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.)
Date: 2001-03-08
Institutions: European Commission
Subjects: EU Member State, dangerous substance, food inspection, foodstuff, public health, research body

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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 Com-
munity,

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

Whereas:

(4)

(5)

(6)

Sampling plays a crucial role in obtaining representative
results for the determination of the levels of the contami-
nants which may be heterogeneously distributed in a lot.

Directive 85/591/EEC has fixed general criteria for
methods of sampling and analysis but in certain cases
more specific criteria become necessary in order to
ensure that
the control,
use methods of analysis with comparable levels of
performance.

in charge of

laboratories,

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.

(1)

(2)

(3)

Council Regulation (EEC) No 315/93 of 8 February
1993 laying down Community procedures for contami-
nants in food (2) provides that maximum levels must be
set for certain contaminants in foodstuffs in order to
protect public health.

(7)

The measures provided for in this Directive are in
accordance with the opinion of the Standing Committee
for Foodstuffs,

Commission Regulation (EC) No 466/2001 of 8 March
2001 setting maximum levels for certain contaminants
in foodstuffs (3) establishes, besides others, maximum
levels for lead, cadmium, mercury and 3-monochlorop-
ropane-1,2-diol (3-MCPD) in foodstuffs and makes refer-
ence to the measures laying down the sampling and
analysis methods to be used.

HAS ADOPTED THIS DIRECTIVE:

Article 1

Council Directive 89/397/EEC of 14 June 1989 on the
official control of foodstuffs (4) lays down the general
principles for the performance of control of 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.

The Member States shall take all measures necessary to ensure
that the sampling for the official control of the levels of lead,
cadmium, mercury and 3-MCPD in foodstuffs is carried out in
accordance with the methods described in Annex I to this
Directive.

Article 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 Official Journal.
(4) OJ L 186, 30.6.1989, p. 23.
(5) OJ L 290, 24.11.1993, p. 14.

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.

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Article 3

Article 4

The Member States shall, not later than 5 April 2003, bring
into force the laws, regulations or administrative provisions
necessary to comply with the provisions of this Directive. They
shall forthwith notify the Commission thereof.

When Member States adopt these provisions, the provisions
shall contain a reference to this Directive or shall be
accompanied by such reference at the time of their official
publication. The procedure for such reference shall be adopted
by Member States.

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.

Done at Brussels, 8 March 2001.

For the Commission

David BYRNE

Member of the Commission

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ANNEX I

METHODS OF SAMPLING FOR OFFICAL CONTROL OF THE LEVELS OF LEAD, CADMIUM, MERCURY
AND 3-MCPD IN CERTAIN FOODSTUFFS

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:

Sublot:

an identifiable quantity of food delivered at one time and determined by the
official to 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 be comparable.

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.

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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
the 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 incremental samples 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)

< 50

50 to 500

> 500

Minimum number of incremental samples to be taken

3

5

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.

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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

26 to 100

> 100

1 package or unit

About 5 %, at least 2 packages or units

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.

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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 FOODSTUFFS

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 general consideration’ 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 REQUIRE-

MENTS

3.1. Definitions

A number of the most commonly used definitions that the laboratory will be required to use are given below:

r =

sr =

RSDr =

R =

sR =

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.

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.

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.

standard deviation, calculated from results under reproducibility conditions.

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RSDR =

relative standard deviation calculated from results generated under reproducibility conditions
[(sR / x-) x 100]

HORRATr =

the observed RSDr divided by the RSDr value estimated from the Horwitz equation using the
assumption r = 0,66R

HORRATR =

the observed RSDR value divided by the RSDR value calculated from the Horwitz
equation (b).

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 trial test materials.

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 specification 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 specification for lead is less than 0,1
mg/kg. For the latter, no more than two fifths of the value of the specification

Precision

Recovery

Specificity

3.3.2. 3-MCPD analysis

HORRATr or HORRATR values of less than 1,5 in the validation collaborative
trial

80-120 % (as indicated in the collaborative trial)

Free from matrix or spectral interferences

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).

(1) OJ L 272, 3.10.1990, p. 1.

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Table 4: Performance criteria of methods for 3-MCPD analysis

Criterion

Recommended value

Concentration

Field blanks

Recovery

Less than the detection limit

75-110 %

Limit of quantification

10 (or less) (cid:236)g/kg on a dry matter basis

Standard deviation of the field blank signal

Less than 4 (cid:236)g/kg

In-house precision estimates — standard
deviation of replicate measurements at
different concentrations

< 4 (cid:236)g/kg
< 6 (cid:236)g/kg
< 7 (cid:236)g/kg
< 8 (cid:236)g/kg
< 15 (cid:236)g/kg

—

All

—

—

20 (cid:236)g/kg
30 (cid:236)g/kg
40 (cid:236)g/kg
50 (cid:236)g/kg
100 (cid:236)g/kg

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
General Considerations’, 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 Michael Thompson, Steven L R Ellison, Ales Fajgelj, Paul Willetts and Roger Wood, Pure Appl. Chem.,
1999, No 71, 337-348