Commission Directive 2002/26/EC of 13 March 2002 laying down the sampling methods and the methods of analysis for the official control of the levels of ochratoxin A in foodstuffs (Text with EEA relevance)
Date: 2002-03-13
Institutions: European Commission
Subjects: consumer protection, food contamination, food standard, foodstuff, public health, toxic substance

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Official Journal of the European Communities

16.3.2002

COMMISSION DIRECTIVE 2002/26/EC

of 13 March 2002

laying down the sampling methods and the methods of analysis for the official control of the levels
of ochratoxin A in foodstuffs

(Text with EEA relevance)

THE COMMISSION OF THE EUROPEAN COMMUNITIES,

HAS ADOPTED THIS DIRECTIVE:

Having regard to the Treaty establishing the European
Community,

Having regard to Council Regulation (EEC) No 315/93 of 8
February 1993 laying down Community procedures
for
contaminants in food (1), and in particular Article 2 thereof,

Having regard to Council Directive 85/591/EEC of 20
December 1985 concerning the introduction of Community
methods of sampling and analysis for the monitoring of food-
stuffs intended for human consumption (2), and in particular
Article 1 thereof,

Whereas:

(1)

(2)

(3)

(4)

(5)

(6)

Commission Regulation (EC) No 466/2001 of 8 March
2001 setting maximum levels for certain contaminants
in foodstuffs (3), as last amended by Regulation (EC) No
472/2002 (4), fixes maximum limits for ochratoxin A in
certain foodstuffs.

Council Directive 93/99/EEC of 29 October 1993 on
the subject of additional measures concerning the official
control of foodstuffs (5) introduces a system of quality
standards for laboratories entrusted by the Member
States with the official control of foodstuffs.

Sampling plays a crucial part in the precision of the
determination of the levels of ochratoxin A, which are
very heterogeneously distributed in a lot.

It seems necessary to fix general criteria, which the
method of analysis has to comply with in order to
ensure that laboratories, in charge of the control, use
levels of
methods of
performance.

analysis with comparable

The provisions for the sampling and methods of analysis
have been drawn up on the basis of present knowledge
and they may be adapted to take account of advances in
scientific and technological knowledge.

The measures provided for in this Directive are in
accordance with the opinion of the Standing Committee
on the Food Chain and Animal Health,

Article 1

the sampling for the official control of

The Member States shall take all measures necessary to ensure
the levels of
that
ochratoxin A in foodstuffs is carried out in accordance with the
methods described in Annex I to this Directive.

Article 2

The Member States shall take all measures necessary to ensure
that sample preparation and methods of analyses used for the
official control of the levels of ochratoxin A in foodstuffs
comply with the criteria described in Annex II to this Directive.

Article 3

Member States shall bring into force the laws, regulations and
administrative provisions necessary to comply with this
Directive by 28 February 2003 at the latest. They shall forth-
with inform the Commission thereof.

those provisions,

When Member States adopt
they shall
contain a reference to this Directive or be accompanied by
such a reference on the occasion of their official publication.
Member States shall determine how such reference is to be
made.

Article 4

This Directive shall enter into force on the 20th day following
its publication in the Official Journal of the European Communities.

This Directive is addressed to the Member States.

Article 5

Done at Brussels, 13 March 2002.

For the Commission

David BYRNE

Member of the Commission

(1) OJ L 37, 13.2.1993, p. 1.
(2) OJ L 372, 31.12.1985, p. 50.
(3) OJ L 77, 16.3.2001, p. 1.
(4) See page 18 of this Official Journal.
(5) OJ L 290, 24.11.1993, p. 14.

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Official Journal of the European Communities

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METHODS OF SAMPLING FOR OFFICIAL CONTROL OF THE LEVELS OF OCHRATOXIN A IN CERTAIN
FOODSTUFFS

ANNEX I

1.

Purpose and scope

Samples intended for official checking of the levels of ochratoxin A 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 Regulation (EC) No 466/2001 shall be established on the basis of the
levels determined in the laboratory samples.

2. Definitions

Lot:

Sublot:

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

designated part of a 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.

3. General provisions

3.1. Personnel

Sampling shall be performed by an authorised person as specified by the Member States.

3.2. Material to be sampled

Each lot which is to be examined must be sampled separately. In accordance with the specific provisions of this
Annex,

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 samples precautions must be taken to avoid any changes which
would affect the ochratoxin A 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.

3.5. Preparation of the aggregate sample

The aggregate sample is made up by uniting the incremental samples.

3.6. Replicate samples

The replicate samples for enforcement, trade (defence) and referee purposes are to be taken from the homogenised
sample, unless this conflicts with Member States' rules on sampling.

3.7. Packaging and transmission of samples

Each 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 sample, which
might arise during transportation or storage.

3.8. Sealing and labelling of samples

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.

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4.

Specific provisions

4.1. 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 points 4.3, 4.4 and 4.5 of this Annex, the following
formula can be used as a guide for the sampling of lots traded in individual packings (sacks, bags, retail packings,
etc.):

— 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 aggregate sample

The weight of the incremental sample should be about 100 grams, unless otherwise defined in this Annex. In the
case of lots in retail packings, the weight of the incremental sample depends on the weight of the retail packing.

4.3. General survey of the sampling procedure for cereals and dried vine fruit

Table 1: Subdivision of lots into sublots depending on product and lot weight

Commodity

Lot weight
(tonnes)

Weight or number of
sublots

Number of incre-
mental samples

Aggregate sample
Weight
(kg)

Cereals and cereal products ≥ 1 500

> 300 and < 1 500
≥ 50 and ≤ 300
< 50

500 tonnes
3 sublots
100 tonnes
—

100
100
100
10-100 (1)

Dried vine fruit
raisins and sultanas)

(currants, ≥ 15
< 15

15-30 tonnes
—

100
10-100 (2)

10
10
10
1-10

10
1-10

(1) Depending on the lot weight — see Table 2 of this Annex.
(2) Depending on the lot weight — see Table 3 of this Annex.

4.4. Sampling procedure for cereals and cereal products (lots ≥ 50 tonnes) and dried vine fruit (lots ≥ 15 tonnes)

— On condition that the sublot can be separated physically, each lot must be subdivided into sublots following
Table 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 of cereals under 50 tonnes and lots of dried vine fruit

under 15 tonnes, see point 4.5. Weight of the aggregate sample = 10 kg.

— If

it

is not possible to carry out

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.

the method of sampling described above because of

4.5. Sampling provisions for cereals and cereal products (lots < 50 tonnes) and for dried vine fruit (lots < 15 tonnes)

For cereal lots under 50 tonnes and for dried vine fruit lots under 15 tonnes, the sampling plan has to be used with
10 to 100 incremental samples, depending on the lot weight, resulting in an aggregate sample of 1 to 10 kg.

The figures in the following table can be used to determine the number of incremental samples to be taken.

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Official Journal of the European Communities

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Table 2: Number of incremental samples to be taken depending on the weight of the lot of cereals

Lot weight
(tonnes)

Number of incremental samples

≤ 1
> 1 - ≤ 3
> 3 - ≤ 10
> 10 - ≤ 20
> 20 - ≤ 50

10

20

40

60

100

Table 3: Number of incremental samples to be taken depending on the weight of the lot of dried vine fruit

Lot weight
(tonnes)

Number of incremental samples

≤ 0,1
> 0,1 - ≤ 0,2
> 0,2 - ≤ 0,5
> 0,5 - ≤ 1,0
> 1,0 - ≤ 2,0
> 2,0 - ≤ 5,0
> 5,0 - ≤ 10,0
> 10,0 - ≤ 15,0

10

15

20

30

40

60

80

100

4.6. Sampling at retail stage

Sampling 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.

5. Acceptance of a lot or sublot

— Acceptance if the aggregate sample conforms to the maximum limit.
— Rejection if the aggregate sample exceeds the maximum limit.

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Official Journal of the European Communities

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SAMPLE PREPARATION AND CRITERIA FOR METHODS OF ANALYSIS USED IN OFFICIAL CHECKING OF
THE LEVELS OF OCHRATOXIN A IN CERTAIN FOODSTUFFS

ANNEX II

1.

Precautions

As the distribution of ochratoxin A is non-homogeneous, samples should be prepared — and especially homoge-
nised — with extreme care.

All the material received by the laboratory is to be used for the preparation of test material.

2.

Treatment of the sample as received in the laboratory

Finely grind and mix thoroughly the complete aggregate sample using a process that has been demonstrated to
achieve complete homogenisation.

3.

Subdivision of samples for enforcement and defence purposes

The 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 requirements

4.1. 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

Standard deviation, calculated from results generated under repeatability conditions

sr= 1
RSDr = Relative standard deviation, calculated from results generated under repeatability conditions [(sr/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

[(sR/x–) × 100].

standard deviation calculated from results generated under

reproducibility conditions

4.2. General requirements

Methods of analysis used for food control purposes must comply with the provisions of items 1 and 2 of the Annex
to Directive 85/591/EEC concerning the introduction of Community methods of sampling and analysis for the
monitoring of foodstuffs intended for human consumption.

4.3. Specific requirements

Where no specific methods for the determination of ochratoxin A levels in foodstuffs are prescribed at Community
level,

laboratories may select any method provided the selected method meets the following criteria:

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Level
µg/kg

< 1

1-10

Performance characteristics for ochratoxin A

RSDr
(%)

≤ 40

≤ 20

Ochratoxin A

RSDR
(%)

≤ 60

≤ 30

Recovery
(%)

50 to 120

70 to 110

— 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:

RSDR = 2(1−0,5logC)
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

The analytical result is to be reported corrected or uncorrected for recovery. The manner of reporting and the level of
recovery must be reported.

4.5. Laboratory quality standards

Laboratories must comply with Directive 93/99/EEC on the subject of additional measures concerning the official
control of foodstuffs.