Commission Regulation (EC) No 627/2006 of  21 April 2006  implementing Regulation (EC) No 2065/2003 of the European Parliament and of the Council as regards quality criteria for validated analytical methods for sampling, identification and characterisation of primary smoke products
Date: 2006-04-21
Institutions: European Commission
Subjects: evaluation method, flavouring, foodstuff, foodstuffs legislation, health risk, qualitative analysis, smoked product

22.4.2006

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Official Journal of the European Union

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COMMISSION REGULATION (EC) No 627/2006

of 21 April 2006

implementing Regulation (EC) No 2065/2003 of the European Parliament and of the Council as
identification and
regards quality criteria

sampling,

for validated analytical methods
characterisation of primary smoke products

for

THE COMMISSION OF THE EUROPEAN COMMUNITIES,

contain a proposed validated method for sampling, iden-
tification and characterisation of the primary product.

Having regard to the Treaty
Community,

establishing the European

Having regard to Regulation (EC) No 2065/2003 of
the
European Parliament and the Council of 10 November 2003
on smoke flavourings used or intended for use in or on
foods (1) and in particular Article 17(3) thereof,

Whereas:

(1)

(2)

(3)

(4)

(5)

Regulation (EC) No 2065/2003 lays down provisions for
the establishment of a list of primary products authorised
for use as such in or on foods and for the production of
smoke flavourings for use in or on foods within the
Community. This list shall, among other things, contain
a clear description and characterisation of each primary
product.

Detailed information about the qualitative and quanti-
tative chemical composition of the primary product is
the scientific evaluation. The portions
necessary for
which have not been identified,
the amount of
structure is not known,
substances whose chemical
should be as small as possible.

i.e.

is

therefore

necessary

to
in this context

establish minimum
It
performance criteria,
referred to as
quality criteria, to which the method of analysis shall
comply
laboratories use
methods with the necessary level of performance.

to ensure

in order

that

Smoked foods in general give rise to health concerns,
especially with respect to the possible presence of poly-
cyclic aromatic hydrocarbons (PAHs).

The person who intends to place primary products on
the market should submit all the information necessary
information should
for

the safety assessment. This

(1) OJ L 309, 26.11.2003, p. 1.

(6)

(7)

(8)

(9)

Regulation (EC) No 882/2004 of
European
Parliament and the Council of 29 April 2004 on
official controls performed to ensure the verification of
compliance with feed and food law, animal health and
animal welfare rules (2), lays down general requirements
for methods of sampling and analysis.

the

The Scientific Committee on Food (SCF) named 15 PAHs
as potentially genotoxic and carcinogenic to humans in
an opinion on the risks to human health of PAH in food,
expressed on 4 December 2002 (3). They represent a
priority group in the assessment of the risk of long-
term adverse health effects following dietary intake of
PAHs. Their presence in primary products should — as
a consequence — be analysed.

the

chemical

the Commission Directorate General

The Institute for Reference Materials and Measurements
(IRMM) of
Joint
Research Centre carried out collaborative studies for
analysing
primary
products and for quantifying the concentration of the
15 PAHs therein. The results of these trials are in part
published in the Report on the Collaborative Trial for
Validation of two Methods for the Quantification of Poly-
Smoke
cyclic Aromatic Hydrocarbons
Condensates (4).

composition

in Primary

of

To describe the precision of the method the repeatability
standard deviation as defined in ISO 5725-1 (5)
is
It should be estimated using data from a
required.
Si
single-laboratory
as
described in the Harmonized Guidelines
for Single-
Laboratory Validation of Methods of Analysis (6) or a
collaborative trial giving Sr and SR as described in the
Protocol for the design, conduct and interpretation of
method-performance studies (7).

validation

exercise

giving

(2) OJ L 191, 28.5.2004, p. 1.
(3) SCF/CS/CNTM/PAH/29 Final, 4 December 2002.
(4) EU-Report LA-NA-21679-EN-C, ISBN 92-894-9629-0.
(5) ISO5725-1: Accuracy (trueness and precision) of measurement methods
and results — Part 1: General principles and definitions. 1994: Geneva.
(6) Thompson, M., S.L.R. Ellison, and R. Wood, Harmonized Guidelines for
Single-Laboratory Validation of Methods of Analysis. Pure and Applied
Chemistry, 2002. 74(5): pp. 835-855.
the design,

conduct and interpretation of
studies. Pure and Applied Chemistry, 1995.

(7) Horwitz, W., Protocol
method-performance
67(2): pp. 331-343.

for

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(10) A full validation of methods to analyse the composition
of primary products, with a maximum of compounds
is not achievable. The high number of
identified,
rise to incalculable amount of work
analytes gives
If however mass spectrometry is
which is impractical.
used for
the resulting
mass spectra can be compared to published data (1) or
to mass spectral libraries and a tentative identification of
the compounds can be achieved.

the detection of compounds,

criteria for validated methods for identification and char-
acterisation of primary smoke products laid down in this
regulation.

(14)

The quality criteria can be adapted, to take into account
advances in scientific and technological knowledge.

(15)

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

opinion

the

the

of

(11)

Based on the results obtained in the inter-laboratory vali-
dation study on PAHs and following Commission
Decision 2002/657/EC (2), minimum quality criteria for
any suitable analytical method for determination of PAHs
in all primary products have been proposed.

HAS ADOPTED THIS REGULATION:

Article 1

(12)

Following the recommendation given in the ISO, IUPAC,
and AOAC International Harmonized Guidelines for the
Use of Recovery Information in Analytical Measurement,
the analytical results should be corrected for recovery.

for validated analytical methods

The quality criteria
for
sampling, identification and characterisation of primary smoke
products, as referred to in point 4 of Annex II to Regulation
(EC) No 2065/2003, shall be as set out in the Annex to this
Regulation.

Article 2

(13)

The European Food Safety Authority has given scientific
and technical assistance for the elaboration of the quality

This Regulation shall enter into force on the twentieth day
following that of its publication in the Official
Journal of the
European Union.

This Regulation shall be binding in its entirety and directly applicable in all Member States.

Done at Brussels, 21 April 2006.

For the Commission

Markos KYPRIANOU
Member of the Commission

(1) http://www.irmm.jrc.be/html/activities/intense_sweeteners_and_

smoke_flavourings/liquid_smoke_components.xls
Faix, O., et al., Holz als Roh- & Werkstoff, 1991. 49: pp. 213-219.
Faix, O., et al., Holz als Roh- & Werkstoff, 1991. 49: pp. 299-304.
Faix, O., D. Meier, and I. Fortmann, Holz als Roh- & Werkstoff,
1990. 48: pp. 281-285.
Faix, O., D. Meier, and I. Fortmann, Holz als Roh- & Werkstoff,
1990. 48: pp. 351-354.

(2) OJ L 221, 17.8.2002, p. 8. Decision as last amended by Decision

2004/25/EC (OJ L 6, 10.1.2004, p. 38).

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ANNEX

Quality criteria for validated analytical methods for sampling, identification and characterisation of primary
smoke products

1. Sampling

The basic requirement is to obtain a representative and homogeneous laboratory sample.

The analyst shall ensure that samples do not become contaminated during sample preparation. Containers have to be
rinsed with high purity acetone or hexane (p.A., HLPC grade or equivalent) before use to minimise the risk of contam-
ination. Wherever possible, apparatus coming into contact with the sample shall be made of inert materials e.g. glass or
polished stainless steel. Plastics such as polypropylene are to be avoided, because the analyte can adsorb onto these
materials.

All of the sample material received by the laboratory is to be used for the preparation of test material. Only very finely
homogenised samples give reproducible results.

There are many satisfactory specific sample preparation procedures which may be used.

2. Identification and characterisation

2.1. Definitions

For the purpose of this Annex the following definitions shall apply:

Solvent free mass:

The mass of the material after abstraction of the solvent, which normally is water.

Volatile fraction:

The part of the solvent free mass, which is volatile and analysable by gas chromatography.

Identification
of a primary product:

Characterisation
of a primary product:

Results of a descriptive analysis, which identifies substances present in the primary product.

Identification of the major physical-chemical fractions and quantification and identification of
the chemical constituents.

LOQ: Limit of Quantification

LOD: Limit of Detection

Si:

Sr:

SR:

The single-laboratory standard deviation, calculated from results generated under repeatability conditions as
defined in ISO standard 5725-1 (1) (= repeatability standard deviation estimated in a single laboratory approach
according to the Harmonized Guidelines for Single-Laboratory Validation of Methods of Analysis (2)).

The average within laboratory standard deviation, calculated from results generated under repeatability conditions
as defined in ISO standard 5725-1 (1) in a collaborative trial with a minimum of eight laboratories conducted
according to the Protocol for the Design, Conduct and Interpretation of Method-Performance Studies (3).

The between laboratory standard deviation, calculated from results under reproducibility conditions as defined in
ISO standard 5725-1 (1) and according to the Protocol for the Design, Conduct and Interpretation of Method-
Performance Studies (3).

RSDi: Relative single-laboratory repeatability standard deviation (Si expressed in percent of the measured value),

RSDr: Relative average repeatability standard deviation (Sr expressed in percent of the measured value),

RSDR: Relative reproducibility standard deviation (SR expressed in percent of the measured value).

(1) ISO 5725-1: Accuracy (trueness and precision) of measurement methods and results — Part 1: General principles and definitions. Geneva, 1994.
(2) Thompson, M., S.L.R. Ellison, and R. Wood, Harmonized Guidelines for Single-Laboratory Validation of Methods of Analysis. Pure and

Applied Chemistry, 2002. 74(5): pp. 835-855.

(3) Horwitz, W., Protocol for the design, conduct and interpretation of method-performance studies. Pure and Applied Chemistry, 1995. 67(2):

pp. 331-343.

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2.2. Requirements

Without prejudice to Article 11 of Regulation (EC) No 882/2004, the validated method for identification and character-
isation to be selected by the laboratory shall comply with the quality criteria indicated in Tables 1 and 2.

Quality criteria for methods for identification and quantification of chemical constituents in the solvent free
mass and the volatile fraction of primary products

Table 1

Parameter

Value/Comment

Solvent free mass

Volatile fraction

At least 50 % by mass shall be identified and quantified

At least 80 % by mass shall be identified and quantified

Minimum method quality criteria for analysing Polycyclic Aromatic Hydrocarbons (PAHs)

Table 2

Analyte(s) PAH

RSDi (*)

RSDr (*)

RSDR (*)

LOD (***)

LOQ (***)

Analytical
range (***)

Recovery (*)

%

20

20

35

%

20

20

35

%

40

40

70

μg/kg

μg/kg

μg/kg

%

1,5

3,0

5,0

5,0

10

15

5,0-15

75-110

10-30

15-45

75-110

50-110

25

25

50

5,0

15

10-30

60-110

benzo[a]pyrene

benzo[a]anthracene

cyclopenta[cd]pyrene (**)
dibenzo[a,e]pyrene (**)
dibenzo[a,i]pyrene (**)
dibenzo[a,h]pyrene (**)

chrysene
5-methylchrysene
benzo[b]fluoranthene
benzo[j]fluoranthene
benzo[k]fluoranthene
indeno[123-cd]pyrene
dibenzo[a,h]anthracene
benzo[ghi]perylene
dibenzo[a,l]pyrene

(*) Over the whole analytical range.
(**) The RSDi, RSDr and RSDR values are relatively high due to the low stability of the analytes in primary smoke condensate.
(***) Corrected for recovery.