1998L0053 — EN — 06.08.1998 — 000.001 — 1
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►B COMMISSIONDIRECTIVE98/53/EC
of16July1998
layingdownthesamplingmethodsandthemethodsofanalysisfortheofficialcontrolofthelevels
forcertain contaminantsinfoodstuffs
(TextwithEEArelevance)
(OJ L 201, 17.7.1998, p. 93)
Amended by:
Official Journal
No page date
►M1Commission Directive 2002/27/EC of 13 March2002 L 75 44 16.3.2002
▼B
COMMISSIONDIRECTIVE98/53/EC
of16July1998
layingdownthesamplingmethodsandthemethodsofanalysisfor
the official control of the levels for certain contaminants in food-
stuffs
(TextwithEEArelevance)
THE COMMISSION OF THE EUROPEAN COMMUNITIES,
Having regard to the Treaty establishing the European Community,
Having regard to Council Directive 85/591/EEC of 20 December 1985
concerning the introduction of Community methods of sampling andanalysis for the monitoring of foodstuffs intended for human consump-tion(
1), and in particular Article 1 thereof,
Whereas Commission Regulation (EC) No 1525/98 of 16 July 1998,
amending Commission Regulation (EC) No 194/97 setting maximumlevels for certain contaminants in foodstuffs(
2) fixes maximum limits
for aflatoxins in certain foodstuffs;
Whereas Council Directive 93/99/EEC of 29 October 1993 on the
subject of additional measures concerning the official control of food-
stuffs(3) introduces a system of quality standards for laboratories
entrusted by the Member States with the official control of foodstuffs;
Whereas sampling plays a crucial part in the precision of the determi-
nation of the levels of the aflatoxins which are very heterogeneouslydistributed in a lot;
Whereas 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 methods of analysis with comparable levelsof performance;
Whereas the provisions for the sampling and methods of analysis have
been drawn up on the basis of present knowledge and they may beadapted to take account of advances in scientific and technological
knowledge;
Whereas the methods of sampling used currently by the competent
authorities largely differ in the Member States; whereas the competentauthorities in certain Member States are not in a position to apply allthe provisions of this Directive in a short time; whereas it is, therefore,
necessary to provide a suitable period to apply these provisions;
Whereas Member States will have to modify their methods of sampling
gradually in order to comply with the provisions laid down in theAnnexes to this Directive by the time the Directive has to be applied;whereas it is, therefore, appropriate to examine regularly with theMember States the application of these provisions;
Whereas the measures provided for in this Directive are in accordance
with the opinion of the Standing Committee on Foodstuffs,
HAS ADOPTED THIS DIRECTIVE:
Article 1
The Member States shall take all measures necessary to ensure that the
sampling for the official control of the levels of aflatoxins in foodstuffsis carried out in accordance with the methods described in Annex I ofthis Directive.1998L0053 — EN — 06.08.1998 — 000.001 — 2
(1) OJ L 372, 31. 12. 1985, p. 50.
(2) See page 43 of this Official Journal.
(3) OJ L 290, 24. 11. 1993, p. 14.
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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 aflatoxins in foodstuffs comply with the criteria
described in Annex II of this Directive.
Article 3
The Member States shall, not later than 31 December 2000, bring into
force the laws, regulations or administrative provisions necessary tocomply with the provisions of this Directive. They shall forthwithnotify the Commission thereof.
When Member States adopt these provisions, the provisions shall
contain a reference to this Directive or shall be accompanied by suchreference at the time of their official publication. The procedure for
suchreference sh all be adopted by Member States.
Article 4
This Directive shall enter into force on the 20
thday following its publi-
cation in the Official Journal of the European Communities .
This Directive is addressed to the Member States.1998L0053 — EN — 06.08.1998 — 000.001 — 3
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ANNEX I
Methodsof samplingfor official checking control of the levels of aflatoxins
incertainfoodstuffs
1.Purposeandscope
Samples 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 Commission
Regulation (EC) No 1525/98 shall be established on the basis of the
levels determined in the laboratory samples.
2.Definitions
Lot: 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.
Eachsublot must be ph ysically 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.Generalprovisions
3.1.Personnel
Sampling shall be performed by an authorised person as specified by
the Member States.
3.2.Material to be sampled
Eachlot wh ichis to be examined must be sampled separately. In accor-
dance with the specific provisions in point 5 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 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 withth e specific provi-
sions of point 5 of this Annex.
The mixing is necessary to ensure that each subsample contains
portions of the whole lot or sublot.1998L0053 — EN — 06.08.1998 — 000.001 — 4
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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
Eachlaboratory sample sh all 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 trans-
portation or storage.
3.8.Sealing and labelling of laboratory 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 eachsampling, permitting eachlot to be identi-
fied unambiguously and giving the date and place of sampling together
withany additional information likely to be of assistance to th e analyst.
4.Explanatoryprovisions
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 point 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 pack-
ings, etc.):
Sampling frequency (SF) =Weight of the lot /C2weight of the incremental sample
Weight of the aggregate sample /C2weight of individual packing
—Weight: in kg
Sampling frequency (SF): every nthsack or bag from wh ichan incremental
sample must be taken (decimal figures should be rounded to the nearestwhole 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 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.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 other-
wise defined in point 5 of this Annex. The figures in the following table
may be used to determine the number of incremental samples to be
taken.
Table1: Number of incremental samples to be taken depending on the
weight of the lot
Lot 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 1001998L0053 — EN — 06.08.1998 — 000.001 — 5
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5.Specificprovisions
5.1.General survey of the sampling procedure for groundnuts, nuts, dried
fruit and cereals
Table2: Subdivision of lots into sublots depending on product and lot weight
CommodityLot weight
(tonnes)Weight or number
of sublotsNumber of
incremental
samplesAggregate
sample
Weight (kg)
Dried figs and other
dried fruit≥15 15-30 tonnes 100 30
< 15 — 10-100 (1)≤30
Groundnuts, pista-
chios, Brazil nuts and
other nuts≥500 100 tonnes 100 30
> 125 and < 500 5 sublots 100 30
≥15 and≤125 25 tonnes 100 30
< 15 — 10-100 (1)≤30
Cereals ≥1500 500 tonnes 100 30
> 300 and < 1 500 3 sublots 100 30
≥50 and≤300 100 tonnes 100 30
< 50 — 10-100 (1) 1-10
(1) Depending on the lot weight — see point 4.3 or 5.3 of this Annex.
5.2.Groundnuts, pistachios and Brazil nuts
Dried figsCereals(lots≥50 tonnes)
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 %,
— eachsublot 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 and dried fruit 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,
— laboratory sample: a subsample of 10 kg (eachsubsample must be
separately ground finely and mixed thoroughly to achieve complete
homogenisation, in accordance with the provisions laid down in
Annex 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.1998L0053 — EN — 06.08.1998 — 000.001 — 6
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5.2.2. Acceptance of a lot or sublot
— For groundnuts, nuts and dried fruit subjected to a sorting or other
physical treatment:
— acceptance if the aggregate sample or the average of the
subsamples conforms to the maximum limit,
— rejection if the aggregate sample or the average of the subsam-
ples exceeds the maximum limit,
— for groundnuts, nuts, dried fruit and cereals intended for direct
human consumption:
— acceptance if none of the subsamples exceeds the maximum
limit,
— rejection if one or more of the subsamples exceeds the
maximum limit,
— where the aggregate sample is under 10 kg:
— acceptance if the aggregate sample conforms to the
maximum limit,
— rejection if the aggregate sample exceeds the maximum
limit.
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.
Table3: Number of incremental samples to be taken depending on the
weight of the lot of cereals
Lot weight
(tonnes)Number of incremental samples
≤11 0
>1-≤32 0
>3-≤10 40
>1 0-≤20 60
>2 0-≤50 100
5.3.2. Acceptance of a lot or sublot
See point 5.2.2.
5.4.Milk
5.4.1. Sampling procedure
Sampling in accordance withCommission Decision 91/180/EEC of 14
February 1991 laying down certain methods of analysis and testing of
raw milk and heat-treated milk(1):
— 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,
— rejection if the aggregate sample exceeds the maximum limit.1998L0053 — EN — 06.08.1998 — 000.001 — 7
(1) OJ L 93, 13. 4. 1991, p. 1.
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5.5.Derived products and compound foods
5.5.1. Milk products
5.5.1.1. Sampling procedure
Sampling in accordance withCommission Directive 87/524/EEC of 6
October 1987 laying down Community methods of sampling for
chemical analysis for the monitoring of preserved milk products(1).
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,
— rejection if the aggregate sample exceeds the maximum limit.
5.5.2. Other derived products with very small particle weight, i.e. flour, fig
paste, peanut butter (homogeneous distribution of aflatoxin contamina-
tion)
5.5.2.1. Sampling procedure
— 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 Annex),
— 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 ►M1in Table 2 under point 5.1 ◄,
— eachsublot must be sampled separately.
5.5.2.3 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.
5.6.Other derived products with a relatively large particle size (heteroge-
neous distribution of aflatoxin contamination)
Sampling procedure and acceptance as defined at points 5.2 and 5.3 of
this Annex for the raw agricultural product.1998L0053 — EN — 06.08.1998 — 000.001 — 8
(1) OJ L 306, 28. 10. 1987, p. 24.
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ANNEX II
Sample preparation and criteria for methods of analysis used in official
checkingofthelevelsofaflatoxinsincertainfoodstuffs
1.Introduction
1.1.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 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 proce-
dure. 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.Treatmentofthesampleasreceived inthelaboratory
Finely grind and mix thoroughly each laboratory sample using a process
that has been demonstrated to achieve complete homogenisation.
3.Subdivisionofsamplesforenforcementanddefencepurposes
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.Methodofanalysistobeusedbythelaboratoryandlaboratorycontrol
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
sr= Standard deviation, calculated from results generated under
repeatability conditions1998L0053 — EN — 06.08.1998 — 000.001 — 9
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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 condi-
tions (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 [(SR/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 Council
Directive 85/591/EEC.
4.3.Specific requirements
Where no specific methods for the determination of aflatoxin levels in
foodstuffs are prescribed at Community level, laboratories may select any
method provided the selected method meets the following criteria:
Criterion Concentration range Recommended valueMaximum permitted
value
Blanks All Negligible
Recovery — Afla-
toxin M1►M10,01-0,05 µg/kg◄ 60 to 120 %
>0,05►M1µg/kg◄ 70 to 110 %
Recovery — Afla-
toxins B1,B2,G1,G2< 1,0►M1µg/kg◄ 50 to 120 %
1-10►M1µg/kg◄ 70 to 110 %
>10►M1µg/kg◄ 80 to 110 %
Precision RSDRAll As derived from
Horwitz equation2 × value derived
from Horwitz equa-
tion
Precision RSDrmay be calculated as 0,66 times precision RSDRat the concentration of interest.
Notes:
— Values to apply to bothB1and sum of B1+B2+G1+G2,
— if sum of individual aflatoxins B1+B2+G1+G2are 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:
— RSDRis 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 inde-
pendant 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.1998L0053 — EN — 06.08.1998 — 000.001 — 10
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4.5.Laboratory quality standards
Laboratories must comply withCouncil Directive 93/99/EEC.1998L0053 — EN — 06.08.1998 — 000.001 — 11