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VETERINARY SERVICES ACT (CAP. 437)
Sampling Methods and Methods of Analysis for the Official Control of the Levels for Certain Contaminants in Foodstuffs Rules, 2005
IN exercise of the powers conferred by article 25 of the Veterinary Services Act, the Minister for Rural Affairs and the Environment has made the following rules>-
1. (1) The title to these rules is the Sampling Methods and Methods of Analysis for the Official Control of the Levels for Certain Contaminants in Foodstuffs Rules, 2005.
(2) The scope of these rules is to implement the rules found under European Union Council Directive 98#53#EC establishing methods of analysis for the official control of feedingstuffs.
2. For the purposes of these rules -
“the competent authority” means the Veterinary Services within Malta as provided under article 2 of the Veterinary Services Act, or any other authority to which such responsibility has been delegated by the Veterinary Services.
3. The competent authority shall take all measures necessary to ensure that the sampling for the official control of the levels of aflatoxins in foodstuffs is carried out in accordance with the methods described in Schedule I to these rules.
4. The competent authority shall take all measures necessary to ensure that sample preparation and methods of analyses used for the official control of the levels of aflatoxins in foodstuffs comply with the criteria described in Schedule II to these rules.
Title and scope.
Definitions.
Necessary measures to ensure sampling for the official control of the levels of aflatoxins in foodstuffs.
Necessary measures to ensure sample preparation and methods of analyses used for the official control of the levels of aflatoxins in foodstuffs.
B 1400
SCHEDULE I
Methods of sampling for official checking control of the levels of aflatoxins in certain foodstuffs1. Purpose and scopeSamples intended for official checking of the levels of aflatoxin content in foodstuffs shall be taken according to the methods described below. Aggregate samples thus obtained shall be considered as representative of the lots. Compliance with maximum limits laid down in European Commission Regulation 98/1525/EC shall be established on the basis of the levels determined in the laboratory samples.
2. DefinitionsLot: an identifiable quantity of a food commodity delivered at one time and determined by the official to have common characteristics, such as origin, variety, type of packing, packer, consignor or markings.
Sublot: designated part of a large lot in order to apply the sampling method on that designated part. Each sublot must be physically separate and identifiable.
Incremental sample: a quantity of material taken from a single place in the lot or sublot.
Aggregate sample: the combined total of all the incremental samples taken from the lot or sublot.
Laboratory sample: sample intended for the laboratory ( = subsample).
3. General provisions
3.1. Personnel
Sampling shall be performed by an authorised person as specified by the competent authority.
B 1401
3.2. Material to be sampled
Each lot which is to be examined must be sampled separately. In accordance with the specific provisions in point 5 of this Schedule, large lots should be subdivided into sublots to be sampled separately.
3.3. Precautions to be taken
In the course of sampling and preparation of the laboratory samples, precautions must be taken to avoid any changes which would affect the aflatoxin content, adversely affect the analytical determination or make the aggregate samples unrepresentative.
3.4. Incremental samples
As far as possible incremental samples should be taken at various places distributed throughout the lot or sublot. Departure from this procedure must be recorded in the record provided for in 3.8.
3.5. Preparation of the aggregate sample and the laboratory samples (subsamples) The aggregate sample is made up by uniting and sufficiently mixing the incremental samples. After mixing, the aggregate sample must be divided into equal subsamples in accordance with the specific provisions of point 5 of this Schedule.
The mixing is necessary to ensure that each subsample contains Portions of the whole lot or sublot.
3.6. Replicate samples
The replicate samples for enforcement, trade (defence) and referee purposes are to be taken from the homogenised laboratory sample, unless this conflicts with Member States' rules on sampling.
3.7. Packaging and transmission of laboratory samples
Each laboratory sample shall be placed in a clean, inert container offering adequate protection from contamination and against damage in transit. All necessary precautions shall be taken to avoid any change in composition of the laboratory sample which might arise during transportation or storage.
3.8. Sealing and labelling of laboratory samples
B 1402
Each sample taken for official use shall be sealed at the place of sampling and identified following the Member State's regulations. A record must be kept of each sampling, permitting each lot to be identified unambiguously and giving the date and place of sampling together with any additional information likely to be of assistance to the analyst.
4. Explanatory provisions4.1. Different types of lots
Food commodities may be traded in bulk, containers, or individual packings (sacks, bags, retail packings, etc.). The sampling procedure can be applied to all the different forms in which the commodities are put on the market.
Without prejudice to the specific provisions as laid down in point 5 of this Schedule, the following formula can be used as a guide for the sampling of lots traded in individual packings (sacks, bags, retail packings, etc.):
Sampling frequency (SF) = Weight of the lot x weight of the incremental sample
Weight of the aggregate sample x weight of individual packing
— Weight: in kg
Sampling frequency (SF): every nth sack or bag from which an incremental sample must be taken (decimal figures should be rounded to the nearest whole number).
4.2. Weight of the incremental sample
The weight of the incremental sample should be about 300 grams unless otherwise defined in point 5 of this Schedule and with the exception of spices in which case the weight of the incremental sample is about 100 grams. In the case of retail packings, the weight of the incremental sample depends on the weight of the retail packing.
4.3. Number of incremental samples for lots of less than 15 tonnes
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, unless otherwise defined in
B 1403
point 5 of this Schedule. The figures in the following table may be used to determine the number of incremental samples to be taken.
Table 1: Number of incremental samples to be taken depending on the weight of the lotLot weight (tonnes) | No 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 |
5. Specific provisions
5.1. General survey of the sampling procedure for groundnuts, nuts, dried fruit, spices and cereals
Table 2: Subdivision of lots into sublots depending on product and lot weightCommodity | Lot weight (tonnes) | Weight or number of sublots | Number of incremental samples | Aggregate sample Weight (kg) |
Dried figs and other dried fruit | ≥ 15 < 15 | 15-30 tonnes — | 100 10-100 (1) | 30 ≤ 30 |
Groundnuts, pistachios, Brazil nuts and other | ≥ 500 > 125 and < 500 ≥ 15 and ≤ 125 | 100 tonnes 5 sublots 25 tonnes | 100 100 100 | 30 30 30 |
B 1404
nuts | < 15 | — | 10-100 (1) | ≤ 30 |
Cereals | ≥ 1 500 > 300 and < 1 500 ≥ 50 and ≤ 300 < 50 | 500 tonnes 3 sublots 100 tonnes — | 100 100 100 10-100 (1) | 30 30 30 1-10 |
Spices | ≥ 15 < 15 | 25 tonnes — | 100 10-100 (1) | 10 1-10 |
(1) Depending on the lot weight — see point 4.3 or 5.3 of this Schedule. |
5.2. Groundnuts, pistachios and Brazil nuts
Dried figs
Cereals (lots ≥ 50 tonnes)
Spices
5.2.1. Sampling procedure
— On condition that the sublot can be separated physically, each lot must be subdivided into sublots following Table 2 at point 5.1. Taking into account that the weight of the lot is not always an exact multiple of the weight of the sublots, the weight of the sublot may exceed the mentioned weight by a maximum of 20 %,
— each sublot must be sampled separately,
— number of incremental samples: 100. In the case of lots under 15 tonnes, 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 (see point 4.3),
— weight of the aggregate sample = 30 kg which has to be mixed and to be divided into three equal subsamples of 10 kg before grinding (this division into three subsamples is not necessary in the case of groundnuts, nuts, dried fruit and maize intended for further sorting or other physical treatment, however, this will depend upon the availability of equipment which is able to homogenise a 30 kg sample). In cases where the aggregate sample weights are under 10 kg, the aggregate sample must not be divided into three subsamples. In the case of spices the aggregate sample weighs not more than 10 kg and therefore no division in subsamples is necessary,
B 1405
— laboratory sample: a subsample of 10 kg (each subsample must be separately ground finely and mixed thoroughly to achieve complete homogenisation, in accordance with the provisions laid down in Schedule II),
— 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 packaging 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.
5.2.2. Acceptance of a lot or sublot
— For groundnuts, nuts, dried fruit and maize subjected to a sorting or other physical treatment and spices:
— acceptance if the aggregate sample or the average of the subsamples conforms to the maximum limit, taking into account the measurement uncertainty and correction for recovery,
— rejection if the aggregate sample or the average of the subsamples exceeds the maximum limit beyond reasonable doubt taking into account the measurement uncertainty and correction for recovery,
— for groundnuts, nuts, dried fruit and cereals intended for direct human consumption and cereals, with the exception of maize, to be subjected to a sorting or other physical treatment:
— acceptance if none of the subsamples exceeds the maximum limit, taking into account the measurement uncertainty and correction for recovery,
— rejection if one or more of the subsamples exceeds the maximum limit beyond reasonable doubt taking into account the measurement uncertainty and correction for recovery,
— where the aggregate sample is under 10 kg:
— acceptance if the aggregate sample conforms to the maximum limit, taking into account the measurement uncertainty and correction for recovery,
B 1406
— rejection if the aggregate sample exceeds the maximum limit beyond reasonable doubt taking into account analytical uncertainty and correction for recovery.
5.3. Nuts other than groundnuts, pistachios and Brazil nuts
Dried fruit other than figs
Cereals (lots under 50 tonnes)
5.3.1. Sampling procedure
For these products, the sampling procedure laid down in point 5.2.1 may be applied. However, taking into account the low incidence of contamination for these products and/or the newer forms of packaging in which products can be traded, simpler sampling methods may be applied.
For cereal lots under 50 tonnes, 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 cerealsLot weight
(tonnes)
≤1
> 1 - ≤3
> 3 - ≤10
> 10 - ≤20
> 20 - ≤50
Number of incremental samples
10
20
40
60
100
5.3.2. Acceptance of a lot or sublot
See point 5.2.2.
5.4. Milk
5.4.1. Sampling procedure
B 1407
Sampling in accordance with European Union Commission Decision
91/180/EEC of 14 February 1991 laying down certain methods of analysis and testing of raw milk and heat-treated milk:
— number of incremental samples: minimum 5,
— weight of aggregate sample: minimum 0,5 kg or litres.
5.4.2. Acceptance of a lot or sublot
— Acceptance if the aggregate sample conforms to the maximum limit, taking into account the measurement uncertainty and correction for recovery,
— rejection if the aggregate sample exceeds the maximum limit beyond reasonable doubt taking into account the measurement uncertainty and correction for recovery.
5.5. Derived products and compound foods
5.5.1. Milk products
5.5.1.1. Sampling procedure
Sampling in accordance with European Union Commission Directive
87/524/EEC of 6 October 1987 laying down European Community methods of sampling for chemical analysis for the monitoring of preserved milk products. Number of incremental samples: minimum 5.
For the other milk products an equivalent method of sampling is used.
5.5.1.2. Acceptance of a lot or sublot
— Acceptance if the aggregate sample conforms to the maximum limit, taking into account the measurement uncertainty and correction for recovery,
— rejection if the aggregate sample exceeds the maximum limit beyond reasonable doubt taking into account the measurement uncertainty and correction for recovery.
5.5.2. Other derived products with very small particle weight, i.e. flour, fig paste, peanut butter (homogeneous distribution of aflatoxin contamination).
5.5.2.1. Sampling procedure
B 1408
— Number of incremental samples: 100. For lots of under 50 tonnes the number of incremental samples should be 10 to 100, depending on the lot weight (see Table 3 at point 5.3.1 of this Schedule),
— the weight of the incremental sample should be about 100 grams. In the case of lots in retail packing, the weight of the incremental sample depends on the weight of the retail packing,
— weight of aggregate sample = 1-10 kg sufficiently mixed.
5.5.2.2. Number of samples to be taken
— The number of aggregate samples to be taken depends on the lot weight.
The division of large lots into sublots must be done as defined for cereals in Table 2 under point 5.1,
— each sublot must be sampled separately.
5.5.2.3 Acceptance of a lot or sublot
— Acceptance if the aggregate sample conforms to the maximum limit, taking into account the measurement uncertainty and correction for recovery,
— rejection if the aggregate sample exceeds the maximum limit beyond reasonable doubt taking into account the measurement uncertainty and correction for recovery.
5.6. Other derived products with a relatively large particle size (heterogeneous distribution of aflatoxin contamination)
Sampling procedure and acceptance as defined at points 5.2 and 5.3 of
This Schedule for the raw agricultural product.
5.7. Foods intended for infants and young children
5.7.1. Sampling procedure
The sampling procedure as mentioned for milk and derived products as well as for compound food in points 5.4, 5.5 and 5.6 applies.
5.7.2. Acceptance of a lot
— Acceptance if the aggregate sample conforms to the maximum limit, taking into account the measurement uncertainty and correction for recovery,
B 1409
— Rejection if the aggregate sample exceeds the maximum limit beyond reasonable doubt, taking into account the measurement uncertainty and correction for recovery.
6. Sampling at retail stageSampling of foodstuffs at the retail stage should be done where possible in accordance with the above sampling provisions. Where this is not possible, other effective sampling procedures at retail stage can be used provided that they ensure sufficient representativeness for the sampled lot.
B 1410
SCHEDULE II
Sample preparation and criteria for methods of analysis used in official checking of the levels of aflatoxins in certain foodstuffs1. Introduction1.1. Precautions
Daylight should be excluded as much as possible during the procedure, since aflatoxin gradually breaks down under the influence of ultra-violet light. As the distribution of aflatoxin is extremely non-homogeneous, samples should be prepared — and especially homogenised — with extreme care.
All the material received by the laboratory is to be used for the preparation of test material.
1.2. Calculation of proportion of shell/kernel of whole nuts
The limits fixed for aflatoxins in European Union Commission Regulation (EC) No 1525/98 apply to the edible part.
The level of aflatoxins in the edible part can be determined by:
— shelling samples of nuts ‘in shell’ 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. 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
B 1411
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 as received in the laboratoryFinely grind and thoroughly mix each laboratory sample using a process that has been demonstrated to achieve complete homogenisation. In case the maximum level applies to the dry matter, the dry matter content shall be determined on a part of the homogenised sample, using a procedure that hasbeen demonstrated to determine accurately the dry matter content.
3. Subdivision of samples for enforcement and defence purposesThe replicate samples for enforcement, trade (defence) and referee purposes shall be taken from the homogenised material unless this conflicts with Member States' rules on sampling.
4. Method of analysis to be used by the laboratory and laboratory control requirements4.1. Definitions
A number of the most commonly used definitions that the laboratory will be required to use are given below:
The most commonly quoted precision parameters are repeatability and reproducibility.
r = repeatability, the value below which the absolute difference between two single test results obtained under repeatability conditions (i. e. same sample, same operator, same apparatus, same laboratory, and short interval of time) may be expected to lie within a specific probability (typically 95 %) and hence r = 2,8 × sr
sr = Standard deviation, calculated from results generated under
repeatability conditions
B 1412
RSDr = relative standard deviation, calculated from results generated under repeatability conditions [(S r/x) × 100], where x is the average of results over all laboratories and samples
R = reproducibility, the value below which the absolute difference between single test results obtained under reproducibility conditions (i. e. on identical material obtained by operators in different laboratories, using the standardised test method) may be expected to lie within a certain probability (typically 95 %); R = 2,8 sR
sR = standard deviation, calculated from results under reproducibility
conditions
RSDR = relative standard deviation calculated from results generated under reproducibility conditions [(S R/x) × 100]
4.2. General requirements
Methods of analysis used for food control purposes must comply whenever possible with the provisions of points 1 and 2 of the Annex to European Union Council Directive 85/591/EEC.
4.3. Specific requirements
Where no specific methods for the determination of aflatoxin levels in foodstuffs are prescribed at European Community level, laboratories may select
any method provided the selected method meets the following criteria:
Criterion | Concentration range | Recommended value | Maximum permitted value |
Blanks | All | Negligible | |
Recovery — Aflatoxin M1 | 0,01-0,05 µg/kg >0,05 µg/kg | 60 to 120 % 70 to 110 % | |
Recovery — Aflatoxins B1, B2, G1, G2 | < 1,0 µg/kg 1-10 µg/kg >10 µg/kg | 50 to 120 % 70 to 110 % 80 to 110 % | |
Precision RSDR | All | As derived from Horwitz equation | 2 × value derived from Horwitz equation |
Precision RSDr may be calculated as 0,66 times precision RSDR at the concentration of interest.
B 1413
Notes:
— Values to apply to both B1 and sum of B1+ B2+ G1+ G2,
— if sum of individual aflatoxins B1+ B2+ G1+ G2 are to be reported, then response of each to the analytical system must be either known or equivalent,
— the detection limits of the methods used are not stated as the precision values are given at the concentrations of interest,
— the precision values are calculated from the Horwitz equation, i. e.: RSDR
= 2 (1-0,5 logC) where:
— RSDR is the relative standard deviation calculated from results generated under reproducibility conditions [(SR/x) × 100]
— C is the concentration ratio (i. e. 1 = 100 g/100 g, 0,001 = 1 000 mg/kg).
This is a generalised precision equation which has been found to be independent of analyte and matrix but solely dependent on concentration for most routine methods of analysis.
4.4. Recovery calculation and reporting of results
The analytical result is to be reported corrected or uncorrected for recovery. The manner of reporting and the level of recovery must be reported. The analytical result corrected for recovery is used for checking compliance (see Schedule I, points 5.2.2, 5.3.2, 5.4.2, 5.5.1.2 and 5.5.2.3).
The analytical result has to be reported as x +/- U whereby x is the analytical result and U is the expanded measurement uncertainty, using a coverage factor of 2 which gives a level of confidence of approximately 95 %.
4.5. Laboratory quality standards
Laboratories must comply with European Council Directive 93/99/EEC.
B 1414
Ippubblikat mid-Dipartiment ta’ l-Informazzjoni (doi.gov.mt) Valletta - Published by the Department of Information - (doi.gov.mt) - Valletta
Mitbug] fl-Istamperija tal-Gvern - Printed at the Government Printing Press
Prezz 72` - Price 72c
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