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).

  • Standard
    34 pages
    English language
    sale 10% off
    e-Library read for
    1 day
  • Draft
    35 pages
    English language
    sale 10% off
    e-Library read for
    1 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.

  • Standard
    14 pages
    English language
    sale 10% off
    e-Library read for
    1 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.

  • Standard
    19 pages
    English language
    sale 10% off
    e-Library read for
    1 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 specification
    25 pages
    English language
    sale 10% off
    e-Library read for
    1 day
  • Technical specification
    26 pages
    English language
    sale 10% off
    e-Library read for
    1 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.

  • Standard
    23 pages
    English language
    sale 10% off
    e-Library read for
    1 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.

  • Standard
    48 pages
    English language
    sale 10% off
    e-Library read for
    1 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.

  • Standard
    23 pages
    English language
    sale 10% off
    e-Library read for
    1 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.

  • Standard
    48 pages
    English language
    sale 10% off
    e-Library read for
    1 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

  • Standard
    55 pages
    English language
    sale 10% off
    e-Library read for
    1 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

  • Standard
    55 pages
    English language
    sale 10% off
    e-Library read for
    1 day

This European Standard method of analysis is applicable for the determination of Deoxynivalenol (DON) in the tested range of 96,2 µg/kg to 3 269 µg/kg, Aflatoxin B1 (AfB1) in the tested range of 2,62 µg/kg to 444 µg/kg, Fumonisin B1 (FB1) in the tested range of 693 µg/kg to 7 529 µg/kg, Fumonisin B2 (FB2) in the tested range of 203 µg/kg to 2 465 µg/kg, T-2 toxin in the tested range of 7,47 µg/kg to 360 µg/kg and HT-2 toxin in the tested range of 13,9 µg/kg to 1 758 µg/kg, Zearalenone (ZON) in the tested range of 34,3 µg/kg to 593 µg/kg and Ochratoxin A (OTA) in the tested range of 10,8 µg/kg to 228 µg/kg in cereals and cereal-based compound feed by liquid-chromatography tandem mass spectrometry (LC-MS/MS). The actual working ranges may extend beyond the tested ranges.

  • Standard
    32 pages
    English language
    sale 10% off
    e-Library read for
    1 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.

  • Standard
    23 pages
    English language
    sale 10% off
    e-Library read for
    1 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 coupled with tandem mass spectrometry (LC-MS/MS). The ergot alkaloids covered in this method are: ergocornine, ergocorninine, ergocristine, ergocristinine, α-ergocryptine, α-ergocryptinine, ergometrine, ergometrinine, ergosine, ergosinine, ergotamine and ergotaminine. The tropane alkaloids covered in this method are: atropine (hyoscyamine) and scopolamine. The limit of quantification for all compounds should be at least 10 µg/kg.
This method has been in-house validated in the range 10 - 500 µg/kg for individual alkaloids. The detection of concentrations above 500 µg/kg is possible via dilution of the sample extract, but this has not been validated.

  • Standard
    38 pages
    English language
    sale 10% off
    e-Library read for
    1 day

This document gives guidance to those involved in designing, executing and evaluating interlaboratory comparison studies for multi-analyte methods of analysis, developed by CEN/TC 327 “Animal feeding stuffs: Methods of sampling and analysis” and its working groups.
For the validation of multi-analyte methods their particularities must be considered which might necessitate deviations from the prescribed validation protocols. This study provides information whether the method is fit for its purpose and which performance can be expected in practical work while at the same time keeping the necessary effort for the study organizer and the participating laboratories minimal.
Next to the abovementioned aspects regarding interlaboratory comparison studies, this document also gives guidance on the preceding steps, viz. in-house validation and preparation of the method protocol. Guidance is also given on the transferability of the method protocol and the familiarization with the method protocol through a training study, elements that – depending on the specific method – could be included in the design of the study.

  • Technical report
    12 pages
    English language
    sale 10% off
    e-Library read for
    1 day
  • Technical report
    12 pages
    English language
    sale 10% off
    e-Library read for
    1 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.

  • Standard
    32 pages
    English language
    sale 10% off
    e-Library read for
    1 day

This document defines terms relating to animal feeding stuffs. NOTE It includes the most common and frequently used terms in the field of animal feeding stuffs.

  • Standard
    14 pages
    English language
    sale 15% off

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.

  • Standard
    23 pages
    English language
    sale 10% off
    e-Library read for
    1 day

This document specifies a high-performance liquid chromatographic (HPLC) mass spectrometric (MS) method for screening and quantification of melamine 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 by the European Commission established maximum level of 2,5 mg/kg.
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 substantially 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.

  • Standard
    37 pages
    English language
    sale 10% off
    e-Library read for
    1 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.

  • Standard
    38 pages
    English language
    sale 10% off
    e-Library read for
    1 day

This document gives guidance to those involved in designing, executing and evaluating interlaboratory comparison studies for multi-analyte methods of analysis, developed by CEN/TC 327 “Animal feeding stuffs: Methods of sampling and analysis” and its working groups.
For the validation of multi-analyte methods their particularities must be considered which might necessitate deviations from the prescribed validation protocols. This study provides information whether the method is fit for its purpose and which performance can be expected in practical work while at the same time keeping the necessary effort for the study organizer and the participating laboratories minimal.
Next to the abovementioned aspects regarding interlaboratory comparison studies, this document also gives guidance on the preceding steps, viz. in-house validation and preparation of the method protocol. Guidance is also given on the transferability of the method protocol and the familiarization with the method protocol through a training study, elements that – depending on the specific method – could be included in the design of the study.

  • Technical report
    12 pages
    English language
    sale 10% off
    e-Library read for
    1 day
  • Technical report
    12 pages
    English language
    sale 10% off
    e-Library read for
    1 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.

  • Standard
    37 pages
    English language
    sale 10% off
    e-Library read for
    1 day

This document specifies a high performance liquid chromatographic – tandem mass spectrometry (LC-MS/MS) method for the simultaneous screening and/or determination of the eleven authorised coccidiostats (halofuginone, robenidine hydrochloride, nicarbazin, diclazuril, decoquinate, monensin sodium, salinomycin sodium, narasin, lasalocid sodium, semduramicin sodium and maduramicin ammonium alpha) contents in poultry, cattle and pig feed at additive and cross-contamination levels and of five non-registered coccidiostats (ethopabate, clopidol, ronidazole, dimetridazole and amprolium) at sub-additive levels and for the screening of the prohibited furazolidone antibiotic at sub-additive level, in the same matrices.
The range of application of the method is fit for the purpose of the screening and determination of all eleven coccidiostats at the values set by European legislation, of the non-registered coccidiostats and of the screening of the banned antibiotic.

  • Standard
    54 pages
    English language
    sale 10% off
    e-Library read for
    1 day

This document specifies a method for the determination of benzoic acid and sorbic acid in animal feeding stuffs by high-performance liquid chromatography method with ultra-violet detection (HPLC-UV).
The method is intended to be used for the determination of benzoic acid and sorbic acid as active substances in feed additives, premixtures and compound feed and for benzoic acid in water. This method determines the total extractable concentration of these organic acids and their salts.
The working range of the method must be determined for each organic acid by the user of this standard. The lower limit of the working range depends on the matrix and the interferences encountered. A working range between 5 mg/l and 100 mg/l should be accessible.
The method was successfully tested in an inter-laboratory study in concentrations between 0,02 % up to 9,0 %.
On the basis of the referred working range, sample weigh and extraction volume, limits of quantification (LOQ), as calculated (Table 1) on the basis of a wavelength of 230 nm, should be achievable.

  • Standard
    18 pages
    English language
    sale 10% off
    e-Library read for
    1 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, compound feed and water and for screening of acetic acid in the same matrices. This method determines the total extractable concentration of the above mentioned organic acids and their salts.
The working range of the method must be determined for each organic acid by the user of this standard. The lower limit of the working range depends on the matrix and the interferences encountered. A working range between 10 [mg/l] and 100 [mg/l] should be 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) should be achievable.

  • Standard
    33 pages
    English language
    sale 10% off
    e-Library read for
    1 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.

  • Standard
    33 pages
    English language
    sale 10% off
    e-Library read for
    1 day

This document specifies a method for the determination of benzoic acid and sorbic acid in animal feeding stuffs by high-performance liquid chromatography method with ultraviolet detection (HPLC-UV).
The method is intended to be used for the determination of benzoic acid and sorbic acid as active substances in feed additives, premixtures, feed materials and compound feed and for benzoic acid in water. This method determines the total extractable concentration of these organic acids and their salts.
It is advisable that the working range of the method is determined for each organic acid by the user of this standard. The lower limit of the working range depends on the matrix and the interferences encountered. It is advisable that a working range between 5 mg/l and 100 mg/l is accessible.
The method was successfully tested in an inter-laboratory study in concentrations between 0,02 % up to 9,0 %.
On the basis of the referred working range, sample weight and extraction volume, limits of quantification (LOQ), as calculated (Table 1) on the basis of a wavelength of 230 nm, can be achievable.

  • Standard
    18 pages
    English language
    sale 10% off
    e-Library read for
    1 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).

  • Standard
    54 pages
    English language
    sale 10% off
    e-Library read for
    1 day

This part of ISO 6495 specifies a method for the determination of water-soluble chloride content,
expressed as sodium chloride, of animal feeding stuffs.
This method is applicable to animal feeding stuffs containing water-soluble chloride content, expressed
as sodium chloride, ≥0,05 %.

  • Standard
    9 pages
    English language
    sale 15% off
  • Standard
    13 pages
    English language
    sale 10% off
    e-Library read for
    1 day
  • Standard
    9 pages
    French language
    sale 15% off

This document specifies performance criteria for the selection of single-laboratory validated or collaborative-trial validated methods of analysis of elements and their chemical species in feed. The terms and definition of the relevant parameters for method validation are included. The performance requirements and characteristics are provided. This document may 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 heavy metals, trace elements, major elements and minerals.

  • Technical specification
    26 pages
    English language
    sale 10% off
    e-Library read for
    1 day

This document specifies performance criteria for the selection of single-laboratory validated or collaborative-trial validated methods of analysis of elements and their chemical species in feed. The terms and definition of the relevant parameters for method validation are included. The performance requirements and characteristics are provided. This document may 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 heavy metals, trace elements, major elements and minerals.

  • Technical specification
    26 pages
    English language
    sale 10% off
    e-Library read for
    1 day

This document specifies a method of determining the urease activity of products derived from soya beans. The method allows inadequate cooking of these products to be detected. It is applicable to products having a urease activity of less than 1 mg of nitrogen per gram of product as received, under the conditions specified. For more active products, the method is applicable provided that the mass of the test portion is reduced (see 9.1).

  • Standard
    5 pages
    English language
    sale 15% off
  • Standard
    5 pages
    French language
    sale 15% off

This European standard specifies a high performance liquid chromatography- mass spectrometry (LC-MS/MS) method for the identification of tylosin, spiramycin, virginiamycin, carbadox and olaquindox in animal feeds.
The method is suitable for the identification of low concentrations of tylosin, spiramycin, virginiamycin, carbadox and olaquindox in compound animal feeds. A limit of identification of 1 mg/kg for tylosin, spiramycin and virginiamycin, 4 mg/kg for carbadox and 3 mg/kg for olaquindox should be obtained by using the described method. The method was fully validated during a collaborative study (see Annex A).
Since tylosin, spiramycin and virginiamycin are fermentation products consisting of a mixture of several closely related compounds, the analysis is based on detection and identification of the most abundant constituents. For tylosin the marker is tylosin A, for spiramycin the marker is spiramycin I and II and for virginiamycin the marker is virginiamycin M1 and S1. The other isomers and forms can be readily detected with the same method but adjustment of the MS parameters according to the molecular mass of precursor and product ions need to be made. Carbadox and olaquindox are analysed as such.

  • Standard
    33 pages
    English language
    sale 10% off
    e-Library read for
    1 day

This European Standard specifies a high performance liquid chromatography - mass spectrometry (LC-MS/MS) method for the identification of tylosin, spiramycin, virginiamycin, carbadox and olaquindox in animal feeds.
The method is suitable for the identification of low concentrations of tylosin, spiramycin, virginiamycin, carbadox and olaquindox in compound animal feeds. A limit of identification of 1 mg/kg for tylosin, spiramycin and virginiamycin, 4 mg/kg for carbadox and 3 mg/kg for olaquindox should be obtained by using the described method. The method was fully validated during a collaborative study (see Annex A).
Since tylosin, spiramycin and virginiamycin are fermentation products consisting of a mixture of several closely related compounds, the analysis is based on detection and identification of the most abundant constituents. For tylosin the marker is tylosin A, for spiramycin the marker is spiramycin I and II and for virginiamycin the marker is virginiamycin M1 and S1. The other isomers and forms can be readily detected with the same method but adjustment of the MS parameters according to the molecular mass of precursor and product ions need to be made. Carbadox and olaquindox are analysed as such.

  • Standard
    33 pages
    English language
    sale 10% off
    e-Library read for
    1 day

This European Standard specifies a method for the determination of trace elements, heavy metals and other elements in animal feed by ICP-MS. The method is used to determine As, Cd, Co, Cu, Fe, Hg, Mn, Mo, Pb, Se, Tl, U and Zn in the extraction solution after pressurised digestion. For the determination of extractable lead in minerals and feeds containing phyllosilicates (e.g. kaolinite clay) wet digestion with nitric acid should be used. The method described is suitable for use in quadrupole instruments equipped either with or without additional technology to reduce molecular ion interferences (e.g. collision or reaction technologies) as well as in high-resolution sector-field systems.
The method was fully statistically tested and evaluated in a collaborative trial comprising eight animal feeding stuff samples for the elements As, Cd, Co, Cu, Fe, Hg, Mn, Mo, Pb, Se, Tl, U and Zn. High-resolution sector-field ICP-MS was not tested in the validation ring trial.
The limit of quantification for each element is dependent on the sample matrix as well as the instrument. For the elements Co, Mn, Mo, Pb, Tl, U a limit of quantification of 0,10 mg/kg should normally be obtained, for the elements Fe and Zn 5,0 mg/kg, while for Cd 0,03 mg/kg, Hg 0,04 mg/kg and As 0,05 mg/kg should normally be quantifiable.
Details on the successfully tested working range for each element are described in this standard.

  • Standard
    29 pages
    English language
    sale 10% off
    e-Library read for
    1 day

This European Standard specifies a method for the determination of trace elements, heavy metals and other elements in animal feed by inductively coupled plasma mass spectrometry (ICP-MS). The method is used to determine As, Cd, Co, Cu, Fe, Hg, Mn, Mo, Pb, Se, Tl, U and Zn in the extraction solution after pressurized digestion. For the determination of extractable lead in minerals and feeds containing phyllosilicates (e.g. kaolinite clay) wet digestion with nitric acid should be used. The method described is suitable for use in quadrupole instruments equipped either with or without additional technology to reduce molecular ion interferences (e.g. collision or reaction technologies) as well as in high-resolution sector-field systems.
The method was fully statistically tested and evaluated in a collaborative trial comprising eight animal feeding stuff samples for the elements As, Cd, Co, Cu, Fe, Hg, Mn, Mo, Pb, Se, Tl, U and Zn. For elements with a HORRAT value higher than 2 (e.g. mercury, see Annex A) the method is more applicable as a screening method and not for confirmatory purposes. High-resolution sector-field ICP-MS was not tested in the validation ring trial.
The limit of quantification for each element is dependent on the sample matrix as well as the instrument. For the elements Co, Mn, Mo, Pb, Tl, U a limit of quantification of 0,10 mg/kg should normally be obtained, for the elements Fe and Zn 5,0 mg/kg, while for Cd 0,03 mg/kg, Hg 0,04 mg/kg and As 0,05 mg/kg should normally be quantifiable.
Details on the successfully tested working range for each element are described in this standard.

  • Standard
    29 pages
    English language
    sale 10% off
    e-Library read for
    1 day

This document gives guidelines for the determination by near infrared spectroscopy of constituents
such as moisture, fat, protein, starch and crude fibre and parameters such as digestibility in animal
feeding stuffs, cereals and milled cereal products.
The determinations are based on spectrometric measurement in the near infrared spectral region.

  • Standard
    36 pages
    English language
    sale 10% off
    e-Library read for
    1 day

This European standard specifies a method for the determination of iodine in animal feeding stuffs by inductively coupled plasma mass spectrometry (ICP-MS) following extraction with an alkaline solution.
This method was successfully tested in the range of 0,70 to 631 mg/kg in following animal feeds: seaweed meal, mineral premixture, fish meal, plant based ingredient, marine based compound feed and a synthetic iodine solution.

  • Standard
    15 pages
    English language
    sale 10% off
    e-Library read for
    1 day

ISO 12099:2017 gives guidelines for the determination by near infrared spectroscopy of constituents such as moisture, fat, protein, starch and crude fibre and parameters such as digestibility in animal feeding stuffs, cereals and milled cereal products.
The determinations are based on spectrometric measurement in the near infrared spectral region.

  • Standard
    36 pages
    English language
    sale 10% off
    e-Library read for
    1 day

The method makes it possible to detect and identify spiramycin, tylosin and virginiamycin in animal feeding stuffs (feed raw materials of mainly plant origin and compound feeds) excluding mineral feeds and premixtures. The limit of detection is about 2 mg/kg for spiramycin, 1 mg/kg for tylosin and 1 mg/kg for virginiamycin. In some milk replacers, it can be slightly higher than 1 mg/kg for virginiamycin.
NOTE    Reported limits of detection are probably little overestimated but were fully validated during the collaborative study (see Annex B). In each laboratory, each day of analysis, spiked blank samples at 1 mg/kg for spiramycin and virginiamycin and at 0,5 mg/kg for tylosin are analysed for checking lower detection limits (see 9.2 and 9.3). These lower limits of detection are achievable, but should be established with an in-house validation first.
Some other antibiotics may interfere in the detection of these 3 specific macrolide antibiotics. The known interferences are specified in Annex A of the method.
That method should be used as a qualitative screening and/or a post-screening method (after microbiological plate test, for example). The follow-up of the antibiotics presence may be done by other analytical technics (LC and/or LC-MS technics) [4] [9]. For confirmatory purposes, LCMS is required.

  • Standard
    26 pages
    English language
    sale 10% off
    e-Library read for
    1 day

This European Standard specifies a method for the determination of the elements cadmium and lead in animal feeding stuffs by graphite furnace atomic absorption spectrometry (GF-AAS) after pressure digestion.
The method was successfully tested in the range of 0,015 to 5,65 mg/kg for Cd and 0,18 to 40,3 mg/kg for lead in 11 animal feeds: 2 complete feeds (pig feed, sheep feed), 2 complementary feeds (2 mineral feeds), 1 mineral premixture, 4 feed materials (MgO, 2 phosphates, CaCO3) and 2 feed additives (CuSO4, bentonite).
For the determination of extractable lead in minerals and feeds, containing phyllosilicates (e.g. kaolinite clay) wet digestion with nitric acid should be used.
The method limit of quantification for each element is dependent on the sample matrix as well as the instrument. For cadmium a limit of quantification of 0,05 mg/kg should normally be obtained while for lead, a limit of quantification of 0,5 mg/kg should be obtained.

  • Standard
    18 pages
    English language
    sale 10% off
    e-Library read for
    1 day

This European Standard specifies a method for the determination of the elements calcium, sodium, phosphorus, magnesium, potassium, sulphur, iron, zinc, copper, manganese and cobalt in animal feeding stuffs by inductively coupled plasma atomic emission spectrometry (ICP-AES) after pressure digestion.
The method was fully statistically tested and evaluated for the elements calcium, sodium, phosphorus, magnesium, potassium, sulphur, iron, zinc, copper, manganese and cobalt within the following 11 animal feeds: 2 complete feeds (pig feed, sheep feed), 3 complementary feeds (3 mineral feeds), 1 mineral premixture, 3 feed materials (MgO, phosphate, CaCO3) and 2 feed additives (CuSO4, bentonite).
For potassium and sulphur the HORRAT values were mostly higher than 2. Therefore, for these elements the method is more applicable as a screening method and not for confirmatory purposes.
Other elements like molybdenum, lead, cadmium, arsenic were not fully statistically tested and evaluated within 11 animal feeding stuff samples because these elements did not occur in concentrations higher than the limit of quantification in most of these samples. A single laboratory validation is therefore necessary for the use of this multi element method for these elements.
For the determination of extractable lead in minerals and feeds, containing phyllosilicates (e.g. kaolinite clay) wet digestion with nitric acid should be used.
The method limit of quantification for each element is dependent on the sample matrix as well as on the instrument. The method is not applicable for determination of low concentrations of elements. A limit of quantification of 1 mg/kg should normally be obtained.
NOTE 1   This method can also be used for the determination in products with high content (> 5 %) of the element to be measured, but for this purpose the accuracy of the method has to be checked individually.
NOTE 2   Results of this European Standard EN 15621 may be higher than of EN 15510 because EN 15621 is using pressure digestion mode.

  • Standard
    41 pages
    English language
    sale 10% off
    e-Library read for
    1 day

This European Standard specifies the inductively coupled plasma atomic emission spectroscopy (ICP-AES) method for the determination of the elements calcium, sodium, phosphorus, magnesium, potassium, iron, zinc, copper, manganese, cobalt, molybdenum and lead.
The elements calcium, sodium, phosphorus, magnesium, potassium, iron, zinc, copper, manganese, cobalt, molybdenum and lead are extracted either in feeds mainly consisting of organic matter after dry ashing and dissolving in hydrochloric acid or in feeds mainly consisting of inorganic matter after wet digestion with hydrochloric acid.
For the determination of extractable lead in minerals and feeds containing phyllosilicates (e.g. kaolinite clay) wet digestion with nitric acid should be used.
The method was successfully tested for:
-   calcium, sodium, phosphorus, magnesium, potassium, iron, zinc, copper, manganese, cobalt and molybdenum in the following animal feeding stuffs: 2 complete feeds (pig feed, sheep feed), 1 feed material  (phosphate), 1 mineral premixture and 2 complementary feeds (2 mineral feeds),
-   lead in 2 feed materials (phosphate, CaCO3), 2 feed additives (Bentonite, CuSO4), 1 complementary feed (mineral feed)
The method detection limit for each element is dependent on the sample matrix and the instrument. The method is not applicable for the determination of a low concentration of elements. The limit of quantification should be 3 mg/kg or lower.
This method also applies for the determination in products with high element content (>5 %). For this purpose the accuracy of the method has to be checked individually.
NOTE 1   EN 15621 uses the pressure digestion mode, therefore lower results may be obtained with the described method in this standard.

  • Standard
    29 pages
    English language
    sale 10% off
    e-Library read for
    1 day

This European standard specifies a method for the determination of iodine in animal feeding stuffs by inductively coupled plasma mass spectrometry (ICP-MS) following extraction with an alkaline solution.
This method was successfully tested in the range of 0,70 to 631 mg/kg in following animal feeds: seaweed meal, mineral premixture, fish meal, plant based ingredient, marine based compound feed and a synthetic iodine solution.

  • Standard
    15 pages
    English language
    sale 10% off
    e-Library read for
    1 day

This method describes the screening on the antibiotics tylosin, virginiamycin, spiramycin, bacitracin-zinc and avoparcin at sub-additive levels in complete feeding stuffs and milk replacers by a microbiological 3-plate test. The limit of detection of the method is 1 mg/kg for avoparcin, tylosin, spiramycin, virginiamycin and 5 mg/kg for zinc bacitracin. The presence of other (veterinary) antibiotics may interfere with the method. Furthermore, high concentrations of metals (Cu, Zn) may interfere. The method should be used as a qualitative screening method. Positive results can be analysed further by TLC, for confirmatory purposes LCMS is recommended [1].
A lower limit of detection for zinc bacitracin (3 mg/kg) is achievable (see Table 2), but should be established with an in house validation first.

  • Standard
    16 pages
    English language
    sale 10% off
    e-Library read for
    1 day

This European Standard specifies a high performance liquid chromatographic – UV detection (HPLC-UV) method for the simultaneous determination of two growth promoters Carbadox and Olaquindox contents in compound feeds and raw materials at levels ranging from the limit of quantification to 100 mg kg-1.
The limit of quantification of the method has been demonstrated to be better than 3 mg kg-1 for olaquindox and 4 mg kg-1 for carbadox.

  • Standard
    26 pages
    English language
    sale 10% off
    e-Library read for
    1 day

This draft European Standard defines predictive equations for the determination of ME in:
-   products of vegetable or animal origin, in their natural state, fresh or preserved, such as meat, offal, milk products, cooked starch sources; highly digestible special products such as milk substitutes or diets for enteral nutrition;
-   complete or complementary products derived from the industrial processing for cats and dogs.

  • Standard
    32 pages
    English language
    sale 10% off
    e-Library read for
    1 day

ISO 12099:2017 gives guidelines for the determination by near infrared spectroscopy of constituents such as moisture, fat, protein, starch and crude fibre and parameters such as digestibility in animal feeding stuffs, cereals and milled cereal products. The determinations are based on spectrometric measurement in the near infrared spectral region.

  • Standard
    28 pages
    English language
    sale 15% off
  • Standard
    29 pages
    French language
    sale 15% off

This European Standard specifies the inductively coupled plasma atomic emission spectroscopy (ICP-AES) method for the determination of the elements calcium, sodium, phosphorus, magnesium, potassium, iron, zinc, copper, manganese, cobalt, molybdenum and lead.
The elements calcium, sodium, phosphorus, magnesium, potassium, iron, zinc, copper, manganese, cobalt, molybdenum and lead are extracted either in feeds mainly consisting of organic matter after dry ashing and dissolving in hydrochloric acid or in feeds mainly consisting of inorganic matter after wet digestion with hydrochloric acid.
For the determination of extractable lead in minerals and feeds containing phyllosilicates (e.g. kaolinite clay) wet digestion with nitric acid should be used.
The method was successfully tested for:
-   calcium, sodium, phosphorus, magnesium, potassium, iron, zinc, copper, manganese, cobalt and molybdenum in the following animal feeding stuffs: 2 complete feeds (pig feed, sheep feed), 1 feed material  (phosphate), 1 mineral premixture and 2 complementary feeds (2 mineral feeds),
-   lead in 2 feed materials (phosphate, CaCO3), 2 feed additives (Bentonite, CuSO4), 1 complementary feed (mineral feed)
The method detection limit for each element is dependent on the sample matrix and the instrument. The method is not applicable for the determination of a low concentration of elements. The limit of quantification should be 3 mg/kg or lower.
This method also applies for the determination in products with high element content (>5 %). For this purpose the accuracy of the method has to be checked individually.
NOTE 1   EN 15621 uses the pressure digestion mode, therefore lower results may be obtained with the described method in this standard.

  • Standard
    29 pages
    English language
    sale 10% off
    e-Library read for
    1 day

This European Standard specifies a method for the determination of the elements calcium, sodium, phosphorus, magnesium, potassium, sulphur, iron, zinc, copper, manganese and cobalt in animal feeding stuffs by inductively coupled plasma atomic emission spectrometry (ICP-AES) after pressure digestion.
The method was fully statistically tested and evaluated for the elements calcium, sodium, phosphorus, magnesium, potassium, sulphur, iron, zinc, copper, manganese and cobalt within the following 11 animal feeds: 2 complete feeds (pig feed, sheep feed), 3 complementary feeds (3 mineral feeds), 1 mineral premixture, 3 feed materials (MgO, phosphate, CaCO3) and 2 feed additives (CuSO4, bentonite).
For potassium and sulphur the HORRAT values were mostly higher than 2. Therefore, for these elements the method is more applicable as a screening method and not for confirmatory purposes.
Other elements like molybdenum, lead, cadmium, arsenic were not fully statistically tested and evaluated within 11 animal feeding stuff samples because these elements did not occur in concentrations higher than the limit of quantification in most of these samples. A single laboratory validation is therefore necessary for the use of this multi element method for these elements.
For the determination of extractable lead in minerals and feeds, containing phyllosilicates (e.g. kaolinite clay) wet digestion with nitric acid should be used.
The method limit of quantification for each element is dependent on the sample matrix as well as on the instrument. The method is not applicable for determination of low concentrations of elements. A limit of quantification of 1 mg/kg should normally be obtained.
NOTE 1   This method can also be used for the determination in products with high content (> 5 %) of the element to be measured, but for this purpose the accuracy of the method has to be checked individually.
NOTE 2   Results of this European Standard EN 15621 may be higher than of EN 15510 because EN 15621 is using pressure digestion mode.

  • Standard
    41 pages
    English language
    sale 10% off
    e-Library read for
    1 day

The method makes it possible to detect and identify spiramycin, tylosin and virginiamycin in animal feeding stuffs (feed raw materials of mainly plant origin and compound feeds) excluding mineral feeds and premixtures. The limit of detection is about 2 mg/kg for spiramycin, 1 mg/kg for tylosin and 1 mg/kg for virginiamycin. In some milk replacers, it can be slightly higher than 1 mg/kg for virginiamycin.
Reported limits of detection are probably little overestimated but were fully validated during the collaborative study (see Annex B). In each laboratory, each day of analysis, spiked blank samples at 1 mg/kg for spiramycin and virginiamycin and at 0,5 mg/kg for tylosin are analysed for checking lower detection limits (see 9.2 and 9.3). These lower limits of detection are achievable, but should be established with an in-house validation first.
Some other antibiotics can interfere in the detection of these 3 specific macrolide antibiotics. The known interferences are specified in Annex A of the method.
That method should be used as a qualitative screening and/or a post-screening method (after microbiological plate test, for example). The follow-up of the antibiotics presence may be done by other analytical technics (LC and/or LC-MS technics) ([4], [10]). For confirmatory purposes, LCMS is required.

  • Standard
    26 pages
    English language
    sale 10% off
    e-Library read for
    1 day