2001L0022 — EN — 05.04.2001 — 000.001 — 1
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►B COMMISSION DIRECTIVE 2001/22/EC
of 8 March 2001
laying down the sampling methods and the methods of analysis for the official control of the levels
of lead, cadmium, mercury and 3-MCPD in foodstuffs
(Text with EEA relevance)
(OJ L 77, 16.3.2001, p. 14)
Amended by:
OfficialJournal
No page date
►M1 Commission Decision 2001/873/EC of 4 December 2001 L 325 34 8.12.2001
▼B
COMMISSION DIRECTIVE 2001/22/EC
of 8 March 2001
laying down the sampling methods and the methods of analysis for
the official control of the levels of lead, cadmium, mercury and 3-
MCPD in foodstuffs
(Text with EEA relevance)
THE COMMISSION OF THE EUROPEAN COMMUNITIES,
Having regard to the Treaty establishing the European Community,
Having regard to CouncilDirective 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:
(1) Council Regulation (EEC) No 315/93 of 8 February 1993 laying
down Community procedures for contaminants in food (2)
provides that maximum levels must be set for certain contami-nants in foodstuffs in order to protect public health.
(2) Commission Regulation (EC) No 466/2001 of 8 March 2001setting maximum levels for certain contaminants in foodstuffs (
3)
establishes, besides others, maximum levels for lead, cadmium,
mercury and 3-monochloropropane-1,2-diol (3-MCPD) in food-stuffs and makes reference to the measures laying down thesampling and analysis methods to be used.
(3) CouncilDirective 89/397/EEC of 14 June 1989 on the official
controlof foodstuffs (4) lays down the general principles for the
performance of controlof foodstuffs. CouncilDirective 93/99/EEC of 29 October 1993 on the subject of additionalmeasuresconcerning the officialcontrolof foodstuffs (
5) introduces a
system of quality standards for laboratories entrusted by theMember States with the officialcontrolof foodstuffs.
(4) Sampling plays a crucial role in obtaining representative resultsfor the determination of the levels of the contaminants which maybe heterogeneously distributed in a lot.
(5) Directive 85/591/EEC has fixed generalcriteria for methods ofsampling and analysis but in certain cases more specific criteria
become necessary in order to ensure that laboratories, in charge of
the control, use methods of analysis with comparable levels ofperformance.
(6) The provisions for the sampling and methods of analysis havebeen drawn up on the basis of present knowledge and they may beadapted to take account of advances in scientific and technolo-
gicalknowl edge.
(7) The measures provided for in this Directive are in accordance
with the opinion of the Standing Committee for 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 lead, cadmium, mercuryand 3-MCPD in foodstuffs is carried out in accordance with the methodsdescribed in Annex I to this Directive.2001L0022 — EN — 05.04.2001 — 000.001 — 2
(1) OJ L 372, 31.12.1985, p. 50.
(2) OJ L 37, 13.2.1993, p. 1.
(3) See page 1 of this OfficialJournal .
(4) OJ L 186, 30.6.1989, p. 23.
(5) OJ L 290, 24.11.1993, p. 14.
▼B
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 lead, cadmium, mercury and 3-MCPD in foodstuffs
comply with the criteria described in Annex II to this Directive.
Article 3
The Member States shall, not later than ►M15 April2002 ◄, bring
into force the laws, regulations or administrative provisions necessary tocomply with the provisions of this Directive. They shall forthwith notifythe 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 officialpubl ication. The procedure for such
reference shall be adopted by Member States.
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.2001L0022 — EN — 05.04.2001 — 000.001 — 3
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ANNEX I
METHODS OF SAMPLINGFOR OFFICALCONTROLOF THE LEVELS
OF LEAD, CADMIUM, MERCURY AND 3-MCPD IN CERTAIN FOOD-
STUFFS
1. PURPOSE AND SCOPE
Samples intended for the official control of the levels of lead, cadmium,
mercury and 3-MCPD contents in foodstuffs shall be taken according to the
methods described below. Aggregate samples thus obtained shall be
considered as representative of the lots or sublots from which they are
taken. Compliance with maximum levels 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: an identifiable quantity of food delivered at one
time and determined by the officialto have
common characteristics, such as origin, variety,
type of packing, packer, consignor or markings.
In the case of fish, also the size of fish shall becomparable.
Sublot: designated part of a large lot in order to apply
the sampling method on that designated part.
Each sublot must be physically separated 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
3. GENERAL PROVISIONS
3.1.Personnel
Sampling shall be performed by an authorised qualified person as specified
by the Member States.
3.2.Material to be sampled
Each lot which is to be examined must be sampled separately.
3.3.Precautions to be taken
In the course of sampling and preparation of laboratory samples precautions
must be taken to avoid any changes which would affect the lead, cadmium,
mercury and 3-MCPD contents, adversely affect the analytical determination
or make the aggregate samples unrepresentative.
3.4.Incremental samples
As far as possible incremental samples shall be taken at various places
distributed throughout the lot or sublot. Departure from this procedure must
be recorded in the record provided for under 3.8.
3.5.Preparation of the aggregate sample
The aggregate sample is made up by uniting all incremental samples. It shall
be at least 1 kg unless not practical, e.g. when a single package has been
sampled.
3.6.Subdivision of aggregate sample in laboratory samples for enforcement,
defence and referee purposes
The laboratory samples for enforcement, trade (defence) and referee
purposes shall be taken from the homogenised aggregate sample unless
this conflicts with Member States' regulations on sampling. The size of the2001L0022 — EN — 05.04.2001 — 000.001 — 4
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laboratory samples for enforcement shall be sufficient to allow at least for
duplicate analyses.
3.7.Packaging and transmission of aggregate and laboratory samples
Each aggregate and laboratory sample shall be placed in a clean, inert
container offering adequate protection from contamination, from loss of
analytes by adsorption to the internal wall of the container and against
damage in transit. All necessary precautions shall be taken to avoid change
of composition of the aggregate and laboratory samples which might arise
during transportation or storage.
3.8.Sealing and labelling of aggregate and laboratory samples
Each sample taken for official use shall be sealed at the place of sampling
and identified following the Member States' 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. SAMPLING PLANS
Sampling should ideally take place at the point where the commodity enters
the food chain and a discrete lot becomes identifiable. The sampling method
applied shall ensure that the aggregate sample is representative for the lot
that is to be controlled.
4.1.Number of incremental samples
In the case of liquid products for which a homogeneous distribution of the
contaminant in question can be assumed within a given lot, it is sufficient to
take one incremental sample per lot which forms the aggregate sample.
Reference to the lot number shall be given. Liquid products containing
hydrolysed vegetable protein (HVP) or liquid soya sauce shall be shaken
well, or homogenised by other suitable means, before the incremental
sample is taken.
For other products, the minimum number of incrementalsampl es to be taken
from the lot shall be as given in Table 1. The incremental samples shall be of
similar weight. Departure from this procedure must be recorded in the record
provided for under 3.8.
Table 1: Minimum number of incremental samples to be taken from the lot
Weight of lot
(kg)Minimum number of incremental
samples to be taken
<5 0 3
50 to 500 5
> 500 10
If the lot consists of individual packages, then the number of packages which
shall be taken to form the aggregate sample is given in Table 2.
Table 2: Number of packages (incremental samples) which shall be taken to
form the aggregate sample if the lot consists of individual packages
Number of packages or units in the lot Number of packages or units to be taken
1 to 25 1 package or unit
26 to 100 About 5 %, at least 2 packages or
units
> 100 About 5 %, at maximum 10
packages or units
5. COMPLIANCE OF THE LOT OR SUBLOT WITH THE SPECIFICATION
The control laboratory shall analyse the laboratory sample for enforcement
at least in two independent analyses, and calculate the mean of the results.
The lot is accepted if the mean conforms to the respective maximum level as
laid down in Regulation (EC) No 466/2001. It is rejected if the mean
exceeds the respective maximum level.2001L0022 — EN — 05.04.2001 — 000.001 — 5
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ANNEX II
SAMPLE PREPARATION AND CRITERIA FOR METHODS OF
ANALYSIS USED IN OFFICAL CONTROL OF THE LEVELS OF
LEAD, CADMIUM, MERCURY AND 3-MCPD IN CERTAIN FOOD-
STUFFS
1. INTRODUCTION
The basic requirement is to obtain a representative and homogeneous
laboratory sample without introducing secondary contamination.
2. SPECIFIC SAMPLE PREPARATION PROCEDURES FOR LEAD,
CADMIUM AND MERCURY
There are many satisfactory specific sample preparation procedures which
may be used for the products under consideration. Those described in the
draft CEN Standard ‘Foodstuffs — Determination of trace elements —
Performance criteria and generalconsideration’ have been found to be
satisfactory (a) but others may be equally valid.
The following points must be noted for any procedure used:
— bivalve molluscs, crustaceans and small fish: where these are normally
eaten whole, the viscera are to be included in the material to be
analysed,
— vegetables: only the edible portion of is to be tested, with note to be
taken of the requirements of the Regulation (EC) No 466/2001.
3. METHOD OF ANALYSIS TO BE USED BY THE LABORATORY AND
LABORATORY CONTROL REQUIREMENTS
3.1.Definitions
A number of the most commonly used definitions that the laboratory will
be required to use are given below:
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
intervalof time) may be expected to l ie within a specific
probability (typically 95 %) and hence r = 2,8 × sr.
sr= standard deviation, calculated from results generated
under repeatability conditions.
RSDr= relative standard deviation, calculated from results
generated under repeatability conditions
sr=/C22xx ðÞ /C2 100 ½/C138 , where /C22xxis 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
sR=/C22xx ðÞ /C2 100 ½/C138
HORRATr= the observed RSDrdivided by the RSDrvalue estimated
from the Horwitz equation using the assumption r
= 0,66R
HORRATR= the observed RSDRvalue divided by the RSDRvalue
calculated from the Horwitz equation (b).2001L0022 — EN — 05.04.2001 — 000.001 — 6
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3.2.General requirements
Methods of analysis used for food control purposes must comply whenever
possible with the provisions of paragraphs 1 and 2 of the Annex to
Directive 85/591/EEC.
For the analysis of lead in wine, Commission Regulation (EEC) No 2676/
90 (1) determining Community methods for the analysis of wines lays
down the method to be used in Chapter 35 of its Annex.
3.3.Specific requirements
3.3.1. Lead, cadmium and mercury analyses
Specific methods for the determination of lead, cadmium and mercury
contents are not prescribed. Laboratories shall use a validated method that
fulfils the performance criteria indicated in Table 3. Where possible, the
validation shall include a certified reference material in the collaborative
trialtest material s.
Table 3: Performance criteria of methods for lead, cadmium and mercury
analyses
Parameter Value/comment
Applicability Foods specified in Regulation (EC) No
466/2001
Detection limit No more than one tenth of the value of the
specification in Regulation (EC) No 466/
2001, except if the value of the specifica-
tion for lead is less than 0,1 mg/kg. For the
latter, no more than one fifth of the value
of the specification
Limit of quantification No more than one fifth of the value of the
specification in Regulation (EC) No 466/
2001, except if the value of the specifica-
tion for lead is less than 0,1 mg/kg. For the
latter, no more than two fifths of the value
of the specification
Precision HORRATror HORRATRvalues of less
than 1,5 in the validation collaborative trial
Recovery 80-120 % (as indicated in the collaborative
trial)
Specificity Free from matrix or spectralinterferences
3.3.2. 3-MCPD analysis
Specific methods for the determination of 3-MCPD contents are not
prescribed. Laboratories shall use a validated method that fulfils the
performance criteria indicated in Table 4. Where possible, the validation
shall include a certified reference material in the collaborative trial test
materials. A specific method has been validated by collaborative trial and
has been shown to meet the requirements of Table 4 (c).
Table 4: Performance criteria of methods for 3-MCPD analysis
Criterion Recommended value Concentration
Field blanks Less than the detection limit —
Recovery 75-110 % All
Limit of quantification 10 (or less) µg/kg on a dry matter
basis—
Standard deviation of the field
blank signalLess than 4 µg/kg —
In-house precision estimates —
standard deviation of replicate
measurements at different concen-
trations<4µg/kg 20 µg/kg
<6µg/kg 30 µg/kg
<7µg/kg 40 µg/kg
<8µg/kg 50 µg/kg
<1 5 µg/kg 100 µg/kg2001L0022 — EN — 05.04.2001 — 000.001 — 7
(1) OJ L 272, 3.10.1990, p. 1.
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3.4.Estimation of the analytical trueness and recovery calculations
Wherever possible the trueness of the analysis shall be estimated by
including suitable certified reference materials in the analytical run.
The ‘Harmonised Guidelines for the Use of Recovery Information in
Analytical Measurement’ (d) developed under the auspices of IUPAC/ISO/
AOAC shall be taken into account.
The analytical result shall be reported corrected or uncorrected. The
manner of reporting and the level of recovery must be reported.
3.5.Laboratory quality standards
Laboratories must comply with Directive 93/99/EEC.
3.6.Expression of results
The results shall be expressed in the same units as the maximum levels laid
down in Regulation (EC) No 466/2001.
REFERENCES
(a) Draft Standard prEN 13804, ‘Foodstuffs — Determination of Trace Elements
— Performance Criteria and GeneralConsiderations’, CEN, Rue de Stassart
36, B-1050 Brussels.
(b) W Horwitz, ‘Evaluation of Analytical Methods for Regulation of Foods and
Drugs’, Anal. Chem., 1982, No 54, 67A-76A
(c) Method of Analysis to determine 3-Monochloropropane-1,2-Diol in Food and
Food Ingredients using Mass Spectrometric Detection, submitted to CEN TC
275 and AOAC International (also available as ‘Report of the Scientific
Cooperation task 3.2.6: Provision of validated methods to support the
Scientific Committee on Food's recommendations regarding 3-MCPD in
hydrolysed protein and other foods’).
(d) ISO/AOAC/IUPAC Harmonised Guidelines for the Use of Recovery
Information in Analytical Measurement. Edited MichaelThompson, Steven
L R Ellison, Ales Fajgelj, Paul Willetts and Roger Wood, Pure Appl. Chem.,
1999, No 71, 337-3482001L0022 — EN — 05.04.2001 — 000.001 — 8