KŽP - Agricultural food products

This part of ISO 23036 specifies a method that is applicable for the detection of Anisakidae L3 larvae commonly found in marine and anadromous fishes. The method can be applied to fresh fish and/or frozen fish, lightly processed fish products, such as marinated, salted or smoked, and it’s also suitable for visceral organs as confirmatory method for visual inspection scheme.
The artificial digestion method allows quantifying parasitic infections by estimating the number of parasites in the fish musculature and, when applied to fresh fish or lightly processed fish products (never frozen before processing), determining the viability of Anisakidae L3, which may be present.
This method doesn’t allow determining species or genotype of detected parasites, which identification is made by morphological and/or molecular methods.

This part of ISO 23036 specifies a method that is applicable for the detection of Anisakidae L3 larvae commonly found in marine and anadromous fishes. The method can be applied to fresh fish and/or frozen fish, lightly processed fish products, such as marinated, salted or cold smoked.
This method allows quantifying parasitic infections by estimating the number of parasites in the fish musculature.
This method doesn’t allow determining species or genotype of detected parasites, which identification
is made by morphological and/or molecular methods

This document specifies a procedure for the determination of the citrinin content in food (cereals, red yeast rice (RYR)), herbs and food supplements by liquid chromatography tandem mass spectrometry (LC-MS/MS).
This method has been validated for citrinin in red yeast rice and in the formulated food supplements in the range of 2,5 µg/kg to 3000 µg/kg and in wheat flour in the range of 2,5 µg/kg to 100 µg/kg.
Laboratory experiences have shown that this method is also applicable to white rice, herbs such as a powder of ginkgo biloba leaves and the formulated food supplements in the range of 2,5 µg/kg to 50 µg/kg.

This document specifies a method for the determination of aflatoxin M1 content in milk and milk powder.
The lowest level of validation is 0,08 μg/kg for whole milk powder, i.e. 0,008 μg/l for reconstituted
liquid milk. The limit of detection (LOD) is 0,05 μg/kg for milk powder and 0,005 μg/kg for liquid milk.
The limit of quantification (LOQ) is 0,1 μg/kg for milk powder and 0,01 μg/kg for liquid milk.
The method is also applicable to low-fat milk, skimmed milk, low-fat milk powder and skimmed milk
powder.

This document gives guidelines for the establishment of a conversion relationship between the results
of an alternative method and an anchor method, and its verification for the quantitative determination
of the microbiological quality of milk.
NOTE The conversion relationship can be used a) to convert results from an alternative method to the anchor
basis or b) to convert results/limits, expressed on an anchor basis, to results in units of an alternative method.

This document specifies a procedure for determining whether a perceptible sensory difference or
similarity exists between samples of two products. The method is a forced-choice procedure. The
method is applicable whether a difference exists in a single sensory attribute or in several attributes.
The method is statistically more efficient than the duo-trio test (described in ISO 10399), but has
limited use with products that exhibit strong carryover and/or lingering flavours.
The method is applicable even when the nature of the difference is unknown [i.e. it determines neither
the size nor the direction of difference between samples, nor is there any indication of the attribute(s)
responsible for the difference]. The method is applicable only if the products are homogeneous.
The method is effective for:
a) determining that:
1) either a perceptible difference results (triangle testing for difference);
2) a perceptible difference does not result (triangle testing for similarity),
when, for example, a change is made in ingredients, processing, packaging, handling or storage;
b) selecting, training and monitoring assessors.

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).

This document describes a method for the determination of the sum total of six ergot alkaloids (ergocornine, ergometrine, ergocristine, ergotamine, ergosine and ergocryptine) and their  inine epimer pairs by liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) after clean-up by dispersive solid phase extraction (SPE).
The method has been validated for cereals and cereal-based food products.
The method has been validated in the range 13,2 µg/kg to 168 µg/kg for the sum of the twelve ergot alkaloids, in rye flour, rye bread and cereal products (breakfast cereal, infant breakfast cereal, and crispbread) that contained rye as an ingredient, as well as seeded wholemeal flour and a barley and rye flour mixture.
Method performance was satisfactory in the range 24,1 µg/kg to 168 µg/kg, however at lower concentrations RSDR values were greater than 44 %, and HorRat values exceeded 2,0, indicating the method may not be fully suitable at concentrations below 24 µg/kg for sum of ergot alkaloids, although it is suitable for screening at these concentrations. Method performance may be improved by inclusion of an isotopically labelled internal standard, but this was not available at the time of the method validation study.

This document specifies two methods:
— a reference method for the determination of the moisture content of maize grains and ground whole
maize, groats, grits and maize flour, see Clause 4;
— a routine method for the evaluation of the moisture content of maize in whole grains, see Clause 5.
The latter is not suitable for use for experts’ reports, or for calibration or checking of humidity meters,
because of its significant bias to the reference method (see Table B.3).

This International Standard describes the quantitative liquid chromatographic determination of specific sugars (galactose, glucose, fructose, sucrose, lactose, and maltose) in various milk and milk products, applying arabinose or fucose as internal standards. The method is applicable for the following different dairy matrices: milk, milk powder, chees, whey powder, infant formula, dessert and yogurt. Soy containing dairy products are excluded. The determination of the lactose content in low lactose milk products is excluded.
A sophisticated high performance anion exchange chromatographic method in combination with
pulsed amperometric detection (HPAEC-AD) is applied. With this method the following 13 different
mono- and disaccharides can be separated: fucose, arabinose, galactose, glucose, fructose, sucrose, lactose, lactulose, maltose, melobiose, trehalose, platinose (maltulose) and maltotriose.

This International Standard specifies a method for the determination of inulin-type fructans (including oligofructose, and fructooligosaccharides) in infant formula and adult nutritionals containing 0,03 g/100 g to 5,0 g/100 g of fructan in the product as prepared ready for consumption.
A high performance anion exchange chromatographic method in combination with pulsed amperometric detection (HPAEC-PAD) is applied.

This document deals with verification of methods for the detection and/or the enumeration of microorganisms, with particular emphasis on the implementation of a reference/alternative method in the user laboratory and verification of a reference/alternative method using items included in the scope of the method and tested routinely but not tested in the original validation study

This document specifies a titrimetric method for the determination of acid value in light coloured Fatty Acid Methyl Esters, hereinafter referred as FAME.
It allows the determination of acid value within a range of 0,10 mg KOH/g to 1,00 mg KOH/g.
NOTE 1 For the purposes of this document, the terms "% (m/m)" and "% (V/V)" are used to represent respectively the mass fraction and the volume fraction.
NOTE 2 For oils and fats the determination of acid value is specified in EN ISO 660 [1].
WARNING - The use of this document can involve hazardous materials, operations and equipment. This document does not purport to address all of the safety problems associated with its use. It is the responsibility of users of this document to take appropriate measures to ensure the safety and health of personnel prior to the application of the document, and to determine the applicability of any other restrictions for this purpose.

This document defines the repeatability and the reproducibility of a method using near infrared spectroscopy in whole kernels for the determination of moisture and protein on wheat and barley. The performance of the method (accuracy) is found in EN 15948.
The values derived from the report are applicable to the following concentration ranges:
-  for wheat:
-   moisture content range from 9,5 % - 15,7 %;
-   protein content range from 10,0 % DM to 18,6 % DM;
-  for barley:
-   moisture content range from 10,6 % - 15,9 %;
-   protein content range from 9,2 % DM - 15,4 % DM.

The purpose of this European Standard is to determine the free glycerol and residual mono-, di- and triglyceride contents in fatty acid methyl esters (FAME) intended for addition to mineral oils. The total glycerol content is then calculated from the obtained results.
Under the conditions described, the quantification limits are 0,001 % (m/m) for free glycerol, 0,10 % (m/m) for all glycerides (mono-, di- and tri-). This method is suitable for FAME prepared from rapeseed, sunflower, soybean, palm, animal oils and fats and mixture of them. It is not suitable for FAME produced from or containing coconut and palm kernel oils derivatives because of overlapping of different glyceride peaks.
NOTE  For the purposes of this European Standard, the term "% (m/m)" is used to represent respectively the mass fraction.
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. It is the responsibility of the user of this standard to take appropriate measures to ensure the safety and health of personnel prior to application of the standard, and fulfil statutory and regulatory requirements for this purpose.

This European Standard specifies a method for the determination of the oxidation stability of fatty acid methyl esters (FAME) at 110 °C, by means of measuring the induction period up to 48 h.
NOTE 1   EN 15751 [1] describes a similar test method for oxidation stability determination of pure fatty acid methyl esters and of blends of FAME with petroleum-based diesel containing 2 % (V/V) of FAME at minimum.
NOTE 2   The precision statement of this test method was determined in a Round Robin exercise with induction periods up to 8,5 h, thus covering the limit value in EN 14214. Results from precision studies on EN 15751 indicate that the precision statement is valid for induction periods up to 48 h but not for higher values.
NOTE 3   Limited studies on EN 15751 with EHN (2-ethyl hexyl nitrate) on FAME blends indicated that the stability is reduced to an extent which is within the reproducibility of the test method. It is likely that the oxidation stability of pure FAMEs is also reduced in the presence of EHN when EN 14112 is used for testing.

This document describes a procedure for the determination of aflatoxins B1, B2, G1 and G2 and total aflatoxins (sum of B1, B2, G1 and G2) in spices for which EU maximum levels are established, other than paprika, by high performance liquid chromatography (HPLC) with post-column derivatization (PCD) and fluorescence detection (FLD) after immunoaffinity column clean-up.
The method is applicable to the spices capsicum, pepper, nutmeg, ginger, turmeric and mixtures thereof.
The method has been validated for aflatoxins B1, B2, G1 and G2 and total aflatoxins in a range of test samples that comprised: ginger, pepper, nutmeg, chilli, turmeric as individual spices and mixed pepper+chilli+nutmeg (90+5+5, m+m+m), mixed spice+ginger (6+4, m+m) mixed spice, mixed turmeric+ginger (2+8, m+m).
The validation was carried out over the following concentration ranges: aflatoxin B1 = 1 µg/kg to 16 µg/kg and total aflatoxins = 2,46 µg/kg to 36,1 µg/kg.

This document specifies a method for determining the content of impurities of animal origin in wheat flours, with or without additives and having an ash yield not exceeding a mass fraction of 0,75 %, and in durum wheat semolinas.
This method permits the separation and quantification of contamination of animal origin, such as insects at all stages of their development and their fragments, rodent hairs and their fragments, and mites.

This document specifies a method for developing a texture profile of food products (solids, semi-solids, liquids) or non-food products (e.g. cosmetics).
This method is one approach to sensory texture profile analysis and other methods exist. This method describes various steps in the process of establishing a complete description of the textural attributes of a product.
This method is applicable to:
— screening and training assessors;
— orientating assessors through the development of definitions and evaluation techniques for textural characteristics;
— characterizing the textural attributes of a product in order to establish its standard profile and to discern any later changes;
— improving old products and developing new products;
— studying various factors that can affect the textural attributes of a product, e.g. changes in process, time, temperature, ingredients, packaging or shelf-life, and storage conditions;
— comparing a product with another similar product to determine the nature and intensity of textural differences;
— correlating sensory and instrumental and/or physical measurements.

This document specifies the conditions required for good keeping of the following groups of citrus fruits during their storage with or without refrigeration, in stores or in various transport equipment (such as containers, railway cars, trucks or ships):
— oranges: Citrus sinensis (Linnaeus) Osbeck;
— mandarins: Citrus reticulata Blanco;
— lemons: Citrus limon (Linnaeus) N. L. Burman;
— grapefruits: Citrus paradisi Macfadyen;
— limes:  
— Citrus aurantifolia (Christmann) Swingle;
— Citrus latifolia Tanaka.  
Detailed information concerning cultivars in these different groups is given in Annexes A and B.

This European Standard defines a routine method for the determination of moisture and protein in whole kernels of barley and wheat using a near-infrared spectrophotometer in the constituent ranges:
a) for wheat:
1)   moisture content minimum range from 8 % to 22 %;
2)   protein content minimum range from 7 % to 20 %.
b) for barley:
1)   moisture content minimum range from 8 % to 22 %;
2)   protein content minimum range from 7 % to 16 %.
This European Standard describes the modalities to be implemented by the supplier (5.3 and 5.4) and the user of the method.

This document specifies three methods (two titrimetric and one potentiometric) for the determination
of acidity in animal and vegetable fats and oils, hereinafter referred to as “fats”. The acidity is expressed
preferably as acid value or, alternatively, as acidity calculated conventionally.
This document is applicable to refined and crude vegetable or animal fats and oils, soap stock fatty
acids or technical fatty acids. It does not apply to waxes.
Since the methods are completely non-specific, they do not apply to differentiating between mineral
acids, free fatty acids and other organic acids. The acid value, therefore, includes any mineral acids that
are present.
Milk and milk products (or fat coming from milk and milk products) are excluded from the Scope of this
document.

The proposed deliverable specifies an alternative technical protocol for the validation of mostly non-proprietary methods in the field of microbiological analysis of food, animal feed, and environmental and primary production stage samples.
It is closely related to ISO 16140-2. The latter specifies the technical protocol for the validation of proprietary methods, including a classical interlaboratory study and a method comparison study to be conducted in one laboratory. The realization of classical interlaboratory studies demands a sufficient number of participating laboratories (at least 8 laboratories are required). There are many occasions where a sufficient number of participating laboratories is not available (e.g. when a new method is required quickly after an outbreak of a new microorganism). In this case, the validation cannot be considered as reliable any longer.
The proposed deliverable uses a modified protocol based on orthogonal, factorial studies. By selection of suitable influencing factors (technician, nutrient media, sample preparation, temperature, duration) a high certainty of the determined method validation parameters is obtained, so that the number of required collaborating laboratories can be reduced up to a minimum of 4.
This validation protocol can be used in different ways. If the 4 collaborators can be considered a “random sample” of independent and competent laboratories and from different organizations, the test method can be considered as being validated in the sense that accurate and precise measurements are to be expected from any competent laboratory. If the 4 collaborators can be considered a “random sample” of independent and competent laboratories from one organization, the test method can be considered as being validated in the sense that accurate and precise measurements are to be expected from any competent laboratory in this organization.

This document specifies requirements for ground sweet and hot paprika (Capsicum annuum L. and
Capsicum frutescens L.).
Recommendations relating to storage and transport conditions are given in Annex A. A list of terms
used in different countries for paprika is given in Annex B.
This document does not apply to ground chillies and other species of capsicums.
NOTE Specifications for ground chillies and capsicums are given in ISO 972.

The proposed deliverable specifies the procedure for single-laboratory validation of mainly non-proprietary methods in the fields of microbiological analysis of food, feed, and environmental and primary production stage samples. Single-laboratory validation is required if an interlaboratory validation according to ISO 16140-2 is not appropriate, e.g. for in-house methods or when the required number of participating laboratories is not available. Single-laboratory validation is not part of the optimization of methods. It can be applied only for methods that are fully specified with regard to all relevant parameters (including tolerances on temperatures and specifications on nutrient media).
The proposed deliverable describes two protocols for single-laboratory validation, a conventional protocol, and a factorial protocol. The conventional protocol is a stepwise procedure; both the study design and the performance measures are derived from ISO 16140-2. The performance measures of the factorial protocol are also derived from ISO 16140-2; however, it is using an orthogonal, factorial study design. By selection of suitable influencing factors (technician, nutrient media, sample preparation, temperature, duration) a high certainty of the determined method validation parameters is obtained, so that the number of required individual tests can be reduced by more than 50 %.

This document specifies a test method to determine the extractable colour in paprika by measuring the
absorbance of an acetone extract of the sample.
It is applicable to ground paprika in every presentation (sweet, hot, smoked, etc).

This document specifies a reference method for the determination of the amylose content of milled rice,
non-parboiled. The method is applicable to rice with an amylose mass fraction higher than 5 %.
This document can also be used for husked rice, maize, millet and other cereals if the extension of this
scope has been validated by the user.
NOTE Amylose values determined with this document can be compared with PDO and PGI legislation.

This document specifies two simplified routine methods for the determination of the amylose mass
fraction of milled rice, non-parboiled. The main difference between the two methods is the dispersion
procedure: method A specifies hot dispersion, and method B specifies cold dispersion.
Both methods are applicable to rice with an amylose mass fraction higher than 5 %.
NOTE These methods describe simplified procedures for the preparation of samples, which are frequently
used in routine laboratories. The methods use the same reagents as the reference method (see ISO 6647-1), but
omit the defatting step. Rice samples where the amylose mass fraction has been determined by the reference
method are used as standards.

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.

This document specifies rules for the preparation of samples of milk and milk products and their
suspensions for microbiological examination when the samples require a different preparation from
the general methods specified in ISO 6887-1.
This document excludes the preparation of samples for both enumeration and detection test methods
where preparation details are specified in the relevant International Standards.
This document is intended to be used in conjunction with ISO 6887-1.
This document is applicable to:
a) milk and liquid milk products;
b) dehydrated milk products;
c) cheese and cheese products;
d) casein and caseinates;
e) butter;
f) milk-based ice-cream;
g) milk-based custard, desserts and sweet cream;
h) fermented milks, yogurt, probiotics milk products and sour cream;
i) dehydrated milk-based infant foods, with or without probiotics.

ISO 16958:2015 specifies a method for the quantification of individual and/or all fatty acids in the profile of milk, milk products, infant formula and adult nutritional formula, containing milk fat and/or vegetable oils, supplemented or not supplemented with oils rich in long chain polyunsaturated fatty acids (LC-PUFA). This also includes groups of fatty acids often labelled [i.e. trans fatty acids (TFA), saturated fatty acids (SFA), monounsaturated fatty acids (MUFA), polyunsaturated fatty acids (PUFA), omega-3, omega-6 and omega-9 fatty acids] and/or individual fatty acids [i.e. linoleic acid (LA), α-linolenic acid (ALA), arachidonic acid (ARA), eicosapentaenoic acid (EPA) and docosahexaenoic acid (DHA)].
The determination is performed by direct transesterification in food matrices, without prior fat extraction, and consequently it is applicable to liquid samples or reconstituted powder samples with water having total fat ≥ 1,5 % m/m.
The fat extracted from products containing less than 1,5 % m/m fat can be analysed with the same method after a preliminary fat extraction using methods referenced in Clause 2. Dairy products, like soft or hard cheeses with acidity level ≤ 1 mmol/100 g of fat, can be analysed after a preliminary fat extraction using methods referenced in Clause 2. For products supplemented or enriched with PUFA with fish oil or algae origins, the evaporation of solvents should be performed at the lowest possible temperature (e.g. max. 40 °C) to recover these sensitive fatty acids.

This document specifies a method for the determination of the saponification value of animal and
vegetable fats and oils. The saponification value is a measure of the free and esterified acids present in
fats and fatty acids.
The method is applicable to refined and crude vegetable and animal fats.
If mineral acids are present, the results given by this method are not interpretable unless the mineral
acids are determined separately.
The saponification value can also be calculated from fatty acid data obtained by gas chromatography
analysis as given in Annex B. For this calculation, it is necessary to be sure that the sample does not
contain major impurities or is thermally degraded.

This document specifies a method for the quantitative determination of calcium (Ca), copper (Cu), iron
(Fe), magnesium (Mg), manganese (Mn), phosphorus (P), potassium (K), sodium (Na) and zinc (Zn)
using inductively coupled plasma atomic emission spectrometry (ICP-AES). The method is applicable
for milk, dried milk, butter, cheese, whey, dried whey, infant formula and adult nutritional formula in
the ranges given in Table 1.

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.

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.

This document specifies a method for the quantitative determination of calcium (Ca), copper (Cu), iron (Fe), magnesium (Mg), manganese (Mn), phosphorus (P), potassium (K), sodium (Na), zinc (Zn), chromium (Cr), molybdenum (Mo) and selenium (Se) using inductively coupled plasma and mass spectrometry (ICP-MS).
The method is applicable for the determination of all 12 elements in infant formula and adult nutritional products. The method is also applicable for milk, milk powder, whey powder, butter and cheese excluding the determination of Cr, because all Cr results were below the quantification limit and reproducibility could not be determined in these matrices[1]. The present method is an extension of ISO 20649 | IDF 235 (AOAC 2011.19[2]) which was validated only for Cr, Mo and Se in infant formula and adult nutritional products.

ISO 20647:2015 specifies a method for the quantitative determination of total iodine in infant formula and adult nutritional formula.[1] The method is applicable to the measurement of total iodine in infant formula and adult nutritional formula from 0,5 µg/100g to 1 500 µg/100g reconstituted final product and for ready-to-feed products from 2,5 µg/100 g to 1 000 µg/100 g using ICP-MS.
Using various infant formula and adult nutritional products, the method was subjected to an interlaboratory study. Levels obtained ranged from 3,47 µg/100 g to 124 µg/100 g. For all precision data related to the interlaboratory study, see Table A.1 located in Annex A.

This standard describes a method for the determination of the colour in durum wheat semolina and soft wheat flour by reflectance diffused colorimetry. The standard is suitable for semolina and flour obtained by experimental or industrial milling.

EN-ISO 665 specifies a method for the determination of the moisture and volatile matter content of oilseeds.

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.

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.

This document specifies a protocol for the evaluation of instrumental alternative methods for total bacterial count in raw milk from animals of different species.

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

This document describes a procedure for the determination of ochratoxin A (OTA) in pork products specifically ham, pork based products (canned chopped pork) and pork liver using high performance liquid chromatography with fluorescence detection (HPLC-FLD).
The method has been validated for ochratoxin A with naturally contaminated ham, pork based products (canned chopped pork) and pork liver containing 0,5 μg/kg to 11 μg/kg [4, 5, 6].
Laboratory experiences have shown that this method is also applicable to pâté and kidney [4].