying the method to premixtures and compound feeds with critical amounts of copper demands a special procedure (see A.2). The document is not applicable to mineral feeds which are defined as complementary feeding stuffs composed mainly of minerals and containing at least 40 % crude ash (Regulation (EC) 767/2009) [4].
There are different categories of feed samples:
a) Additives containing about 1010 colony forming units (CFU)/g;
b) Premixtures containing 1011 CFU/kg;
c) Compound feeds, meal or pellets which contain about 109 CFU/kg.
- Standard20 pagesEnglish languagesale 10% offe-Library read for1 day
- Draft20 pagesEnglish languagesale 10% offe-Library read for1 day
This document specifies general rules for the enumeration of Saccharomyces cerevisiae in feeding stuffs (additives, premixtures and compound feeds excluding mineral feeds) that contain Saccharomyces cerevisiae as a single microorganism component or in a mixture with other microorganisms. Applying the method to premixtures and compound feeds with critical amounts of copper demands a special procedure (see Annex A). The document is not applicable to mineral feeds, which are defined as complementary feeding stuffs composed mainly of minerals and containing at least 40 % crude ash (Regulation (EC) 767/2009) [3].
There are different categories of feed samples:
a) Additives containing about 1010 colony forming units (CFU)/g;
b) Premixtures containing about 1011 CFU/kg;
c) Compound feeds, meal or pellets which contain about 109 CFU/kg.
- Standard16 pagesEnglish languagesale 10% offe-Library read for1 day
- Draft16 pagesEnglish languagesale 10% offe-Library read for1 day
This document specifies general rules for the enumeration of pediococci in feeding stuffs (additives, premixtures and compound feeds excluding mineral feeds) that contain pediococci as a single microorganism component or in a mixture with other microorganisms. Applying the method to premixtures and compound feeds with critical amounts of copper demands a special procedure (see A.2). The document is not applicable to mineral feeds which are defined as complementary feeding stuffs composed mainly of minerals and containing at least 40 % crude ash (Regulation (EC) 767/2009) [3]. There are different categories of feed samples:
a) Additives containing about 1010 colony forming units (CFU)/g;
b) Premixtures containing about 1011 CFU/kg;
c) Compound feeds, meal or pellets which contain about 109 CFU/kg.
- Standard20 pagesEnglish languagesale 10% offe-Library read for1 day
- Draft20 pagesEnglish languagesale 10% offe-Library read for1 day
This document specifies a method for the determination of the content of the total vitamin A (retinol), vitamin E (α-tocopherol) and vitamin D3 (cholecalciferol) in animal feed using solid phase extraction (SPE) clean-up and high-performance liquid chromatography (HPLC).
NOTE The procedure also enables determination of vitamin D2 but with the use of another internal standard. The method is fully validated only for vitamin D3.
The method has been successfully tested in collaborative trial for complete feed for broilers, pigs, and turkey, for premixture for broilers and piglets, for complementary feed for cows and mineral feed within the following ranges:
• vitamin A: 4 365 IU/kg - 4 118 352 IU/kg;
• vitamin E: 22 mg/kg - 13 800 mg/kg;
• vitamin D3: 1 668 IU/kg - 1 638 150 IU/kg.
The limits of quantification were not determined within the validation study. Quantification limits of 1 100 IU for vitamin A/kg (using UV-detection), 4 mg for vitamin E/kg (using UV-detection), 2 mg for vitamin E/kg (using fluorescence detection) and 2 000 IU for vitamin D/kg (using UV-detection) should be normally achieved. Lower limits are possible provided they are validated by the user.
- Standard38 pagesEnglish languagesale 10% offe-Library read for1 day
- Draft39 pagesEnglish languagesale 10% offe-Library read for1 day
This document describes a method for the determination of free gossypol, extractable by acidified
acetonitrile/water, in cottonseeds, cottonseed cake and complete feed by high performance liquid
chromatography (HPLC) coupled with tandem mass spectrometry (MS/MS)
This method has been in-house validated in the range 20-6000 mg/kg.
- Standard21 pagesEnglish languagesale 10% offe-Library read for1 day
- Draft21 pagesEnglish languagesale 10% offe-Library read for1 day
This document specifies a method for the determination of saturated and aromatic hydrocarbons (from C10 to C50) in feed. The method has been interlaboratory validated with on-line-HPLC-GC-FID – see [1], [2] and [3]. This method 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 is applicable for feed materials, in particular vegetable oils and other fat rich feed materials, compound feeds and pre-mixtures. It is not applicable to additives or deodistillates.
NOTE 1 The method was not designed for encapsulated matrices.
The method has been tested in an interlaboratory study via the analysis of both naturally contaminated and spiked samples (pre-mixture, soybean meal, sunflower seeds, chicken feed, pig feed, vegetable oil) ranging from 3 mg/kg to 286 mg/kg for MOSH and from 1 mg/kg to 16 mg/kg for MOAH.
According to the results of the interlaboratory study, the method has been proven suitable for MOSH and MOAH mass concentrations, each above 10 mg/kg. However, the method was not fully validated during the collaborative study for the premixture sample due to too low concentrations of MOSH and MOAH. The method was also not fully validated during the collaborative study for the sunflower seeds sample due to a too low concentration of MOAH.
NOTE 2 The conclusions regarding MOAH are based on 4 analyte / matrix combinations while the IUPAC protocol [4] expects this to be a minimum of 5.
In case of suspected interferences from natural sources, the fossil origin of the MOSH and MOAH fraction can be verified by examination of the pattern by GC-MS.
For the determination of MOSH and MOAH in edible fats and oils, another CEN standard is also available: EN 16995. For more information see [5].
Annex C proposes a manual alternative method to on-line HPLC-GC-FID analysis that can be used as a screening method for the determination of MOSH.
- Standard40 pagesEnglish languagesale 10% offe-Library read for1 day
- Draft41 pagesEnglish languagesale 10% offe-Library read for1 day
This document specifies a method for the determination of crude ash of animal feeding stuffs.
- Standard7 pagesEnglish languagesale 15% off
- Standard8 pagesFrench languagesale 15% off
- Amendment7 pagesEnglish languagesale 10% offe-Library read for1 day
- Draft4 pagesEnglish languagesale 10% offe-Library read for1 day
- Amendment8 pagesEnglish languagesale 10% offe-Library read for1 day
- Draft5 pagesEnglish languagesale 10% offe-Library read for1 day
This European Standard defines general rules for the enumeration of probiotic yeasts (Saccharomyces cerevisiae) in feed samples (additives, premixtures and feeding stuffs) that contain yeast as a single microorganism component or in a mixture with other microorganisms. Applying the method to feeds with a high copper content (> 400 mg/kg) demands a special procedure (see Annex B).The standard is not applicable to mineral feeds which are defined as complementary feeding stuffs composed mainly of minerals and containing at least 40 % crude ash (Council Directive 79/373/EEC).
There are different categories of feed samples:
a) Additives which contain about 10+9 CFU/g to 10+10 CFU/g (CFU = colony forming units).
b) Premixtures which contain about 10+8 CFU/g
c) Feeds, meal or pellets, which contain about 10+6 CFU/g and include complete feedingstuffs, and milk replacers.
The detection limit is as defined in EN ISO 7218.
- Standard16 pagesEnglish languagesale 10% offe-Library read for1 day
- Draft16 pagesEnglish languagesale 10% offe-Library read for1 day
This European Standard defines general rules for the enumeration of enterococci in feed samples (additives, premixtures and feeding stuffs) that contain enterococci (E. faecium) as a single microorganism component or in a mixture with other microorganisms. Applying the method to feeds with a high copper content (> 400 mg/kg) demands a special procedure (see Annex A).This standard is not applicable to mineral feeds which are defined as complementary feeding stuffs composed mainly of minerals and containing at least 40 % crude ash (Council Directive 79/373/EEC).
There are different categories of feed samples:
a) Additives containing about 10+10 colony forming units (CFU)/g;
b) Premixtures containing 10+8 CFU/g;
c) Feeds, meal or pellets which contain about 10+6 CFU/g and include complete feeding stuffs,and milk replacers.
The detection limit is as defined in EN ISO 7218.
- Standard20 pagesEnglish languagesale 10% offe-Library read for1 day
- Draft20 pagesEnglish languagesale 10% offe-Library read for1 day
This European Standard defines general rules for the enumeration of probiotic lactobacilli in feed samples (additives, premixtures and feeding stuffs) that contain lactobacilli as a single bacterial component or in a mixture with other microorganisms. Applying the method to feeds with high copper content (>200 mg/kg) demands a special procedure (see Annex A). This standard is not applicable to mineral feeds, which are defined as complementary feeding stuffs composed mainly of minerals and containing at least 40 % crude ash (Council Directive 79/373/EEC).
There are different categories of feed samples:
a) Additives containing about 10+10 colony forming units (CFU)/g
b) Premixtures containing about 10+8 CFU/g
c) Feeds, meal or pellets, which contain about 10+6 CFU/g and include complete feeding stuffs and milk replacers.
The detection limit is as defined in ISO 7218.
- Standard20 pagesEnglish languagesale 10% offe-Library read for1 day
- Draft18 pagesEnglish languagesale 10% offe-Library read for1 day
This European Standard defines general rules for the enumeration of probiotic bacilli in feeds containing bacilli (Bacillus species) as a single microorganism, component or mixed with other microorganisms. This method is not applicable to mineral feeds which are defined as complementary feeding stuffs composed mainly of minerals and containing at least 40 % crude ash (Council Directive 79/373/EEC).
There are different categories of feed samples:
a) Additives containing about 10+10 colony forming units (CFU)/g;
b) Premixtures containing about 10+8 CFU/g;
c) Feeds, meal or pellets, which contain about 10+6 CFU/g and include complete feeding stuffs, and milk replacers.
The detection limits are 500 (5 × 10+2) colony forming units per gram (CFU/g). The limits of determination are 2 × 10+4 CFU/g.
- Standard16 pagesEnglish languagesale 10% offe-Library read for1 day
- Draft16 pagesEnglish languagesale 10% offe-Library read for1 day
This analytical procedure specifies a reverse phase high performance liquid chromatographic with UV detection (RP-HPLC-UV) method for the simultaneous determination of four authorized carotenoids in fish compound feed, namely astaxanthin (AXN), canthaxanthin (CXN), adonirubin (ADR) and astaxanthin dimethyldisuccinate (AXN DMDS), and of six authorized carotenoids in poultry feed, namely canthaxanthin (CXN); capsanthin (CSN), ethyl ester of beta-apo-8'-carotenoic acid (BACARE), citranaxanthin (CIXN), lutein (LUT) and zeaxanthin (ZEA) at levels ranging from ca. 2 to ca. 4 500 mg/kg (depending on the carotenoid). Beta-carotene (BCAR), authorized in compound feed for all animal species, was also added to the scope. The analytical procedure is fit for the purpose of quantitation of declared carotenoids and labelling confirmation. The procedure applies to natural and synthetic feed additives.
Xanthophyll esters like those of lutein, zeaxanthin and capsanthin that might be present in feed materials are not authorized feed additives and therefore not part of the scope of this method.
- Standard49 pagesEnglish languagesale 10% offe-Library read for1 day
- Draft47 pagesEnglish languagesale 10% offe-Library read for1 day
This international standard defines general rules for the enumeration of probiotic pediococci in feed samples (additives, premixtures and feeding stuffs) that contain pediococci as a single bacterial component or in a mixture with other microorganisms. This standard is not applicable for mineral feeds which are defined as complementary feeding stuffs composed mainly of minerals and containing at least 40 % crude ash (Council Directive 79/373/EEC).
There are different categories of feed samples:
a) Additives containing about 10+10 (colony forming units) CFU/g
b) Premixtures containing about 10+8 CFU/g
c) Feeds, meal or pellets, which contain about 10+6 CFU/g and include complete feeding stuffs, and milk replacers.
- Standard20 pagesEnglish languagesale 10% offe-Library read for1 day
- Draft20 pagesEnglish languagesale 10% offe-Library read for1 day
This European Standard specifies a method for the determination of the content of the total vitamin A (retinol), vitamin E (alpha-tocopherol) and vitamin D (D2 ergocalciferol or D3 cholecalciferol) content in animal feed using solid phase extraction (SPE) clean-up and high performance liquid chromatography (HPLC).
The limit of quantification is XXXX IU vitamin A/kg (using UV-detection), XX IU vitamin A/kg (using fluorescence detection), XX mg vitamin E/kg (using UV-detection), XX mg vitamin E/kg (using
fluorescence detection), XX IU vitamin D/kg (using UV-detection) and XX IU vitamin D/kg (using fluorescence detection).
- Standard38 pagesEnglish languagesale 10% offe-Library read for1 day
- Draft39 pagesEnglish languagesale 10% offe-Library read for1 day
This document specifies a method for the determination of saturated and aromatic hydrocarbons (from C10 to C50) in feed. The method has been interlaboratory validated with online-HPLC-GC-FID – see [1], [2] and [3]. This method 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 is applicable for feed materials, in particular vegetable oils and other fat rich feed materials, compound feeds and pre-mixtures. It is not applicable to additives or deodistillates.
The method has been tested in an interlaboratory study via the analysis of both naturally contaminated and spiked samples (pre-mixture, soybean meal, sunflower seeds, chicken feed, pig feed, vegetable oil) ranging from 3 mg/kg to 286 mg/kg for MOSH and from 1 mg/kg to 16 mg/kg for MOAH.
According to the results of the interlaboratory study, the method has been proven suitable for MOSH and MOAH mass concentrations, each above 10 mg/kg. However, the method was not fully validated during the collaborative study for the premixture sample due to too low concentrations of MOSH and MOAH. The method was also not fully validated during the collaborative study for the sunflower seeds sample due to a too low concentration of MOAH.
NOTE The conclusions regarding MOAH are based on 4 analyte / matrix combinations while according to the IUPAC protocol [4] expects this to be a minimum of 5.
In case of suspected interferences from natural sources, the fossil origin of the MOSH and MOAH fraction can be verified by examination of the pattern by GC-MS.
For the determination of MOSH and MOAH in edible fats and oils, another CEN standard is also available: EN 16995. For more information see [5].
Annex C proposes a manual alternative method to online HPLC-GC-FID analysis that can be used as a screening method.
- Standard40 pagesEnglish languagesale 10% offe-Library read for1 day
- Draft41 pagesEnglish languagesale 10% offe-Library read for1 day
This document describes a method for determination of the massic activity (Bq/kg) of 131I, 134Cs and 137Cs in animal feeding stuffs in monitoring laboratories.
General guidance on the preparation of feed samples and the measurement of the three radionuclides 131I, 134Cs and 137Cs by high resolution gamma-ray spectrometry is provided. The current document aims to be complementary to existing standards. More information on sample preparation, moisture content determination and gamma-ray spectrometry can be found in specific standards referred to in this document. For example, generic advice on the equipment selection, detectors and quality assurance for gamma-ray spectrometry can be found in ISO 20042 [4].
The method was fully statistically tested and evaluated in a collaborative trial comprising five animal feeding stuff samples for the radionuclides 131I, 134Cs and 137Cs. Details on the successfully tested working range for each of the examined radionuclides are described in Annex C.
- Standard34 pagesEnglish languagesale 10% offe-Library read for1 day
- Draft35 pagesEnglish languagesale 10% offe-Library read for1 day
This standard describes a method of Iodium-131, Caesium-134 and Caesium-137 massic activity (Bq/kg) determination in animal feed.
Today, the most commonly used method for identification and quantification of radioactivity from these radionuclides in feed samples is high-resolution gamma-ray spectrometry. It is based on analysis of full-energy peaks (FEP) of the emitted gamma rays. Therefore, care should be taken to use appropriate energy and efficiency calibrations for each detector and test portion used.
In this standard, general guidance on the preparation of feed samples is provided together with specific information on high resolution gamma-ray spectrometry of the three radionuclides Iodium-131, Caesium-134 and Caesium-137. More information on these and related topics can be found in specific standards referred to in this document. For example, generic advice on the equipment selection, detectors and quality assurance for gamma-ray spectrometry can be found in ISO 20042:2016. The current standard aims to be complementary to existing standards, as an aid to laboratory practitioners that are faced with a situation, which requires response to the current topic without having to go through and interpret standards with general descriptions of gamma-ray spectrometry in order to measure in a standardised way. This standard contains information specific to the three radionuclides that it covers. Examples are provided in Annex …(to be added).
- Standard34 pagesEnglish languagesale 10% offe-Library read for1 day
- Draft35 pagesEnglish languagesale 10% offe-Library read for1 day
This document specifies a procedure for the determination of inorganic arsenic in animal feeding stuffs by anion-exchange HPLC-ICP-MS following water bath extraction.
This method was successfully tested in the range of 0,149 mg/kg to 9,69 mg/kg in the following animal feed matrices: rice meal, seaweed meal, fish meal, grass meal, complete feed (marine-based), complete feed (cereal based) and a synthetic solution.
NOTE Mineral feed matrices are not included in the scope of this method. It is good to perform a determination of the total arsenic content in such matrices.
- Standard14 pagesEnglish languagesale 10% offe-Library read for1 day
- Draft13 pagesEnglish languagesale 10% offe-Library read for1 day
This document specifies a liquid chromatographic method with triple-quadrupole mass spectrometry (MS/MS) detection for the determination of pentachlorophenol (PCP) in feed materials and animal feed.
The limit of quantitation (LOQ) for the PCP determination in guar gum, fatty acid distillates (FAD) and animal feed is 10 µg/kg. Individual laboratories are responsible for ensuring that the equipment that they use will achieve this limit of quantification.
The method is validated in an international collaborative trial for pentachlorophenol in compound feed, guar gum and fatty acid distillate in the range between 9 µg/kg and 22 µg/kg.
The results of the collaborative trial, in which 16 laboratories participated, have shown that the method is applicable for the determination of PCP in compound feed, guar gum and FAD at the desired limit of 10 µg/kg. Satisfactory results were obtained for one compound feed sample, guar gum and the two FAD samples (HorRat <2), while for the second compound feed sample a HorRat value of 2,2 was obtained.
- Standard19 pagesEnglish languagesale 10% offe-Library read for1 day
- Draft18 pagesEnglish languagesale 10% offe-Library read for1 day
This document specifies a gas chromatographic method with electron capture detection (ECD) for the determination of organochlorine pesticides (OCPs) in compound feeds and oil and fats.
The method is applicable to animal compound feed, oils and fats and fish meals with a water content up to about 20 % by weight and oil/fatty samples containing residues of one or more of the following OCPs, toxaphene and some of their isomers and degradation products:
— aldrin;
— dieldrin;
— dichlorodiphenyltrichloroethane (DDT) (the isomers op'-DDT, pp'-DDT, pp'-TDE (pp'-DDD), and pp'-DDE);
— endosulfan (as the sum of α-/β-isomers);
— endrin;
— hexachlorobenzene (HCB);
— hexachlorocyclohexane isomers α-HCH (α-BHC), β-HCH (β-BHC), γ-HCH (γ-BHC or lindane);
For the following OCPs, the method is considered a screening method. Additional in-house validation is required for reporting validated data.
— chlordane (as the sum of chlordane isomers and oxychlordane);
— endosulfan-sulphate;
— delta-keto-endrin;
— heptachlor (as the sum of heptachlor and heptachlor epoxide);
— photo-heptachlor;
— cis
— and trans-nonachlor.
A limit of quantification (LOQ) for the mentioned OCPs of 5 µg/kg is intended to be obtained. However, 10 µg/kg applies for heptachlor, aldrin, endrin, dieldrin, and endosulfan (α-/β– and sulphate). Individual laboratories are responsible for ensuring that the equipment that they use, achieves these limits of quantifications. The LOQs apply to the individual OCPs.
- Standard23 pagesEnglish languagesale 10% offe-Library read for1 day
- Draft25 pagesEnglish languagesale 10% offe-Library read for1 day
This document specifies a gas chromatographic mass spectrometric (GC/MS) method for the determination of organochlorine pesticides (OCPs) and polychlorinated biphenyls (PCBs) in animal feeding stuffs and oil.
The method is applicable to animal feeding stuffs consisting of less than 20 % by mass and oil/fatty samples containing residues of one or more of the following OCPs and PCBs and some of their isomers and degradation products:
aldrin;
dieldrin;
chlordane, as the sum of chlordane isomers and oxychlordane;
dichlorodiphenyltrichloroethane (DDT), as the sum of isomers op'-DDT, pp'-DDT, pp'-TDE (pp'-DDD), and pp'-DDE;
endosulfan, as the sum of α-/β-isomers and endosulfan-sulphate;
endrin, as the sum of endrin and delta-keto-endrin;
heptachlor, as the sum of heptachlor and heptachlor epoxide;
hexachlorobenzene (HCB);
hexachlorocyclohexane isomers α-HCH (α-BHC), β-HCH (β-BHC), γ-HCH (γ-BHC or lindane);
photo heptachlor;
cis- and trans-nonachlor;
non dioxin-like PCBs (ndl-PCBs), as the sum of PCB 28, 52, 101, 138, 153 and 180.
The method has been fully validated by a collaborative trial for the substances and corresponding ranges (ng/g) noted in Table 1.
The method has not been fully validated for oxychlordane, endrin ketone, cis- and trans-nonachlor and photo heptachlor in all matrices.
The method is not applicable to chlorocamphene (toxaphene), a complex mixture of polychlorinated camphenes. Chlorocamphene has a very distinctive chromatographic profile and is easily recognisable by GC/ECD. Positive identification of the toxaphene isomers can be performed by negative chemical ionisation mass spectrometry (NCI-MS), electron impact tandem mass spectrometry (EI MS × MS) or electron impact high resolution mass spectrometry (EI-HRMS), which is not within the scope of this method.
A limit of quantification (LOQ) for the mentioned organochlorine pesticides of 5 ng/g should normally be obtained. However, 10 ng/g applies for heptachlor aldrin, endrin, dieldrin, and endosulfan (α-, β- and sulphate). For the ndl-PCBs an LOQ of 0,5 to 1,0 ng/g should be obtained. The LOQs mentioned apply to the individual compounds (i.e. not the sum of two or more compounds). Individual laboratories are responsible for ensuring that the equipment that they used will achieve these LOQs. On customers' demand the standard may be applied to solely the analysis of PCBs or OCPs.
- Standard48 pagesEnglish languagesale 10% offe-Library read for1 day
- Draft60 pagesEnglish languagesale 10% offe-Library read for1 day
This document is applicable to the determination of polychlorinated dibenzo-p-dioxins (PCDDs), polychlorinated dibenzofurans (PCDFs), (together termed ‘dioxins’ (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
- 0,05 pg/g (OCDD/F = 0,1 pg/g) for the relevant individual congeners of dioxins/furans,
- 0,05 pg/g for non-ortho PCBs,
- 10 pg/g for mono-ortho PCBs, and
- 100 pg/g for non-dioxin-like-PCBs.
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]. 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 [2]) provided that appropriate analytical performance criteria are met in the relevant range for the matrix of interest.
This document is split into four modules. Each module describes a part of the whole procedure (see Figure 1 and Figure 2) to be followed:
a) Module A: Description of standards which might be used;
b) Module B: Description of extraction procedures;
c) Module C: Description of clean-up procedures;
d) Module D: GC/HRMS determination.
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, "performance based" procedure. It is permitted to modify the method if all performance criteria laid down in Commission Regulation (EC) No 152/2009 [1] are met.
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.
Figure 1 - Flow scheme for the determination of dioxins, dl-PCBs and non-dioxin-like-PCBs in feed
Figure 2 - Flow scheme for the determination of dioxins, dl-PCBs and non-dioxin-like-PCBs in oil and fat
- Standard55 pagesEnglish languagesale 10% offe-Library read for1 day
- Draft54 pagesEnglish languagesale 10% offe-Library read for1 day
This method procedure describes a procedure for the determination of inorganic arsenic in animal feeding stuffs by anion-exchange HPLC-ICP-MS following water bath extraction.
- Standard14 pagesEnglish languagesale 10% offe-Library read for1 day
- Draft13 pagesEnglish languagesale 10% offe-Library read for1 day
This document specifies performance criteria for the selection of single-laboratory validated or collaborative study validated methods of analysis of mycotoxins in feed. The terms and definition of the relevant parameters for method validation are included. The performance requirements and characteristics are provided. This document could serve as a guide:
— to assess the quality of new European Standard methods under validation;
— to review the quality of previous collaborative trials;
— to confirm the extension of the scope of an already published European Standard applied to other analyte concentrations or matrices; or
— to evaluate the fitness-for-purpose of single-validated methods.
The performance criteria can apply to methods dedicated to the determination of mycotoxins.
- Technical specification25 pagesEnglish languagesale 10% offe-Library read for1 day
- Draft26 pagesEnglish languagesale 10% offe-Library read for1 day
This document specifies a liquid chromatographic method with triple-quadrupole mass spectrometry (MS/MS) detection for the determination of pentachlorophenol (PCP) in feed materials and animal feed.
The limit of quantitation (LOQ) for the PCP determination in guar gum, fatty acid distillates (FAD) and animal feed is 10 µg/kg. Individual laboratories are responsible for ensuring that the equipment that they use will achieve this limit of quantification.
The method is validated in an international collaborative trial for pentachlorophenol in compound feed, guar gum and fatty acid distillate in the range between 9 µg/kg and 22 µg/kg.
The results of the collaborative trial, in which 16 laboratories participated, have shown that the method is applicable for the determination of PCP in compound feed, guar gum and FAD at the desired limit of 10 µg/kg. Satisfactory results were obtained for one compound feed sample, guar gum and the two FAD samples (HorRat <2), while for the second compound feed sample a HorRat value of 2,2 was obtained.
- Standard19 pagesEnglish languagesale 10% offe-Library read for1 day
- Draft18 pagesEnglish languagesale 10% offe-Library read for1 day
This document's method of analysis is applicable for the determination of:
- deoxynivalenol (DON) in the tested range of 100 µg/kg to 3 300 µg/kg,
- aflatoxin B1 (AfB1) in the tested range of 2,5 µg/kg to 440 µg/kg,
- fumonisin B1 (FB1) in the tested range of 690 µg/kg to 7 500 µg/kg,
- fumonisin B2 (FB2) in the tested range of 200 µg/kg to 2 500 µg/kg,
- T-2 toxin in the tested range of 7,5 µg/kg to 360 µg/kg,
- HT-2 toxin in the tested range of 14 µg/kg to 1 800 µg/kg,
- zearalenone (ZEN) in the tested range of 30 µg/kg to 600 µg/kg, and
- ochratoxin A (OTA) in the tested range of 10 µg/kg to 230 µg/kg
in cereals and cereal-based compound feed by liquid-chromatography tandem mass spectrometry (LC-MS/MS). The actual working ranges could extend beyond the tested ranges.
- Standard32 pagesEnglish languagesale 10% offe-Library read for1 day
This document method is applicable for the determination of theobromine in compound feed by liquid chromatography with UV detection in the tested range of 27 to 307 mg/kg. This method has been validated using complementary compound feed for adult dogs and complementary compound feedstuff for horses. The actual working range may extend beyond the tested range. Alternative chromatography conditions using liquid chromatography tandem mass spectrometry (LC-MS/MS) are also provided for the validated range of 49 to 307 mg/kg. This method has also been shown to be fit for purpose for the determination of theobromine in baking chocolate by both HPLC-UV and LC-MS/MS.
- Standard23 pagesEnglish languagesale 10% offe-Library read for1 day
- Draft25 pagesEnglish languagesale 10% offe-Library read for1 day
This document describes a method for the determination of individual ergot alkaloids and tropane alkaloids in unprocessed cereals and cereal-based compound feeds by high performance liquid chromatography with tandem mass spectrometry (LC-MS/MS).
This method has been successfully validated by collaborative trial in the following matrices: rye, barley, wheat, complete feed for bovine, porcine and poultry. Validation in buckwheat produced acceptable results, but the relative standard reproducibility was higher for most analytes in comparison with the other matrices. This may be related to the matrix. The validated range of the method is approximately 10 to 250 µg/kg for individual alkaloids. Determination of concentrations above 250 µg/kg is possible by applying a higher spiking level and dilution of the sample extract, but this has not been validated in the collaborative trial.
The method is applicable for the determination, by means of one-point standard addition to the sample, of ergocornine in the tested range of 12 µg/kg to 221 µg/kg, ergocorninine in the tested range of 9 µg/kg to 196 µg/kg, ergocristine in the tested range of 14 µg/kg to 312 µg/kg, ergocristinine in the tested range of 12 µg/kg to 258 µg/kg, α-ergocryptine in the tested range of 10 µg/kg to 184 µg/kg, α-ergocryptinine in the tested range of 8 µg/kg to 171 µg/kg, ergometrine in the tested range of 12 µg/kg to 174 µg/kg, ergometrinine in the tested range of 3 µg/kg to 172 µg/kg, ergosine in the tested range of 12 µg/kg to 226 µg/kg, ergosinine in the tested range of 9 µg/kg to 273 µg/kg, ergotamine in the tested range of 11 µg/kg to 443 µg/kg, ergotaminine in the tested range of 10 µg/kg to 273 µg/kg, atropine in the tested range of 16 µg/kg to 252 µg/kg and scopolamine in the tested range of 15 µg/kg to 246 µg/kg.
- Standard38 pagesEnglish languagesale 10% offe-Library read for1 day
- Draft39 pagesEnglish languagesale 10% offe-Library read for1 day
This document specifies performance criteria for the selection of single-laboratory validated or collaborative study validated methods of analysis of mycotoxins in feed. The terms and definition of the relevant parameters for method validation are included. The performance requirements and characteristics are provided. This document could serve as a guide:
- to assess the quality of new European Standard methods under validation;
- to review the quality of previous collaborative trials;
- to confirm the extension of the scope of an already published European Standard applied to other analyte concentrations or matrices; or
- to evaluate the fitness-for-purpose of single-validated methods.
The performance criteria can apply to methods dedicated to the determination of mycotoxins.
- Technical specification25 pagesEnglish languagesale 10% offe-Library read for1 day
- Draft26 pagesEnglish languagesale 10% offe-Library read for1 day
This document specifies a gas chromatographic method with electron capture detection (ECD) for the determination of organochlorine pesticides (OCP’s) in animal feeding stuffs.
The method is applicable to animal feeding stuffs with a water content up to about 20 % by weight and oil/fatty samples containing residues of one or more of the following OCP’s, toxaphene and some of their isomers and degradation products:
aldrin;
dieldrin;
chlordane (as the sum of chlordane isomers and oxychlordane);
dichlorodiphenyltrichloroethane (DDT) (as the sum of isomers op'-DDT, pp'-DDT, pp'-TDE (pp'-DDD), and pp'-DDE);
endosulfan (as the sum of α-/β-isomers and endosulfan-sulphate);
endrin (sum of endrin and delta-keto-endrin);
heptachlor (as the sum of heptachlor and heptachlor epoxide);
hexachlorobenzene (HCB);
hexachlorocyclohexane isomers α-HCH (α-BHC), β-HCH (β-BHC), γ-HCH (γ-BHC or lindane);
photo heptachlor;
cis- and trans-nonachlor;
A limit of quantification (LOQ) for the mentioned OCPs of 5 ng/g should normally be obtained. However, 10 ng/g applies for heptachlor, aldrin, endrin, dieldrin, and endosulfan (α-/β-- and sulphate). Individual laboratories are responsible for ensuring that the equipment that they use, achieves these limits of quantifications. The LOQs apply to the individual OCPs.
- Standard23 pagesEnglish languagesale 10% offe-Library read for1 day
- Draft25 pagesEnglish languagesale 10% offe-Library read for1 day
This document specifies a gas chromatographic mass spectrometric (GC/MS) method for the determination of organochlorine pesticides (OCPs) and polychlorinated biphenyls (PCBs) in animal feeding stuffs and oil.
The method is applicable to animal feeding stuffs consisting of less than 20 % by mass and oil/fatty samples containing residues of one or more of the following OCPs and PCBs and some of their isomers and degradation products:
aldrin;
dieldrin;
chlordane, as the sum of chlordane isomers and oxychlordane;
dichlorodiphenyltrichloroethane (DDT), as the sum of isomers op'-DDT, pp'-DDT, pp'-TDE (pp'-DDD), and pp'-DDE;
endosulfan, as the sum of α-/β-isomers and endosulfan-sulphate;
endrin, as the sum of endrin and delta-keto-endrin;
heptachlor, as the sum of heptachlor and heptachlor epoxide;
hexachlorobenzene (HCB);
hexachlorocyclohexane isomers α-HCH (α-BHC), β-HCH (β-BHC), γ-HCH (γ-BHC or lindane);
photo heptachlor;
cis- and trans-nonachlor;
non dioxin-like PCBs (ndl-PCBs), as the sum of PCB 28, 52, 101, 138, 153 and 180.
The method has been fully validated by a collaborative trial for the substances and corresponding ranges (ng/g) noted in Table 1.
The method has not been fully validated for oxychlordane, endrin ketone, cis- and trans-nonachlor and photo heptachlor in all matrices.
The method is not applicable to chlorocamphene (toxaphene), a complex mixture of polychlorinated camphenes. Chlorocamphene has a very distinctive chromatographic profile and is easily recognisable by GC/ECD. Positive identification of the toxaphene isomers can be performed by negative chemical ionisation mass spectrometry (NCI-MS), electron impact tandem mass spectrometry (EI MS × MS) or electron impact high resolution mass spectrometry (EI-HRMS), which is not within the scope of this method.
A limit of quantification (LOQ) for the mentioned organochlorine pesticides of 5 ng/g should normally be obtained. However, 10 ng/g applies for heptachlor aldrin, endrin, dieldrin, and endosulfan (α-, β- and sulphate). For the ndl-PCBs an LOQ of 0,5 to 1,0 ng/g should be obtained. The LOQs mentioned apply to the individual compounds (i.e. not the sum of two or more compounds). Individual laboratories are responsible for ensuring that the equipment that they used will achieve these LOQs. On customers' demand the standard may be applied to solely the analysis of PCBs or OCPs.
- Standard48 pagesEnglish languagesale 10% offe-Library read for1 day
- Draft60 pagesEnglish languagesale 10% offe-Library read for1 day
This document specifies a high-performance liquid chromatographic (HPLC) mass spectrometric (MS) method for screening and quantification of melamine and cyanuric acid in the concentration range between 1 mg/kg and 100 mg/kg feed.
The method is validated in an international collaborative trial for melamine in complete feed, complementary feed, feed material, milk replacer and pet food including canned pet food in the range between 1 mg/kg and 80 mg/kg with particular regard to the maximum level of 2,5 mg/kg as established by the European Commission.
Laboratory experiences have shown that the method is also applicable for cyanuric acid in the same concentration range in complete feed (n = 7), complementary feed (n = 6), feed material (n = 7, resp. 9), milk replacer (n = 7) and pet food (n = 7) including canned pet food.
Since the LC-MS/MS sensitivity for cyanuric acid is lower than for melamine, it has to be ensured that the LC-MS/MS system is in excellent working order. The method is applicable to feeding stuffs but not tested for pre-mixtures and feed additives.
Quantification of concentrations above 100 mg/kg is possible, but the method has to be validated by the operator.
- Standard37 pagesEnglish languagesale 10% offe-Library read for1 day
This document specifies requirements for light fire storage units providing protection against fire.
The method of test is specified to determine the ability of light fire storage units to protect paper media from the effects of fire. Two levels of fire exposure periods (LFS 30 and LFS 60) are specified using the maximum temperature increase permitted within the storage space of the light fire storage unit.
Protection after the fire exposure of 30 min (LFS 30) or 60 min (LFS 60) is not ensured by this document, but by European Standard EN 1047-1. Requirements are also specified for the test specimen, the technical documentation for the test specimen, correlation of the test specimen with the technical documentation, preparation for type testing and test procedures.
A scheme to classify the light fire storage units from the test results is also given (see Table 1).
- Standard54 pagesEnglish languagesale 10% offe-Library read for1 day
- Draft51 pagesEnglish languagesale 10% offe-Library read for1 day
This document specifies a method for the determination of organic acids in animal feeding stuffs by Ion Chromatography with conductivity detection (IC-CD).
The method is intended to be used for the determination of formic acid, lactic acid, propionic acid, citric acid, fumaric acid and malic acid as active substances in feed additives, premixtures, feed materials, compound feed and water and for acetic acid in a limited manner in the same matrices. This method determines the total extractable concentration of the above mentioned organic acids and their salts.
It is advisable that the user of this standard determines the working range of the method for each organic acid. The lower limit of the working range depends on the matrix and the interferences encountered. It is advisable that a working range between 10 mg/l and 100 mg/l is achievable.
The method was successfully tested in an inter-laboratory study in concentrations between 0,02 % up to 27 % of the above mentioned organic acids.
NOTE Limitation occurs during simultaneous determination of high concentration of lactic acid and low concentration of acetic acid. If the ratio of concentration of lactic acid to acetic acid exceeds factor 20, the determination of acetic acid is not guaranteed.
On the basis of the referred working range, sample weight and extraction volume, limits of quantification (LOQ), as calculated (Table 1) can be achievable.
- Standard33 pagesEnglish languagesale 10% offe-Library read for1 day
- Draft34 pagesEnglish languagesale 10% offe-Library read for1 day