Regulation on Sampling and Analysis Methods for the Official Control of Feed

Purpose and scope

ARTICLE 1 − (1) The purpose of this Regulation is;

Sampling for the determination of the composition of the feed, additives and undesirable substances, excluding microorganisms, in the official control of feed,
The preparation of samples for analysis and the reporting of results,
The analysis methods to be applied in the official control of feed,
The analysis methods to be used in the determination of components of animal origin in the official control of feed,
The calculation of the energy value of poultry compound feed,
To determine the analysis methods to be used in the control of the illegal presence of feed additives whose use is prohibited.

Legal basis

ARTICLE 2. (1) This Regulation has been prepared;

On the basis of Article 31 of the Law on Veterinary Services, Plant Health, Food and Feed dated 11/6/2010 and numbered 5996,
In parallel with the European Union Regulation on Sampling and Analysis Methods for the Official Control of Feed dated 27/1/2009 and numbered 152/2009.

Definitions

ARTICLE 3. (1) In this Regulation;

Divider: The instruments used to divide the sample into approximately equal parts during the preparation of the primary sample, the reduced sample and the laboratory samples,
Reduced sample: The sample obtained from the aggregate sample by the reduction method and representing the aggregate sample,
Ministry: The Ministry of Food, Agriculture and Livestock,
Primary sample: The quantity taken from one point of the batch from which the sample is taken,
Hand tools: The shovel, sampling probe and similar tools used when sampling by hand,
Laboratory sample: The sample taken from the homogenized aggregate sample or from the reduced sample,
Mechanical tools: The tool used when sampling from feed in motion,
Sampling personnel: The person authorized for official control by the Ministry,
Batch from which the sample is taken: The feed which, by its characteristics, constitutes one example and one unit,
Sampling tools and devices: The tools and devices made of materials that will not cause contamination in the feed from which the sample is taken, the use of which is deemed appropriate by the Ministry,
Sampling probe: The sampling tool of various sizes, with long slots or compartments, suitable for the particle size of the batch from which the sample is taken and of the feed,
Aggregate sample: The sample obtained by combining and homogeneously mixing the primary samples taken from the batch from which the sample is taken.

General provisions concerning sampling

ARTICLE 4. (1) When sampling from solid feed, hand tools, mechanical tools and dividers are used.

(2) The numbers and quantities of samples that must be taken, depending on the characteristics and size of the batch from which the sample is to be taken, are specified in Annex-1.

(3) The sampling tools and devices, the surfaces on which the sample will be prepared and the sample containers must be clean and dry. In order not to change the characteristics of the feed and to prevent possible contamination, samples are taken and prepared as quickly as possible, and the necessary measures are taken for this.

Taking of primary samples

ARTICLE 5. (1) The primary samples to be taken for the control of substances or products showing a homogeneous distribution within the feed are taken randomly and in approximately equal quantities from the batch from which the sample is taken.

In bulk feed, the batch from which the sample is taken is divided into approximately equal parts by estimation and visual judgment, and from each part, as specified in row A.2 of Annex-1, as many random samples as the required number of primary samples are taken. When necessary, sampling may also be carried out during loading or unloading.
In packaged feed, after the required number of packages specified in row A.2 of Annex-1 is selected, a part of the content of each package is taken as a sample using a shovel and similar hand tools. When necessary, the sample may also be taken after the packages are emptied separately. If there are caked pieces in the sample taken, these are broken up and mixed.
In homogenized or homogenizable liquid or semi-liquid feed, the number of containers specified in row A.2 of Annex-1 is taken into account. If necessary, the content is homogenized, and the required quantity of sample is taken from each container. The sample may also be taken while the content is being emptied.
In liquid or semi-liquid feed that cannot be homogenized, taking into account the number of containers specified in row A.2 of Annex-1, samples are taken from different levels. The samples may also be taken while the content is being emptied, but are taken after discarding the first initial portions. In any case, the total volume of the sample taken cannot be less than 10 liters.
d) For feed blocks and mineral licking stones, the number of blocks or licking stones specified in row A.2 of Annex-1 is selected and a part of each block or licking stone is taken as a sample.

(2) For the primary samples to be taken in connection with the control of undesirable substances or products that are not homogeneously distributed within the feed, such as aflatoxin, ergot, castor oil plant and the leguminous genus crotalaria; the batch from which the sample is to be taken is divided into approximately equal portions by estimation and visual judgment, according to the number of aggregate samples specified in row B.3 of Annex-1. If the estimated number of separated portions is more than one, from each portion, primary samples are taken in approximately equal quantities from as many different places as specified in row B.2 of Annex-1. The total quantity of primary samples taken for the aggregate samples from each portion cannot be less than 4 kilograms. Primary samples taken from different portions are not made into an aggregate sample.

Preparation of aggregate samples

ARTICLE 6. (1) The primary samples taken for the control of substances or products showing a homogeneous distribution within the feed are combined and mixed to form an aggregate sample.

(2) For the control of undesirable substances or products that are not homogeneously distributed within the feed, such as aflatoxin, ergot, castor oil plant and the leguminous genus crotalaria, in order to form the number of aggregate samples specified in row B.3 of Annex-1, the primary samples taken from each portion are combined and mixed. The aggregate sample taken from each portion formed by estimation and visual judgment is coded according to the portion from which it was taken.

Preparation of laboratory samples

ARTICLE 7. (1) In order to obtain a homogeneous sample, each aggregate sample is mixed carefully and meticulously. If necessary, the aggregate sample is reduced to 2 kilograms or 2 liters using a mechanical or automatic divider or by the quartering method to form a reduced sample.

(2) (Amended sentence: OG-11/2/2012-28201) To be sent to the laboratory, at least three samples are formed equally and so as to bear the same characteristics, in the quantity specified in row A.4 of Annex-1 or row B.4 of Annex-1. Each sample is placed separately in suitable containers. All necessary measures are taken to prevent contamination that may occur during storage and transport, or to prevent adverse situations that may cause the sample to deteriorate and its composition to change.

Packaging of laboratory samples

ARTICLE 8. (1) Samples taken for official controls are sealed and labelled. The sealing operation is carried out in such a way that the package cannot be opened without the seal being broken, in order to ensure the security of the sample.

Sample records

ARTICLE 9. (1) The records concerning the portion to which the sample belongs and the sample are kept in such a way as not to give rise to confusion and doubt.

Sending of samples to the laboratory

ARTICLE 10. (1) In order for the analysis to be carried out, at least one of the samples taken from each aggregate sample is sent to the authorized laboratory as soon as possible together with the necessary information concerning the requested analyses.

Preparation of samples for analysis

ARTICLE 11. (1) From the feed sample taken in accordance with this Regulation and sent to the authorized laboratory, the sample is weighed and taken in the quantity specified in the analysis method. This quantity taken must be homogeneous and of a nature representing the sample.

(2) The points to be observed when preparing samples for analysis are specified below:

Samples are prepared according to the method specified in the applied analysis methods.
All operations applied are carried out in such a way as to prevent, as far as possible, possible contamination and changes that may occur in the composition.
In order to ensure that the sample is exposed to air and light to the minimum level, the grinding, mixing and sieving operations to be carried out are performed as quickly as possible. Mills and grinders that cause significant heating in the sample are not used.
Feed that is particularly heat-sensitive is ground by hand. Care is taken to ensure that the tools used are not a source of contamination in the sample in terms of trace elements.
If, when the sample is being prepared, the moisture content of the sample cannot be preserved and a change occurs in the moisture content, moisture determination is carried out before and after preparation according to the method specified in subparagraph (a) of the first paragraph of Article 13.

(3) When the sample is being prepared for analysis, using appropriate separation techniques, it is divided into sufficient sub-samples for analysis and reference. Coning and quartering methods are not used when dividing into sub-samples. The reference sample is kept in a clean, dry and airtight suitable container. Depending on the characteristics of the feed, sub-samples of at least 100 g are prepared for analysis as specified below.

For grindable feed; if a different method is not specified in the analysis method, it is ground when necessary, but excessive grinding is avoided when carrying out this grinding operation. The whole of the ground sample is passed through a sieve with 1 mm2 mesh (according to ISO R565). The sieved sample is mixed and placed in a clean, dry, airtight suitable container. When a sample is to be taken for analysis, the sample is mixed again immediately before being weighed.
For feed grindable after drying; if a different method is not specified in the analysis method, the sample is dried, in accordance with the pre-drying operation in the method specified in subparagraph (a) of the first paragraph of Article 13, until the moisture content falls within the range of 12 , 8 %. The subsequent operations are carried out as specified in subparagraph (a).
For liquid or semi-liquid feed; the sample is placed in a clean, dry and airtight suitable container. When a sample is to be taken for analysis, the sample is mixed immediately before being weighed.
For other feed; depending on the characteristics of the feed, other different methods may be applied in the preparation of other feed that cannot be prepared in the manners specified above. However, the quantity taken for analysis is such that it is homogeneous and represents the sample to be analyzed.

(4) In the storage of samples; samples are stored at a suitable temperature that will not cause any change in their composition. In particular, samples taken for the analyses of vitamins or substances sensitive to light are kept in brown glass containers.

Provisions concerning the equipment and chemicals used in analyses

ARTICLE 12. (1) If a different method is not specified in the analysis method, the chemicals used must be analytically pure. The purity of the chemicals used in the analysis of trace amounts of substances is checked by a blank test. Depending on the results obtained, further purification of the chemicals may be necessary.

(2) If a special solvent, diluent or any substance is not specified in the analysis method, water is used in the preparation of solutions, diluents, rinsing and washing solutions. The water to be used in these operations is distilled or demineralized. If a special purification of the water used is required in the analysis method, the purification operation is carried out according to the specified analysis method.

(3) The equipment and materials used in the laboratory must be the equipment and materials specified in the analysis methods, and these equipment and materials must be clean.

Analysis methods

ARTICLE 13. (1) The Ministry;

Control of the compositions of feed materials and compound feed,
Control of the levels of additives in feed,
Control of undesirable substances in feed,
Official control of the determination of components of animal origin in feed,
Control of feed additives whose use is not permitted,
Calculation of the energy value of poultry compound feed,

determines the analysis methods related to these and publishes them on the Ministry's website.

(2) Different methods may be applied in the extraction operation. In the event that an extraction method other than the one specified in the analysis method is applied, this applied method ensures an extraction efficiency equivalent to the method specified in the analysis method for that product.

(3) The cleaning operation may be carried out by different methods. In the event that a method other than the one specified in the analysis method is applied, this applied method ensures a cleaning efficiency equivalent to the method specified in the analysis method for that product.

(4) Where necessary, within the scope of the Regulation on the Determination of the Establishment, Duties, Powers and Responsibilities of Food Control Laboratories and Their Working Procedures and Principles, other different methods that are scientifically accepted and permitted by the Ministry may also be applied, apart from the methods specified in this Regulation.

Reporting of analysis results

ARTICLE 14. (1) The analysis result is written with significant figures as specified in the analysis method. According to the change occurring in the moisture content of the sample arriving at the laboratory, a correction is made in the result, when necessary, according to the moisture content before preparation.

(2) The applied method is stated in the report.

(3) The number of samples worked on and the number of repetitions from which the result value given in the analysis report was obtained are stated in the report. The result value is determined by taking the average of the number of samples worked on and the number of repetitions. Parallel work is carried out with at least two samples. If analysis is being carried out in terms of undesirable substances, provided that the quality procedures have been complied with, if the value obtained from the analysis result determined in the first sample worked on is a value lower than half of the value specified in its specification, a second study is not necessary. In the control of the content of a substance or the declared value, provided that the quality procedures have been complied with, if the analysis result determined in the first sample worked on confirms the declared value and the content and is within the acceptable variation range, a second study is not necessary.

(4) The determination and evaluation of undesirable substances such as dioxins and dioxin-like Polychlorinated biphenyls (PCBs) in feed is carried out taking into account the expanded measurement uncertainty and the recovery correction. If the analysis result of undesirable substances exceeds the determined maximum level, this feed is evaluated as non-compliant feed. This evaluation is carried out in cases where it is possible to calculate the measurement uncertainty and the recovery correction according to the analysis method. Since this kind of evaluation is not suitable for microscopic analyses, it is not carried out. In the reporting of the analysis result, the measurement uncertainty and the recovery rate are stated as follows:

In the correction made for recovery, the recovery level is determined. The correction made for recovery is not necessary in cases where it is between 90 % and 110 %.
In the equation 'x +/ - U', "x" expresses the analysis result and "U" expresses the expanded measurement uncertainty. For an approximately 95 % confidence interval, a coverage factor of 2 is used. However, provided that the quality procedures have been complied with, if the value obtained from the determined analysis result is a value lower than half of the value specified in its specification, there is no need to state the measurement uncertainty and the recovery correction in the analysis result report.

Entry into force

ARTICLE 15 − (1) This Regulation enters into force on the date of its publication.

Execution

ARTICLE 16 − (1) The provisions of this Regulation are executed by the Minister of Food, Agriculture and Livestock.