Potravinářské produkty

Oblast zaměření: Potravinářské produkty
Komise : CEN/TC 275 (Food analysis - Horizontal methods)
Původce: CEN
K připomínkám do: 25.09.2018
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This document describes a procedure for the determination of nivalenol (NIV), deoxynivalenol (DON) and its acetyl derivatives (3-acetyl-DON and 15-acetyl-DON), HT-2 and T-2 toxins (HT-2, T-2) and zearalenone (ZEA) in cereals and cereal products by high performance liquid chromatography (HPLC) coupled with tandem mass spectrometry (MS/MS) after cleanup by solid phase extraction (SPE).

The method has been validated with both contaminated and spiked samples of wheat, wheat flour, and wheat crackers.

Validation levels for NIV ranged from 27,7μg/kg to 377,8 μg/kg.

Validation levels for DON ranged from 233,9μg/kg to 2420,0 μg/kg.

Validation levels for 3-acetyl-DON ranged from 18,5μg/kg to 136,5 μg/kg.

Validation levels for 15-acetyl-DON ranged from 11,4μg/kg to 141,8 μg/kg.

Validation levels for HT-2 ranged from 6,6 μg/kg to 133,8 μg/kg.

Validation levels for T-2 ranged from 2,1 μg/kg to 37,6 μg/kg.

Validation levels for ZEA ranged from 31,6μg/kg to 229,7 μg/kg

Laboratory experiences have shown that this method is also applicable to barley and oat flour, and rye based crackers [5], however, this has not been validated in a collaborative study.

Oblast zaměření: Potravinářské produkty
Komise : CEN/TC 275 (Food analysis - Horizontal methods)
Původce: CEN
K připomínkám do: 26.09.2018
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This document describes a screening method for the determination of aflatoxin B1, deoxynivalenol, fumonisin B1 and B2, ochratoxin A, HT-2 and T-2 toxins, and zearalenone in foodstuffs by high performance liquid chromatography (HPLC) coupled with tandem mass spectrometry (MS/MS).

The aim of the screening method is to test compliance of foodstuff with regulatory limits or to determine whether a certain pre-defined level (the screening target concentration, STC) is exceeded or not. The result of the screening is either “negative” or “suspect”. “Negative” (screen negative) means that the targeted mycotoxins are not detected or potentially present but below the STC. “Suspect” (screen positive) means that the established cut-off level is exceeded and the sample can contain one or more mycotoxins at a level higher than the STC.

For full identification and accurate quantification a second confirmatory quantitative analysis method is required which is outside the scope of this document.

The method is suitable for various types of foodstuff and has been validated for representative matrices from four commodity groups:

—   high starch and/or protein content and low water and fat content: wheat, cereal mixture, wheat flour and cornflakes;

—   high oil content: peanuts;

—   high sugar low water content: figs;

—   high water content: grape juice.

During validation, cut-off levels were established for the following screening target concentrations:

—   aflatoxin B1: 2 µg/kg to 5 µg/kg;

—   deoxynivalenol: 250 µg/kg to 865 µg/kg;

—   fumonisin B1: 200 µg/kg to 790 µg/kg;

—   fumonisin B2: 110 µg/kg to 230 µg/kg;

—   ochratoxin A: 4 µg/kg to 9 µg/kg;

—   T-2 toxin: 25 µg/kg;

—   HT-2 toxin: 25 µg/kg to 50 µg/kg;

—   zearalenone: 30 µg/kg to 100 µg/kg.

Oblast zaměření: Potravinářské produkty
Komise : CEN/TC 327 (Animal feeding stuffs: Methods of sampling and analysis)
Původce: CEN
K připomínkám do: 1.10.2018
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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 is intended to 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.

Oblast zaměření: Potravinářské produkty
Komise : CEN/TC 327 (Animal feeding stuffs: Methods of sampling and analysis)
Původce: CEN
K připomínkám do: 1.10.2018
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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.

Oblast zaměření: Potravinářské produkty
Komise : CEN/TC 327 (Animal feeding stuffs: Methods of sampling and analysis)
Původce: CEN
K připomínkám do: 1.10.2018
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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 mg/kg 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 can 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 mg/kg 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.

Oblast zaměření: Potravinářské produkty
Komise : CEN/TC 327 (Animal feeding stuffs: Methods of sampling and analysis)
Původce: CEN
K připomínkám do: 8.10.2018
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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 authorized 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.

Oblast zaměření: Potravinářské produkty
Komise : CEN/TC 327 (Animal feeding stuffs: Methods of sampling and analysis)
Původce: CEN
K připomínkám do: 8.10.2018
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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.

It is advisable that the user of this standar determine 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. 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.

Oblast zaměření: Potravinářské produkty
Komise : CEN/TC 327 (Animal feeding stuffs: Methods of sampling and analysis)
Původce: CEN
K připomínkám do: 8.10.2018
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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 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 weigh and extraction volume, limits of quantification (LOQ), as calculated (Table 1) on the basis of a wavelength of 230 nm, can be achievable.

Oblast zaměření: Potravinářské produkty
Komise : CEN/TC 307 (Oilseeds, vegetable and animal fats and oils and their by-products - Methods of sampling and analysis)
Původce: CEN
K připomínkám do: 20.10.2018
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This International Standard specifies a rapid method for extraction of oil and for preparation of the methyl esters of fatty acids. The methyl esters thus obtained can be used for gas chromatography.

This International Standard is applicable to the following oilseeds: rape, sunflower, soya beans, mustard, linseed.

NOTE          Applying this rapid method to high erucic acid content rapeseed leads to an overestimation of erucic acid content by approximately a mass fraction of 1 %. This difference was observed in the study [6] and may be due to the partial extraction of the oil from the sample (yield around 70%). High content of erucic acid in triglycerides could increase their solubility in hexane because of the lipophilic effect of the carbon long-chain (C22). However, as this effect was not checked on a large set of high erucic rapeseed samples, it is not recommended to apply a correction factor to the erucic acid content when analysing high erucic acid rapeseed.

Oblast zaměření: Potravinářské produkty
Komise : CEN/TC 307 (Oilseeds, vegetable and animal fats and oils and their by-products - Methods of sampling and analysis)
Původce:
K připomínkám do: 6.11.2018
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The purpose of this document is to describe a procedure for the determination of the ester content in fatty acid methyl esters (FAME) intended for incorporation into diesel oil. It also allows determining the linolenic acid methyl ester content. It allows verifying that the ester content of FAME is greater than 90 % (m/m) and that the linolenic acid content is between 1 % (m/m) and 15 % (m/m).

This method is suitable for FAME which contains methyl esters between C6 and C24.

NOTE 1       For the purposes of this document, the terms “% (m/m)” and “% (v/v)” are used to represent respectively the mass and volume fractions.

NOTE 2       This method was elaborated for FAME samples from usual raw material. For FAME sample from unidentified raw material, a solution of the test sample is prepared without any internal standard addition, in order to verify the absence of natural nonadecanoic acid methyl ester.

NOTE 3       The distribution off fatty acid methyl esters is given in Annex C.

WARNING — The use of this method may involve hazardous equipment, materials and operations. This method does not purport to address to all of the safety problems associated with its use, but it is the responsibility of the user to search and establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.