Decree No. 459 / 2005 Coll.
Decree amending Decree No. 211 / 2004 Coll., on methods of testing and method of sampling and preparation of control samples, as amended
Valid
Order
Effective from 01.12.2005
Text versions:
01.12.2005
28.11.2005
459
DECLARATION
of 4 November 2005
amending Decree No. 211 / 2004 Coll., on methods of testing and method of sampling and preparation of control samples, as amended
According to Article 18 (1) (m) of Act No. 110 / 1997 Coll., on Food and Tobacco Products and amending and supplementing certain related laws, as amended by Act No. 316 / 2004 Coll.:
Decree No. 211 / 2004 Coll., on methods of testing and method of sampling and preparation of reference samples, as amended by Decree No. 611 / 2004 Coll. and Decree No. 238 / 2005 Coll., is amended as follows:
1. In footnote 1a, at the end of the text, the sentence "Commission Directive 2005 / 38 / EC of 6 June 2005 laying down the methods of sampling and the methods of testing for the official control of the levels of Fusarium toxins in foodstuffs' is added.
2. in Paragraph 4, the following paragraph 13 is added:
"(13) Sampling to check the content of Fusarium toxins in foodstuffs shall be carried out in accordance with Annex 46. ';
3. In Article 7, the following paragraph 16 is added:
"(16) The preparation of samples for the control of the content of Fusarium toxins in foodstuffs shall be as set out in Annex 47. ';
4. In Section 10, the following paragraph 23 is added:
"(23) The control of the content of Fusarium toxins in foodstuffs shall be carried out in accordance with Annex 47. ';
5. The following Annexes 46 and 47 are inserted after Annex 45:
"Annex No 46 to Decree No 211 / 2004 Coll.
Methods of sampling for official control of levels of Fusarium toxins in foodstuffs
1. Purpose and scope
Samples for official control of the levels of Fusarium toxins in foodstuffs shall be taken using the following methods. The aggregate samples thus obtained shall be considered representative of the lots. Compliance with the maximum levels laid down in Annex I to Commission Regulation (EC) No 466 / 2001 shall be assessed on the basis of the quantities found in laboratory samples.
2. Definitions
For the purposes of this Annex, a lot shall mean the identifiable quantity of food delivered at the same time, which, according to the person referred to in Article 3 (1), has common characteristics such as origin, type, type of packaging, packer, consignor or mark.
3. General provisions
3.1. Material to be collected
Each batch to be tested must be sampled separately. The large lots shall be divided into sublots of the lot sampled separately in accordance with point 4.3.
3.2. Preliminary measures
When samples are taken and prepared, precautions must be taken to prevent any changes likely to affect the content of the Fusarium toxin, adversely affect the analytical determination or impair the representativeness of the aggregate samples.
3.3. Partial samples
Where possible, incremental samples shall be taken from different locations throughout the lot or sublot.
The derogation from the procedure must be recorded in the protocol.
3.4 Preparation of the aggregate sample
The aggregate sample shall be prepared by association of incremental samples.
3.5 Duplicate samples
Duplicated samples shall be taken from a homogenised aggregate sample for testing to confirm the result, defence in a trade dispute or for arbitration.
3.6 Packaging and transport of samples
Each sample shall be stored in a clean container of inert material which provides adequate protection against contamination and damage during transport. All necessary measures shall be taken to prevent a change in the composition of the sample which may occur during transport or storage.
3.7 Closure and marking of samples
Each sample taken for official purposes shall be sealed at the place of collection and marked in accordance with Section 6. Each sampling shall be subject to a sampling report in accordance with Section 5.
4.
4.1 Different types of lots
Foodstuffs shall be put into circulation in bulk, in containers or in individual packs such as bags, bags or single retail packs. Sampling shall be carried out for each type of putting into circulation.
Without prejudice to the specific provisions of points 4.3, 4.4 and 4.5, the formula below may be used as a guide for the sampling of batches to take the form of individual packages when put into circulation, such as bags, bags or individual retail packages.
range n = weight of lot × weight of incremental sample weight of aggregate sample × weight of individual package
- weight - in kg
- selection range - each nth bag or bag from which a partial sample must be taken (decimal places are rounded to the nearest integer).
4.2. Weight of the incremental sample
The weight of the incremental sample shall be at least 100 grams, unless otherwise specified in this Annex. For lots in the form of retail packages, the weight of the incremental sample depends on the weight of the retail package.
4.3. Sampling procedure for cereals and cereal products
Table 1: Distribution of lots into sublots depending on product and batch weight
| Komodita | Hmotnost šarže (t) | Hmotnost nebo počet částí šarže | Počet dílčích vzorků | Hmotnost souhrnného vzorku (kg) |
|---|---|---|---|---|
| Obiloviny a výrobky z obilovin | ≥ 1500 | 500 t | 100 | 10 |
| > 300 a < 1500 | 3 části šarže | 100 | 10 | |
| ≥ 50 a ≤ 300 | 100 t | 100 | 10 | |
| < 50 | - | 3 - 100*) | 1 - 10 | |
| *) v závislosti na hmotnosti šarže – viz tabulka 2 | ||||
4.4. Sampling procedure for cereals and cereal products for lots exceeding 50 tonnes inclusive
Where a portion of the lot can be physically separated, each batch shall be physically divided into parts of the lot in accordance with Table 1. Since the weight of the lot is not always an exact multiple of the weight of the sublot, the weight of the sublot may not exceed that weight by more than 20%.
Each part of the lot must be sampled separately.
Where it is not possible to use the sampling method referred to in this point because of the economic consequences resulting from the damage to the lot, such as the form of packaging or means of transport, an alternative sampling method may be used provided that it is as representative as possible and is fully described and documented.
4.5. Sampling procedure for cereals and cereal products for lots up to 50 tonnes
For lots of cereals and cereal products up to 50 tonnes, a sampling plan consisting of 10 to 100 incremental samples shall be used, depending on the weight of the lot, resulting in an aggregate sample of 1 to 10 kg. For very small batches (≤ 0,5 tonnes), a smaller number of incremental samples may be taken, but a aggregate sample of all incremental samples must also be at least 1 kg.
The numbers given in Table 2 shall be used to determine the number of incremental samples to be taken.
Table 2: Number of incremental samples to be taken depending on the weight of the lot of cereals and cereal products
| Hmotnost šarže (t) | Počet dílčích vzorků |
|---|---|
| ≤ 0,05 | 3 |
| >0,05 - ≤ 0,50 | 5 |
| >0,50 - ≤ 1,00 | 10 |
| >1,00 - ≤ 3,00 | 20 |
| >3,00 - ≤ 10,00 | 40 |
| >10,00 - ≤ 20,00 | 60 |
| >20,00 - ≤ 50,00 | 100 |
4.6. Sampling procedure for foods intended for infants and young children
For foods intended for infants and young children, the sampling procedure for cereals and cereal products in point 4.5 shall apply. The number of incremental samples to be taken depends on the weight of the lot, with a minimum of 10 and a maximum of 100 incremental samples taken according to Table 2. For very small batches (≤ 0,5 tonnes), a smaller number of incremental samples may be taken, but a aggregate sample of all incremental samples must also be at least 1 kg.
The weight of the incremental sample shall be at least 100 grams. For lots in the form of retail packages, the weight of the incremental sample depends on the weight of the commercial packaging and for very small batches (< 0,5 tonnes), the incremental samples must have a mass such that a aggregate sample of at least 1 kg is obtained by combining the incremental samples.
The weight of the aggregate sample shall be between 1 and 10 kg and shall be sufficiently mixed.
4.7 Sampling at retail sale
Sampling of foodstuffs at retail stage shall be carried out mutatis mutandis in accordance with the provisions of this Annex concerning sampling. Where this is not possible, other effective retail sampling procedures may be used provided that they are sufficiently representative of the sampled lot.
5. Admission of the lot or sublot
The lot shall be accepted if the aggregate sample complies with the maximum limit taking into account measurement uncertainty and correction for recovery.
The lot shall be rejected if the aggregate sample exceeds the maximum limit without any doubt, taking into account measurement uncertainty and correction for recovery.
Příloha č. 47
Annex No 47 to Decree No 211 / 2004 Coll.
Preparation of samples and testing requirements for official control of compliance with maximum levels of Fusarium toxins in foodstuffs
1. Provisional measures
As the distribution of Fusarium toxins is very uneven, the preparation of laboratory samples and, in particular, homogenisation of samples must be given greater attention.
Any quantity of food collected shall be used to prepare the test sample.
2. Processing of the sample received by the laboratory
Each laboratory sample shall be finely ground and thoroughly mixed by a process to achieve complete homogenisation.
Where the maximum level applies to the dry matter, the dry matter content of the product in the part of the homogenised sample shall be determined by a method which can be shown to allow accurate determination of the dry matter.
3. Distribution of samples for testing to confirm result and defence
Duplicated samples shall be taken from a homogenised sample for testing to confirm the result, defence in a trade dispute and arbitration.
4. Methods of testing and requirements for laboratory control
4.1 Definitions
The most common definitions to be used by the laboratory are:
r = repeatability: the value below which the absolute value of the difference between the results of the 2 separate determinations under repeatability conditions (i.e. the same sample, the same worker, the same apparatus, the same laboratory, will be determined shortly) is expected to lie with a given probability (usually 95%); r = 2,8 × sr.
sr = standard deviation calculated from results obtained under repeatability conditions.
RSDr = Relative standard deviation calculated from results obtained under the given repeatability conditions sr / x tj × 100.
R = Reproducibility: the value below which the absolute value of the difference between the results of the two separate determinations under reproducibility conditions (i.e. for the same material obtained by the workers of different laboratories, using the standardised test method, is expected to lie with a given probability (usually 95%); R = 2.8 x sR.
sR = standard deviation calculated from results obtained under reproducibility conditions.
RSDR = Relative standard deviation calculated from results obtained under reproducibility conditions sR / x ^ × 100.
4.2 General requirements
The methods of testing used for food control purposes shall comply with Section 9.
4.3. Specific requirements
4.3.1. Working characteristics
Where specific methods are not laid down directly by the European Communities' applicable regulation, laboratories shall choose a validated method provided that the method chosen meets the working characteristics set out in Tables 1, 2, 3 and 4.
Table 1: Working characteristics for deoxynivalenol
| Množství μg/kg | deoxynivalenol | ||
|---|---|---|---|
| RSDr % | RSDR % | Výtěžnost % | |
| >100,00 - ≤ 500,00 | ≤ 20,00 | ≤ 40,00 | 60,00 – 110,00 |
| >500,00 | ≤ 20,00 | ≤ 40,00 | 70,00 – 120,00 |
Table 2: Working characteristics for zearalenone
| Množství μg/kg | zearalenon | ||
|---|---|---|---|
| RSDr % | RSDR % | Výtěžnost % | |
| ≤ 50,00 | ≤ 40,00 | ≤ 50,00 | 60,00 – 120,00 |
| > 50,00 | ≤ 25,00 | ≤ 40,00 | 70,00 – 120,00 |
Table 3: Working characteristics for fumonisin B1 and B2
| Množství μg/kg | Fumosin B1 nebo B2 | ||
|---|---|---|---|
| RSDr % | RSDR % | Výtěžnost % | |
| ≤ 500,00 | ≤ 30,00 | ≤ 60,00 | 60,00 – 120,00 |
| >500,00 | ≤ 20,00 | ≤ 30,00 | 70,00 – 110,00 |
Tabulka 4: Pracovní charakteristiky pro T-2 a HT-2 toxin
| Množství μg/kg | T-2 toxin | ||
|---|---|---|---|
| RSDr % | RSDR % | Výtěžnost % | |
| 50,00 – 250,00 | ≤ 40,00 | < 60,00 | 60,00 – 130,00 |
| >250,00 | ≤ 30,00 | ≤ 50,00 | 70,00 – 130,00 |
| Množství μg/kg | HT-2 toxin | ||
|---|---|---|---|
| RSDr % | RSDR % | Výtěžnost % | |
| 100,00 – 200,00 | ≤ 40,00 | ≤ 60,00 | 60,00 – 130,00 |
| >200,00 | ≤ 30,00 | ≤ 50,00 | 70,00 – 130,00 |
The detection limits of the methods used are not given because the accuracy is given for the concentrations considered.
The accuracy of the method corresponds to the value calculated from the Horwitz equation:
RSDR = 2 (1 - 0,5logC)
where:
- RSDR is the relative standard deviation calculated from the results obtained under reproducibility conditions sR / x ^ × 100,
- C is the concentration ratio (i.e. 1 = 100g / 100g, 0,001 = 1,000 mg / kg).
This is a generalized precision equation, which has shown that for most routine methods of analysis, analyte and matrix do not matter but only concentration.
4.3.2. Access based on suitability for the purpose
An alternative approach based on suitability for a given purpose may be used to evaluate the acceptability of test methods, within which only suitability functions are defined as a single parameter where there is a limited number of fully validated test methods. The suitability function is a function of uncertainty which sets the highest value of uncertainty considered appropriate for the purpose.
In view of the limited number of test methods that are fully validated by the inter-laboratory test, in particular for the determination of T-2 and HT-2 toxin, an approach based on the function of uncertainty determining the highest acceptable uncertainty shall also be used to assess the suitability for the purpose of the test method used by the laboratory. A laboratory may use a method that provides results with maximum standard uncertainty. The maximum standard uncertainty shall be calculated using the following equation:
Uf = LOD / 22 + α x C2
where:
Uf is the maximum standard uncertainty,
LOD is the limit of detection of the method,
C is the appropriate concentration (μg / kg),
α is a constant numerical factor used depending on the value C. The values to be used are given in Table 5.
If the test method provides results with uncertainty of measurement less than the maximum standard uncertainty, the method shall be appropriate to the same extent as the method that meets the working characteristics given in the tables.
Table 5: Numeric values to be used for α as a constant in the equation given in this point depending on the respective concentration
| C (μg/kg) | α |
|---|---|
| ≤ 50,00 | 0,20 |
| 51,00 – 500,00 | 0,18 |
| 501,00 – 1000,00 | 0,15 |
| 1001,00 – 10000,00 | 0,12 |
| > 10000,00 | 0,10 |
4.4 Calculation of recovery and presentation of results
The test results shall be reported with or without correction for recovery. The method of indicating recovery and its value shall be indicated. The result of the recovery correction test shall be used to check compliance with the limit.
The test result shall be given in the form (x ± U) where x is the test result and U is the expanded measurement uncertainty.
4.5 Requirements for laboratories
Laboratories must comply with the requirements of the specific legislation *).
*) For example § 3 (3) of Act No. 146 / 2002 Coll., on State Agricultural and Food Inspection and on the amendment of certain related laws, as amended. '
Efficacy
This Decree shall take effect on 1 December 2005.
Minister:
Ing. Zgarba v. r.
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Regulation Information
| Citation | Decree No. 459 / 2005 Coll., amending Decree No. 211 / 2004 Coll., on methods of testing and method of sampling and preparation of reference samples, as amended |
|---|---|
| Regulation Type | Order |
| Author | - |
| Collection | Code of Laws |
| Date of Promulgation | 28.11.2005 |
|---|---|
| Effective from | 01.12.2005 |
| Effective until | - |
| Status | Valid |
The regulation text is for informational purposes only.
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