T.C.
GIDA, TARIM ve HAYVANCILIK BAKANLIÐI
Gýda ve Kontrol Genel Müdürlüðü
Communiqué on Sampling and Methods of analysis for the Official Controls of Certain Contaminant Levels in Foodstuffs
Authorization Law: Turkish Food Codex
The Official Gazette:25.03.2002-24706
Communication No :2002/25
Objective
Article 1. The objective of this Communiqué is to determine the sampling from foodstuffs and methods of analysis for the official controls of certain contaminant levels.
Scope
Article 2. This Communiqué covers the sampling method for official controls of aflatoxin levels in some foodstuffs and sample preparation and criteria for the methods of analysis used in official controls.
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, reiterated no.23172.
Definitions
Article 4. For the purpose of this Communiqué;
Lot: means product samples having the same size, type and package, or packed product group produced at the same time and under the same conditions.
Sub – lot: means designated part of a large lot in order to apply the sampling method
Incremental sample: means the amount of material taken from a single placa of the lot or sub-lot
Aggregated sample: means the sample obtained by gathering all of the incremental samples taken from the lot or sub-lot
Laboratory sample: means sample or sub-sample reserved for laboratory
Blank sample: Sample reserved for cases of defensive or conflictive cases
General provisions
Article 5. The facts which should be considered during sampling are listed below.
a) The sample shall be taken by the food controller / food inspector.
b) Each lot which to be examined must be sampled separately. Large lotes should be subdivided into smaller sub-lotes to be sampled separately according to the provisions of Article 7 of this Communiqué.
c) All precautions must be taken, during sampling and preparation of laboratory samples, to avoid any change that will alter the aflatoxin amount, have negative impact on analytic determination or make the aggregate samples unrepresentative.
d) As far as possible the incremental samples must be taken at various places distrubuted throughout the lot or sub-lot. Otherwise, it must be recorded in compliance with the (h) sub-paragraph of this article.
e) The aggregate sample is obtained through gathering and well mixing of incremental samples. The aggregate sample should, after being mixed, be divided into equal sub-samples in compliance with the other provisions in Article 7 of this Communiqué. Mixing operation is essential to ensure that each sub-sample contains particles from all lotes or sub-lots.
f) Blank sample shall be taken from the homogenated sub-samples.
g) Each laboratory sample shall be put in clean containers that protect sample against contamination and damage during transportation, and have no interaction with other containers. All necessary precautions should be taken to avoid any change in the composition of the laboratory sample during transportation and storage.
h) Each sample taken for official controls shall be sealed at the place of sampling. A record must be kept for each sample to provide exact determination of the sample. Date and place of sampling and other information to be helpful for the analyst should also be kept within this record.
i) Preparation of sample and criteria for the methods of analysis used in official controls of the aflatoxin levels in some foodstuffs should comply with Annex 5.
Explanatory Provisions
Article 6. Explanatory provisions for sampling are given below:
a) Different types of lots
Wholesale trading of foodstuffs may be carried out in barrels and crates or sacks, bags, retail packages, etc. Sampling procedure can be applied to all the different forms in which the commodities are put on the market.
The following formula may be used as a guide for sampling from the lots marketed in small packages as small sacks, bags, retailing packages, etc. so as not to be contrary to the other provisions in the Article 7 of this Communiqué.
(Lot weight x incremental sample weight)
Sampling Frequency (SF) = -------------------------------------------------------
(Aggragated sample weight x unit package weight)
Weight : should be in kg
SF : decimal numbers should be rounded to nearest whole number
a) Weight of theincremental sample
The average weight of incremental sample should be about 300 g unless otherwise is stated in the other provisions of the Article 7 of this Communiqué. For lots with retail packages, the weight of incremental sample depends on the weight of retail package.
b) Number of incremental samples to be taken from lots of less than 15 tonnes by weight.
Unless otherwise is stated in the other provisions of the Article 7 of this Communiqué, the number of incremental samples to be taken is between min.10 and max.100 depending on the lot weight. The figures in Table 1 of the Annex 1 may be used to determine number of incremental samples to be taken.
Other provisions
Article 7. The general survey on the sampling procedure for groundnuts, hazelnuts, dried fruits, cereals, milk and dairy products are stated below:
a) For groundnuts, hazelnuts, dried fruits, cereals, the table regarding the division of lotes into sub–lots must comply with the Table 2 of Annex 1.
b) The sampling method from groundnuts, pistachio, hazelnuts and other nuts, dried fig and from cereals, the lot weight of which is equal to or more than 50 tons, must comply with the Annex 2.
c) The sampling procedure from fatty dried fruits other than hazelnut and nut; dried fruits other than fig, and from cereals, weight of the lot which is less than 50 tons, must comply with the Annex 3.
d) The sampling procedure for milk and dairy products must comply with the Annex 4.
Compliance with European Union
Article 8. This Communiqué has been prepared within the framework of compliance with European Union having regard to the Commission Directive 98/53/EEC for “sampling methods and the methods of analysis for the official control of the levels for certain contaminants in foodstuffs”.
Inspection
Article 9. The provisions of this Communiqué are inspected both by the Ministry of Agriculture and Rural Affairs and the Ministry of Health in accordance with the Decree Law No. 560, dated 24/6/1995, on the “Production, Consumption and Inspection of Foods”.
Provisional Article 1. Presently active institutions and establishments sampling and analysis for official controls of the products under the scope of this Communiqué are obliged to obey the provisions of this Communiqué within 1 year.
Enforcement
Article 10. This Communiqué enters into force on the date of publication.
Execution
Article 11. The provisions of this Communiqué are executed by the Minister of Agriculture and Rural Affairs and the Minister of Health.
ANNEX 1
Number of incremental samples and subdivision of lots into sub-lots
Table 1
Number of incremental samples to be taken from the lots weight of less than 15 tonnes
| Weight of Lot (tonnes) | Number of incremental samples |
< 0.1 |
10 |
>0.1 - <0.2 |
15 |
>0.2 - <0.5 |
20 |
>0.5 - < 1.0 |
30 |
>1.0 - <2.0 |
40 |
>2.0 - <5.0 |
60 |
>5.0 - <10.0 |
80 |
>10.0 - <15.0 |
100 |
Table 2
Subdivision of lots into sub-lots depending on product and lot weight
Product |
Lot weight (tonnes) |
Weight or number of sub-lots |
Number of Incremental samples |
Weight of Aggregate Sample (kg) |
Dried fig and other dried fruits |
>15 |
15-30 tonnes |
100 |
30 |
Groundnut, pistachio nut, hazelnut and other fatty dried fruits |
>500 |
100 tons |
100 |
30 |
Cereals |
>1500 |
500 tonnes |
100 |
30 |
(*) depends on the lot weight (see. Table 1 and Annex 3) |
||||
ANNEX- 2
Sampling method for groundnut, pistachio nut, hazelnut and other nuts, dried fig and cereals with a lot weight equal to or more than 50 tons
a) Sampling procedure
- Each lot should be subdivided into sub-lots according to Table 2 of Annex 1, provided that the sub-lot can physically be separated. Taking into account that the fact that the weight of the lot may not always be an exact multiple of the weight of the sub-lots, the difference between the weight of each separated sub-lot and the calculated weight of sub-lot should not exceed a maximum of 20%.
- Each sub-lot must be sampled separately.
- Number of incremental samples : 100. The number of incremental sample to be taken depends on the lots, the weight of which is less than 15 tonnes, is between a minimum of 10 and a maximum of 100 as specified in Paragraph (c) of Article 6 of this Communiqué.
- Weight of aggregate sample : It is the sample weight of 30 kg, obtained by gathering the incremental samples that require to be divided into 3 equal sub-samples of 10 kg each and mixed before grinding. (The process of dividing into 3 sub-samples is not necessary for groundnut, hazelnut and dried fruits which will be subject to further sorting and / or other physical treatment. This, however, depends upon the availability of such equipment for homogenizing a sample of 30 kg). Sub-samples divided into 3 equal pieces as A, B and C are redivided into 3 subgroups as A1-A2-A3, B1-B2-B3 and C1-C2-C3 following grinding. They are taken from each sub-group (A1 - B1 - C1) in separate packages in order to avoid from mixing and sent to the laboratory. Similarly, replicate sample (A2 - B2 - C2) and company samples (A3 - B3 – C 3) are taken in separate packages.
- If the weight of aggregate sample is less than 10 kg, it should not be divided into 3 sub-samples.
- Laboratory sample is a sub-sample of 10 kg. Each sub-sample should be ground finely and mixed throughly to achive complete homogenization in accordance with the provisions of the Annex 5.
- If it is not possible to carry out the method of sampling described above because of the commercial consequences resulting from damage to the lot (because of packing forms means of transport, etc.) an alternative method of sampling may be applied provided that it is as representative as possible and is fully described and documented.
b) Acceptance of a lot or sub-lot
- For groundnut, hazelnut or dried fruits subject to sorting or other physical treatment:
accepted if the aggregate sample or the average of sub-samples is within the maximum limits,
rejected if aggregate sample or the average of sub-samples exceeds the maximum limit.
- For groundnut, hazelnut, dried fruit and cereals intended for direct human consumption
accepted if none of the sub-lots exceeds the maximum limit,
rejected if one or more sub-lots exceed the maximum limit.
- When the weight of aggregate sample is less than 10 kg,
accepted if the aggregate sample conforms to the maximum limit,
rejected if the aggregate sample exceeds the maximum limit.
ANNEX 3
Sampling method for fatty dry fruits other than hazelnut and nut, dried fruits other than fig and for cereals with a lot weight less than 50 tonnes
a) Sampling Procedure
The sampling method stated in Annex 2 may be applied for these products. . However, more simpler sampling methods may be applied for these products taking into account the low contamination risk and/or new packing types for the trading of products.
For cereal lots under than 50 tons, a sampling plan consisting of, depending on the lot weight, 10 to 100 incremental samples each of 100 grams, resulting in an aggregate sample of 1 to 10 kg may be used. The figures in the following table can be used to determine the number of incremental samples to be taken.
Table 3
Number of incremental samples to be taken depending
on the weight of the lot of the cereals
Lot weight (tonnes) |
Number of Incremental Samples |
<1 |
10 |
>1 - <3 |
20 |
>3 - <10 |
40 |
>10 - < 20 |
60 |
>20 - < 50 |
100 |
b) Acceptance of a lot or sub-lot
The provisions in Annex 2 for the acceptance of a lot or sub-lot are applicable.
ANNEX 4
Sampling Procedure for Milk and Dairy Products
Milk
a) Sampling Procedure
Testing of and some methods of analysis for raw milk and heat–treated milk will be determined in the relevant Communiqué to be issued in accordance with The Turkish Food Codex Regulation.
- number of incremental samples: should be minimum 5.
- weight of aggregate sample: should be minimum 0.5 kg or litres.
b) Acceptance of a lot or sub-lot
- accepted if the aggregate sample conforms to the maximum limit,
- rejected if the aggregate sample exceeds the maximum limit.
Derivated products and compound foods
1) Dairy products
a) Sampling procedure
Sampling procedures from concentrated milk and milk powder will be determined in the relevant Communiqué to be issued in accordance with The Turkish Food Codex Regulation.
- number of incremental samples should be minimum 5.
- An equivalent method of sampling shall be applied for other dairy products.
b) Acceptance of a lot or sub-lot
- accepted if the aggregate sample conforms to the maximum limit,
- rejected if the aggregate sample exceeds the maximum limit.
2) Other derivated products with very small particle weight :
Such products as flour, crushed fig, groundnut butter etc. where aflatoxin contamination is homogenously distributed
a) Sampling procedure
- Number of incremental samples : Number of incremental samples should be between 10-100 depending on the lot weight for lotes less than 50 tonnes as stated in the table of Annex 3.
- Average weight of incremental samples should be 100 g. For lotes with retail packages, the weight of the incremental sample depends on the weight of retail package.
- Weight of the aggregate sample should be between 1-10 kg sufficiently mixed.
b) Number of samples to be taken:
- Number of aggregate samples to be taken depends on the lot weight. The division of large lots into smaller ones should be performed in accordance with the table for cereals in Annex 1.
- Each sub-lot must be sampled separately.
c) Acceptance of a lot or sub-lot
- accepted if the aggregate sample conforms to the maximum limit,
- rejected if the aggregate sample exceeds the maximum limit
3) Other derivated products having relatively larger pieces
Heterogeneous distrubution of aflatoxin contamination is:
- Sampling method and acceptance for raw agricultural products should conform to Annex 2 and Annex 3.
ANNEX 5
Sample preparation and criteria for methods of analysis used in official controls of the levels of aflatoxin in some foodstuffs
1) Introduction
a) Precautions
The sample should be well protected against daylight during sampling, transferring to laboratory and analyzing. As the distrubution of aflatoxin is extremely non-homogeneous, samples should be prepared and especially homogenised with extreme care.
All materials taken by the laboratory are used for preparing the test material.
b) Calculation of proportion of shell/kernel of whole nuts
The limits fixed for aflatoxins determined by the “Turkish Food Codex Regulations” are applied to the edible parts.
The level of aflatoxins in the edible part is determined as follows:
- Shelling the samples of nuts in “shells” and the level of aflatoxins is directly determined in the edible part.
- Homogenise the nuts “in shell” by taking them through the sample preparation procedure. The sampling and analytical procedure must estimate the weight of nut kernel in the aggregate sample is estimated after establishing a suitable factor for the proportion of nut shell to nut kernel in whole nuts. This proportion is used to ascertain the amount of kernel in the bulk sample taken through the sample preparation and analysis procedure. Approximately 100 whole nuts are taken at random separately from the lot or are to be put aside from each aggregate sample. The ratio may, for each laboratory sample, be obtained by weighing the whole nuts, shelling and re-weighing the shell and kernel portions. However, the proportion of shell to kernel may be established by the laboratory from a number of samples and so can be assumed for future analytical work. But if a particular laboratory sample is found to be in contravention of any limit, the proportion should be determined for that sample using the approximately 100 nuts that have been set aside.
2) Treatment of the sample taken to the laboratory
Each laboratory sample is ground and throughly mixed by means of a method determined in order to achive the complete homogenization.
3) Blank sample
Blank sample should be taken from a homogenized material unless otherwise is concerned
4) method of analysis to be used by the laboratory and laboratory control
a) The most common definitions used by the laboratories are given below.
Repeatability and reproducibility are the most common parameters used by the laboratories.
r (repeatability) : The value below the absolute difference between 2 different test results obtained under such repeatable conditions as same sample, same operator, same apparatus, same laboratory and short interval of time is expected to lie within the specific probabilities, the approximate value of which is
95 %; therefore r = 2.8 x sr .
Sr: standard deviation calculated from the results generated under repeatable conditions
RSDr: Relative standard deviation calculated from the results generated under repeatable conditions [(Sr / X) x 100],
X: the average of all laboratory and sample results
R: reproducibility; the absolute difference between different test results generated under reproducible conditions such as material provided by the operators in different laboratories using standard test method, is expected to lie within specific probabilities, the approximate value of which is 95%; therefore R = 2.8 x Sr .
SR : standard deviation calculated from the results generated under reproducible conditions.
RSDR : Relative standard deviation calculated from the results generated under reproducible conditions [(SR / X) x 100],
b) General Requirements
Methods of analysis intended for food control will be determined in the relevant Communiqué to be issued in accordance with The Turkish Food Codex Regulation.
c) Specific Requirements
If no specific method is assigned for the determination of aflatoxin levels in foodstuffs, laboratories can use any method complying with the following criteria.
Criterion |
Concentration range |
Recommended value |
Maximum permitted value |
Blanks |
All |
Negligible |
|
Recovery Aflatoxin M1 |
1. – 0.5µg/L |
60%-120% |
|
Recovery Aflatoxin |
<1.0µg/L |
50%-120% |
|
Precision RSDR |
All |
As derived from Horwitz equation |
2 x the value derived from Horwitz Equation |
Precision RSDR is calculated as (precision RSDR x 0,66) at the concentration of interest |
|||
Explanatory Notes
- Value applied both to B1 and sum of (B1 +B2 + G1 + G2)
- If B1 +B2 + G1 + G2 sum of aflatoxin is to be reported, the effect of each one on the analytical system should be known or equivalent
- The precision values in the concentration studied can not be indicated as the determination limits of applied methods.
- Precision values are calculated from Horwitz Equation.
RSDR = 2(t-0.5 log C)
- RSDR : Relative standard deviation calculated from the results derivated under reproducible conditions [(SR / X) x 100],
- C, concentration ratio (1=100 g / 100 g, 0.001 = 1000 mg / kg)
- This is a generalized precision equation, independent from analyte and matrix but dependent on the concentration of mostly routine method of analysis.
d) Recovery Calculation
Analytical results are reported for recovery, whether being corrected or not. Reporting method and recovery level should be notified.
Official Gazette: 17.07.2003 – No. 25171
Communiqué On The Amendment Of Turkish Food Codex
Communiqué On Methods of Sampling and Analysis for
Official Controls of the Level of Certain Contaminants in Foodstuffs
(Communiqué No: 2003/28)
Article 1 – Paragraph (b) of article 6 of the Turkish Food Codex Communiqué On Methods of Sampling and Analysis for the Official Controls of the Level of Certain Contaminants in Foodstuffs, published in the Official Gazette dated 25/03/2002 and no.24706 has been amended as follows.
“b) Weight of the incremental sample:
Unless stated in a different way in the provisions of article 7 of this Communiqué and excluding spices, incremental sample weight must be approximately 300 g. Incremental sample weight in spices must be approximately 100 g. In retail packaged lots the incremental sample weight depends on weight of the retail packaging.”
Article 2 – Article 7 of the same Communiqué has been amended as follows.
“Article 7 – The general survey of the method of sampling from groundnuts, hazelnuts, dried fruits, cereals, spices, milk and dairy products is stated below.”
a) The Table concerning the division of lots into sub-lots depending on the product and the lot weight for groundnuts, hazelnuts, dried fruits, cereals and spices must be in conformity with Table-2 in Annex-1.
b) The sampling method for groundnuts, pistachios, hazelnuts and other nuts, dried fig and lots of cereals having a size equal to and larger than 50 tonnes must conform to Annex-2.
c) The sampling method for dried fruits that contain fat excluding hazelnuts and groundnuts, dried fruits excluding fig and lots of cereals having a size less than 50 tonnes must conform to Annex-3.
d) The sampling method for milk and dairy products must conform to Annex-4.
e) According to the provisions stated above for sampling from foodstuffs, sampling should be made as far as possible during the retailing phase. In case this is not possible, another sampling method can be used provided it sufficiently represents the lot from which sampling is to be made.”
Article 3 – The provisional article 1 of the same Communiqué has been amended as follows.
“Provisional Article 1 – Presently active institutions and establishments sampling and analyzing for the purpose of official controls the foodstuffs other than imported foodstuffs within the scope of this Communiqué, must conform to the provisions of this Communiqué within 1 year; and for the official controls of imported foodstuffs until December 31, 2003.
Article 4 – Table-2 in Annex-1 of the same Communiqué has been amended as follows.
Table-2
Subdivision of lots into sub-lots according to product and lot weight
Product |
Lot weight |
Weight or number of |
Number of incremental samples |
Aggregate sample weight (kg) |
Dried fig and other dried fruits |
>15 |
15-30 tonnes |
100 |
30 |
Groundnuts, pistachios, hazelnuts and other dried fruits containing fat |
>500 |
100 tonnes |
100 |
30 |
Cereals |
>1500 |
500 tonnes |
100 |
30 |
Spices |
>15 |
25 tonnes |
100 |
10 |
(*) Depending on lot weight (refer to Table 1 and Annex-3) |
||||
Article 5 – Annex 2 of the same Communiqué has been amended as follows.
ANNEX-2
Method of Sampling for groundnuts, pistachios, hazelnuts and other nuts, dried fig, spices and lots of cereals of a size equal to and larger than 50 tonnes
a) Sampling procedure
- On condition that the sub-lot can physically be separated, each lot must be subdivided into sub-lots according to Table-2 in Annex-1. Considering the fact that the weight of the lot cannot always be an exact multiple of the weight of the sub-lots, the difference between the actual weight and the calculated weight of the separated sub-lot must not exceed a maximum of 20%.
- Each sub-lot must be sampled separately.
- Number of incremental samples: 100. As stated in paragraph c of article 6 of this Communiqué, the number of incremental samples to be taken from lots that weigh less than 15 tonnes depends on the weight of the lot and varies between a minimum of 10 and a maximum of 100.
- Weight of the aggregate sample: Is a sample weight of 30 kg, which before grinding, must be subdivided into 3 equal sub-samples and must be mixed, weighing 10 kg each, and which is obtained by combining incremental samples (this division into three sub-samplesis not necessary in the case of groundnuts, nuts,and dried fruits intended for further sorting or other physical treatment,however, this will depen upon the availability of equipment which is able to homogenise a 30 kg sample.) The sub-samples, divided into 3 equal pieces as A, B and C are separated individually once more into two sub-groups as A1-A2, B1-B2 and C1-C2. Samples are taken from each sub-group (A1-B1-C1) separately and sent to the laboratory in individual packages. Likewise, witness samples (A2-B2-C2) are also packed individually.”
- If aggregate sample weight is less than 10 kg, the aggregate sample must not be divided into 3 sub-samples. The maximum weight of aggregate sample for spices is 10 kg. Therefore there is no need to divide it into sub-samples.
- Laboratory sample: Is a sub-sample of 10 kg. In conformity with the provisions stated in Annex-5, each sub-sample must one by one be very finely grinded and be thoroughly mixed in order to obtain a full homogenization.
- If it is not possible to carry out the method of sampling described above because of the commercial consequences resulting from damage to the lot (because of packing forms means of transport, etc.) an alternative method of sampling may be applied provided that it is as representative as possible and is fully described and documented.
b) The acceptance of a lot or sub-lot
- For groundnuts, hazelnuts, dried fruits and spices, which are subject to a sorting or other physical treatment:
accepted if the aggregate sample or the average of sub-samples is within the maximum limits,
rejected if aggregate sample or the average of sub-samples exceeds the maximum limits.
- For groundnuts, hazelnuts, dried fruits and cereals for the purpose of direct human consumption,
Accepted if none of the sub-lots exceed the maximum limit.
Rejected if one or more than one of the sub-lots exceeds the maximum limit.
- When aggregate sample is less than 10 kg:
Accepted if aggregate sample corresponds to the maximum limit.
Rejected if aggregate sample exceeds the maximum limit.”
Article 6 – Sub-paragraph (b) of paragraph 2, titled “Derived products and compound foods” in Annex-4 of the same Communiqué has been amended as follows.
“b) Number of samples to be taken:
- The number of aggregate samples to be taken depends on the weight of the lot. The subdivision of large lots into small ones must be made as stated for cereals in Table-2 of Annex-1.”
Article 7 – The table in sub-paragraph (c), titled “Specific Requirements”, which takes place in the fourth paragraph of Annex-5 of the same Communiqué has been amended as follows.
Criterion |
Concentration range |
Recommended value |
Maximum permitted value |
Blanks |
All |
At a negligible level |
|
Recovery Aflatoxin M1 |
0.01 - 0.05 mg/kg |
%60 - %120 |
|
Recovery- Aflatoxin |
< 1.0 mg/kg |
%50 - %120 |
|
Precise RSDR |
All |
As obtained from Horwitz equation |
Value obtained from 2xHorwitz equation |
Precision RSDR is calculated as (precision RSDR x 0,66) at the concentration of interest |
|||
Enforcement
Article 7 – This Communiqué enters into force on the date of publication.
Execution
Article 8 – The provision of this Communiqué are executed by the Minister of Agriculture and Rural Affairs and the Minister of Health.