T.C.
TARIM ve KÖYİŞLERİ BAKANLIĞI
Koruma ve Kontrol Genel Müdürlüğü
Communiqué on the Criteria for Sampling Methods, Sample Preparation and Methods of Analysis for the Official Control of the Levels of Lead, Cadmium, Mercury and 3-Monochloropropane-1,2-diol
Authorization Law: Turkish Food Codex
The Official Gazette:04.07.2005 - 25865
Communication No :2005/35
Objective
Article 1- The objective of this Communiqué is to specify the criteria for sampling methods, preparation of samples and methods of analysis for the official control of the levels of lead, cadmium, mercury and 3-monochloropropane-1,2-diol in foodstuffs.
Scope
Article 2- This Communiqué covers the sampling methods and the preparation of samples as well as the criteria for the methods of analysis used in the official controls of the levels of lead, cadmium, mercury and 3-MCPD present in certain foodstuffs.
Legal Basis
Article 3- This Communiqué has been prepared in accordance with the “Turkish Food Codex Regulation” published in the Official Gazette dated 16/11/1997 and reiterated number 23172.
Sampling
Article 4- The procedures and principles of sampling for the official control of the levels of lead, cadmium, mercury and 3-MCPD in foodstuffs are described in Annex 1.
Criteria for methods of analysis and preparation of samples
Article 5- The procedures and principles for the preparation of samples and criteria for methods of analysis for the official control of the levels of lead, cadmium, mercury and 3-MCPD in foodstuffs are described in Annex 2.
Compliance with European Union
Article 6- This Communiqué has been prepared within the framework of compliance with European Union and taking into consideration Commission Directive 2001/22/EC.
Inspection
Article 7- The provisions of this Communiqué are inspected according to to the Decree Law on “The Production, Consumption and Inspection of Foodstuffs”, dated 27/5/2004 and Numbered 5179, by the Ministry of Agriculture and Rural Affairs
Provisional Article 1- Presently active establishments, that performing the analyse and taking sample for the official control from the products covered within the scope of this Communiqué, are obligated to obey the provisions of this Communiqué within 1 year.
Enforcement
Article 8- This Communiqué enters into force on the date of publication.
Execution
Article 9- The provisions of this Communiqué are executed by the Minister of Agriculture and Rural Affairs.
ANNEX 1
PROCEDURES AND PRINCIPLES OF SAMPLING FOR THE OFFICIAL CONTROL OF THE LEVELS OF LEAD, CADMIUM, MERCURY AND 3- MONOCHLOROPROPANE-1,2-DIOL IN FOODSTUFFS
1. DEFINITIONS
a) Lot: shall mean an identifiable quantity of foodstuff delivered at one time and determined by the sampling official to have common characteristics, such as origin, producer, variety, packer, type of packing, marking, shipment and other similar properties,
b) Sublot: shall mean a physically separated and identified part of a large lot in order to apply the sampling method,
c) Incremental sample: shall mean a quantity of material taken from a single place in the lot or sublot.
d) Aggregate sample: shall mean the combined total of all the incremental samples taken from the lot or sublot.
e) Laboratory sample: shall mean the sample from the aggregate sample sent to the laboratory,
f) Witness Sample: shall mean the sample separated from the aggregate sample for cases of objection.
2- GENERAL PROVISIONS
a) Sampling shall be performed by officially authorized persons.
b) Each lot which is to be examined must be sampled separately.
c) Sample shall be taken at the place where the commodity enters the food chain and from an identifiable lot. It shall be ensured that the aggregate sample is representative of the lot to be controlled.
d) In the case of liquid products, the incremental sample shall be shaken well or homogenized by other suitable means before it is taken. In the case of liquid products for which the contaminant in the lot shows a homogenous distribution it is sufficient to take a single incremental sample as aggregate sample from each lot.
e) The number of incremental samples to be taken from other lots according to the lot weight is given in Table 1.
f) The number of packages required to form the aggregate sample where the lot consists of individual packages is given in Table 2.
g) All necessary precautions shall be taken to avoid all kinds of changes which might alter the level of lead, cadmium, mercury and 3-MCPD or affect the analytical determination adversely or make aggregate samples unrepresentative in the course of sampling and, preparation, transportation and storage of the laboratory samples, and samples shall be placed in clean, inert containers of quality which shall not change the characteristics of the sample.
h) As far as possible incremental samples shall be taken at various places distributed throughout the lot or sublot. In the case of departure from this procedure it shall be recorded as provided for in paragraph (m) of this Article.
i) Quantities of the incremental samples shall be at equal weights.
j) The aggregate sample shall be at least 1 kg in so far as it is practical.
k) The witness sample shall be taken from the homogenized aggregate sample.
l) Where procedure above is not applicable the laboratory sample and the witness sample to be separated from the aggregate sample shall at least be sufficiently big to enable concurrent analyses.
m) Each sample taken for official use shall be sealed at the place of sampling. A record must be kept of each sample permitting the lot it is representative of to be identified unambiguously. The date and place of sampling as well as any other information likely to be of assistance to the person who shall carry out the analysis shall take place in this record.
n) In the case of fish lots, the fish shall be of similar sizes.
o) The laboratory sample shall be subjected to at least two independent analyses and the mean of the analyses shall be reported in the analysis report.
p) The lot is accepted if the detected quantity of residue complies with the maximum acceptable levels and rejected if the quantity of residue exceeds such levels.
Table 1
Minimum number of incremental samples necessary to be taken depending on the weight of the lot
Weight of the Lot (kg) |
Number of incremental samples |
< 50 |
3 |
50 – 500 |
5 |
>500 |
10 |
Table 2
Number of packages of incremental samples which shall be taken if the lot consists of individual Packages
| Number of packages or units in the lot | Number of packages or units to be taken |
1 – 25 |
1 package or unit |
26 – 100
|
About 5 %, at least 2 packages or units
|
>100
|
About 5 %, at maximum 10 packages or units |
ANNEX 2
SAMPLE PREPARATION AND CRITERIA FOR METHODS OF ANALYSIS USED IN THE OFFICIAL CONTROL OF THE LEVELS OF LEAD, CADMIUM, MERCURY AND 3-MCPD IN FOODSTUFFS
The samples for analysis shall be taken without introducing contamination and in homogenous form.
Specific Sample Preparation Procedures for Lead, Cadmium and Mercury
The sample preparation procedure which may be used for the products under consideration shall be made in accordance with the CEN Standard under the title of ‘Foodstuffs – Determination of trace elements – Performance criteria and general consideration’ or internationally validated methods.
Bivalve molluscs, crustaceans and small fish which are eaten whole shall be analyzed together with the viscera. As for the vegetables only the edible portions shall be put under analysis.
Method of Analysis Used by the Laboratory and Laboratory Control Requirements
a) Definitions
r : It is a measurement of repeatability which expresses the absolute difference between the results obtained by two subsequent analyses made by the same sample, same operator, same apparatus in the same laboratory, within a 95 % confidence range, and calculated by the formulae R = 2.8xsr.
sr : Standard deviation, calculated from results generated under repeatability conditions.
RSDr : Relative standard deviation, calculated from results generated under repeatability conditions, [(sr/x)x100].
x: Mean calculated from results generated under repeatability conditions.
R : It is a measurement of reproducibility among laboratories which expresses the absolute difference among the results obtained by the same sample and method but different operators and laboratories, within a 95 % confidence range, and calculated by the formulae R = 2.8xsR.
sR : Standard deviation, calculated from results generated under reproducibility conditions.
RSDR :Relative standard deviation calculated from results generated under reproducibility conditions [(sR / x) x100].
HORRATr : RSDr value obtained under repeatability conditions in the same laboratory, divided by the RSDr value estimated from the Horowitz equation using the assumption r = 0,66xR.
HORRATr : RSDR value obtained under reproducibility conditions among different laboratories, divided by the RSDR value calculated from the Horowitz equation.
Collaborative trial test: comparison test made among national and international laboratories.
b)General requirements
Methods of analysis used for food control purposes must comply with the section on Sampling Methods and Methods of Analysis of the Turkish Food Codex.
c)Specific requirements
1- Analyses of lead, cadmium and mercury:
Specific methods for the determination of lead, cadmium and mercury contents are not prescribed in this Communiqué. Laboratories shall use internationally validated methods that fulfill the performance criteria indicated in Table 3. Where possible, the validation shall include a certified reference material in the collaborative trial test materials.
2- 3-MCPD analysis
Specific methods for the determination of 3-MCPD contents are not prescribed. Laboratories shall use internationally validated methods that fulfill the performance criteria indicated in Table 4. Where possible, the validation shall include a certified reference material in the collaborative trial test materials.
Table 3
Performance criteria of methods for lead, cadmium and mercury
| Parameter | Value/comment |
| Applicability | Foodstuffs referred to in the Turkish Food Codex-Communiqué on the Determination of the Maximum Levels of Certain Contaminants in Foodstuffs Communiqué No. 2002/63 |
| Detection limit | No more than one tenth of the maximum levels Described in the Turkish Food Codex- Communiqué on the Determination of the Maximum Levels of Certain Contaminants in Foodstuffs, where maximum level of lead is less than 0,1 mg/kg no more than one fifth of the maximum level |
| Limit of quantification | No more than one fifth of the maximum levels Described in the Turkish Food Codex-Communiqué on the Determination of the Maximum Levels of Certain Contaminants in Foodstuffs, where maximum level of lead is less than 0,1 mg/kg no more than two fifths of the maximum level |
| Precision | HORRATr or HORRATR values must be less than 1,5 in the validation collaborative trial |
| Recovery | Must be between 80 and 120 %. |
| Specificity | Free from matrix or spectral interference |
Table 4
Performance criteria of methods of analysis for 3-MCPD
| Criterion | Recommended value | Concentration |
| Field Blanks | Less than the detection limit | - |
| Recovery | 75 – 110 % | All |
| Limit of quantification | 10 (or less) µg/kg on a dry matter basis | - |
| Standard deviation of the field blank signal | less than 4 µg/kg | - |
| In-house precision estimates- Deviation of replicate measurements at different concentrations |
< 4 µg/kg < 6 µg/kg < 7 µg/kg < 8 µg/kg < 15 µg/kg | 20 µg/kg 30 µg/kg 40 µg/kg 50 µg/kg 100 µg/kg |
d)Evaluation of the recovery calculations
Wherever possible the trueness of the analysis shall be estimated by including suitable reference materials in the analytical run.
Analysis results, suitable or not, shall be in the form to include the recovery levels. Analytical results shall be reported corrected or uncorrected. Whichever is used shall be indicated in this report and the recovery rates shall take place in the reports.
e)Expression of results
The results shall be expressed in the same units as those used to express the maximum levels described in the Turkish Food Codex-Communiqué on the determination of the maximum levels of certain contaminants in foodstuffs.