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20.8.2011 Official
Journal
of
the
European
Union L
215/9
COMMISSION REGULATION (EU) No 836/2011
of 19 August 2011
amending Regulation (EC) No 333/2007 laying down the methods of sampling and analysis for the
official control of the levels of lead, cadmium, mercury, inorganic tin, 3-MCPD and benzo(a)pyrene
in foodstuffs
(Text with EEA relevance)
THE EUROPEAN COMMISSION,
(5) The
European
Union
Reference
Laboratory
for
Polycyclic
Aromatic Hydrocarbons (EU-RL PAH) in collaboration
with the national reference laboratories carried out a
Having regard to the Treaty on the Functioning of the European
survey among official control laboratories to assess
Union,
which analytical performance criteria would be
achievable for benzo(a)pyrene, benz(a)anthracene,
benzo(b)fluoranthene and chrysene in relevant food
matrices. The outcome of this survey was summarised
Having regard to Regulation (EC) No 882/2004 of the European
by the EU-RL PAH in the Report on ‘Performance char
Parliament and of the Council of 29 April 2004 on official
acteristics of analysis methods for the determination of 4
controls performed to ensure the verification of compliance
polycyclic aromatic hydrocarbons in food’ ( 6 ). The results
with feed and food law, animal health and animal welfare
of the survey show that the analytical performance
rules ( 1 ), in particular Article 11(4) thereof,
criteria currently applicable to benzo(a)pyrene are also
suitable for the other three substances.
Whereas:
(6) Experience
acquired
while
implementing
Regulation
(EC)
No 333/2007 revealed that in some cases the current
(1) Commission
Regulation
(EC)
No
1881/2006 of
sampling provisions may be impracticable or may lead
19 December 2006 setting maximum levels for certain
to unacceptable economic damage to the sampled lot.
contaminants in foodstuffs ( 2 ) established, inter alia,
For such cases, departure from the sampling procedures
maximum levels for the contaminant benzo(a)pyrene.
should be allowed, provided that sampling remains
sufficiently representative of the sampled lot or sublot
and that the procedure used is fully documented. For
(2) The
Scientific
Panel
on
Contaminants
in
the
Food
Chain
sampling at the retail stage, flexibility to depart from
of the European Food Safety Authority (EFSA) adopted
the sampling procedures existed already. The provisions
an opinion on Polycyclic Aromatic Hydrocarbons in
for sampling at retail stage should be aligned with the
Food on 9 June 2008 ( 3 ). The EFSA concluded that
general sampling procedures.
benzo(a)pyrene is not a suitable marker for the
occurrence of polycyclic aromatic hydrocarbons (PAH)
in food and that a system of four specific substances
or eight specific substances would be the most suitable
(7) More
detailed
provisions
are
needed
as
regards
the
markers of PAH in food. The EFSA also concluded that a
material of sampling containers when samples are
system of eight substances would not provide much
taken for PAH analysis. Plastic containers are widely
added value compared to a system of four substances.
used by enforcement authorities, but they are not
suitable when sampling is carried out for PAH analysis,
as the PAH content of the sample can be altered by these
materials.
(3) As
a
consequence
Commission
Regulation
(EU)
No
835/2011 ( 4 ) amended Regulation (EC) No 1881/2006
in order to set maximum levels for the sum of four
polycyclic aromatic hydrocarbons (benzo(a)pyrene,
(8) Clarification
is
needed
for
some
aspects
of
the
specific
benz(a)anthracene, benzo(b)fluoranthene and chrysene).
requirements for analytical methods, in particular the
requirements regarding the use of the performance
criteria and the ‘fitness-for-purpose’ approach.
(4) Commission
Regulation
(EC)
No
333/2007
(
Furthermore, the presentation of the tables with the

5 ) lays down
analytical performance criteria only for benzo(a)pyrene. It
performance criteria should be modified to appear
is therefore necessary to lay down analytical performance
more uniform across all analytes.
criteria for the other three substances for which
maximum levels are now set out in Regulation (EC) No
1881/2006.
(9) Regulation
(EC)
No
333/2007
should
therefore
be
amended accordingly. Since Regulation (EU) No
( 1 ) OJ L 165, 30.4.2004, p. 1.
835/2011 and this Regulation are inter-linked, both
( 2 ) OJ L 364, 20.12.2006, p. 5.
Regulations should become applicable on the same date.
( 3 ) The EFSA Journal (2008) 724, p. 1.
( 4 ) See page 4 of this Official Journal.
( 5 ) OJ L 88, 29.3.2007, p. 29.
( 6 ) JRC Report 59046, 2010.

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L 215/10
EN
Official Journal of the European Union
20.8.2011
(10) The
measures
provided
for
in
this
Regulation
are
in
‘1. Sampling
and
analysis
for
the
official
control
of
the
accordance with the opinion of the Standing
levels of lead, cadmium, mercury, inorganic tin, 3-MCPD
Committee on the Food Chain and Animal Health and
and polycyclic aromatic hydrocarbons (“PAH”) listed in
neither the European Parliament nor the Council have
Sections 3, 4 and 6 of the Annex to Regulation (EC) No
opposed them,
1881/2006 shall be carried out in accordance with the
Annex to this Regulation.’;
HAS ADOPTED THIS REGULATION:
Article 1
(3) the Annex is amended in accordance with the Annex to this
Regulation (EC) No 333/2007 is amended as follows:
Regulation.
(1) the title is replaced by the following:
Article 2
‘Commission Regulation (EC) No 333/2007 of 28 March
2007 laying down the methods of sampling and
This Regulation shall enter into force on the 20th day following
analysis for the official control of the levels of lead,
its publication in the Official Journal of the European Union.
cadmium, mercury, inorganic tin, 3-MCPD and
polycyclic aromatic hydrocarbons in foodstuffs’;
(2) in Article 1, paragraph 1 is replaced by the following:
It shall apply from 1 September 2012.
This Regulation shall be binding in its entirety and directly applicable in all Member States.
Done at Brussels, 19 August 2011.
For the Commission
The President
José Manuel BARROSO

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EN
20.8.2011 Official
Journal
of
the
European
Union L
215/11
ANNEX
The Annex to Regulation (EC) No 333/2007 is amended as follows:
(1) in
point
B.1.7
‘Packaging
and
transmission
of
samples’,
the
following
second
paragraph
is
added:
‘In case of sampling for PAH analysis plastic containers shall be avoided if possible as they could alter the PAH
content of the sample. Inert, PAH-free glass containers, adequately protecting the sample from light, shall be used
wherever possible. Where this is practically impossible, at least direct contact of the sample with plastics shall be
avoided, e.g. in case of solid samples by wrapping the sample in aluminium foil before placing it in the sampling
container.’;
(2) points B.2 and B.3 are replaced by the following:
‘B.2. SAMPLING
PLANS
B.2.1. Division of lots into sublots
Large lots shall be divided into sublots on condition that the sublot may be separated physically. For products
traded in bulk consignments (e.g. cereals) Table 1 shall apply. For other products Table 2 shall apply. 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 %.
B.2.2. Number of incremental samples
The aggregate sample shall be at least 1 kg or 1 litre except where it is not possible, e.g. when the sample
consists of 1 package or unit.
The minimum number of incremental samples to be taken from the lot or sublot shall be as given in Table 3.
In the case of bulk liquid products the lot or sublot shall be thoroughly mixed in so far as possible and in so
far it does not affect the quality of the product, by either manual or mechanical means immediately prior to
sampling. In this case, a homogeneous distribution of contaminants is assumed within a given lot or sublot. It
is therefore sufficient to take three incremental samples from a lot or sublot to form the aggregate sample.
The incremental samples shall be of similar weight/volume. The weight/volume of an incremental sample
shall be at least 100 grams or 100 millilitres, resulting in an aggregate sample of at least about 1 kg or 1 litre.
Departure from this method shall be recorded in the record provided for under point B.1.8 of this Annex.
Table 1
Subdivision of lots into sublots for products traded in bulk consignments
Lot weight (ton) Weight
or
number
of
sublots
≥ 1 500 500
tonnes
> 300 and < 1 500 3
sublots
≥ 100 and ≤ 300 100
tonnes
< 100
—
Table 2
Subdivision of lots into sublots for other products
Lot weight (ton) Weight
or
number
of
sublots
≥ 15 15-30
tonnes
< 15
—
Table 3
Minimum number of incremental samples to be taken from the lot or sublot
Weight or volume of lot/sublot (in kg or litre) Minimum
number
of
incremental
samples
to
be
taken
< 50
3
≥ 50 and ≤ 500
5
> 500 10

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L 215/12
EN
Official Journal of the European Union
20.8.2011
If the lot or sublot consists of individual packages or units, then the number of packages or units which shall
be taken to form the aggregate sample is given in Table 4.
Table 4
Number of packages or units (incremental samples) which shall be taken to form the aggregate
sample if the lot or sublot consists of individual packages or units
Number of packages or units in the lot/sublot Number
of
packages
or
units
to
be
taken
≤ 25 at
least
1
package
or
unit
26-100 about
5
%,
at
least
2
packages
or
units
> 100 about
5
%,
at
maximum
10
packages
or
units
The maximum levels for inorganic tin apply to the contents of each can, but for practical reasons it is
necessary to use an aggregate sampling approach. If the result of the test for an aggregate sample of cans is
less than but close to the maximum level of inorganic tin and if it is suspected that individual cans might
exceed the maximum level, then it might be necessary to conduct further investigations.
Where it is not possible to carry out the method of sampling set out in this chapter because of the
unacceptable commercial consequences (e.g. because of packaging forms, damage to the lot, etc.) or where
it is practically impossible to apply the abovementioned method of sampling, an alternative method of
sampling may be applied provided that it is sufficiently representative for the sampled lot or sublot and is
fully documented.
B.2.3. Specific provisions for the sampling of large fish arriving in large lots
In case the lot or sublot to be sampled contains large fishes (individual fishes weighing more than about 1 kg)
and the lot or sublot weighs more than 500 kg, the incremental sample shall consist of the middle part of the
fish. Each incremental sample shall weigh at least 100 g.
B.3. SAMPLING
AT
RETAIL
STAGE
Sampling of foodstuffs at retail stage shall be done where possible in accordance with the sampling
provisions set out in point B.2.2 of this Annex.
Where it is not possible to carry out the method of sampling set out in point B.2.2 because of the unac
ceptable commercial consequences (e.g. because of packaging forms, damage to the lot, etc.) or where it is
practically impossible to apply the abovementioned method of sampling, an alternative method of sampling
may be applied provided that it is sufficiently representative for the sampled lot or sublot and is fully
documented.’;
(3) in
the
first
paragraph
of
point
C.1
‘Laboratory
Quality
Standards’,
footnote
1
is
deleted;
(4) in
point
C.2.2.1
‘Specific
procedures
for
lead,
cadmium,
mercury
and
inorganic
tin’,
the
second
paragraph
is
replaced
by the following:
‘There are many satisfactory specific sample preparation procedures which may be used for the products under
consideration. For those aspects not specifically covered by this Regulation, the CEN Standard “Foodstuffs - Deter
mination of trace elements – Performance criteria, general considerations and sample preparation”( 1 ) has been found
to be satisfactory but other sample preparation methods may be equally valid.’;
(5) point
C.2.2.2
is
replaced
by
the
following:
‘C.2.2.2. S p e c i f i c p r o c e d u r e s f o r p o l y c y c l i c a r o m a t i c h y d r o c a r b o n s
The analyst shall ensure that samples do not become contaminated during sample preparation. Containers
shall be rinsed with high purity acetone or hexane before use to minimise the risk of contamination.
Wherever possible, apparatus and equipment coming into contact with the sample shall be made of inert
materials such as aluminium, glass or polished stainless steel. Plastics such as polypropylene or PTFE shall
be avoided because the analytes can adsorb onto these materials.’;

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EN
20.8.2011 Official
Journal
of
the
European
Union L
215/13
(6) point
C.3.1
‘Definitions’
is
amended
as
follows:
(a) the definition for ‘HORRAT r ’ is replaced by the following:
‘HORRAT (*) r = The observed RSD r divided by the RSD r value estimated from the (modified) Horwitz
equation (**) (cf. point C.3.3.1 (“Notes to the performance criteria”)) using the assumption
r = 0,66 R.
___________
(*) Horwitz W. and Albert, R., 2006, The Horwitz Ratio (HorRat): A useful Index of Method Performance with
respect to Precision, Journal of AOAC International, Vol. 89, 1095-1109.
(**) M. Thompson, Analyst, 2000, p. 125 and 385-386.’
(b) the definition for ‘HORRAT R ’ is replaced by the following:
‘HORRAT (*) R = The observed RSD R divided by the RSD R value estimated from the (modified) Horwitz
equation (**) (cf. point C.3.3.1 (“Notes to the performance criteria”)).
___________
(*) Horwitz W. and Albert, R., 2006, The Horwitz Ratio (HorRat): A useful Index of Method Performance with
respect to Precision, Journal of AOAC International, Vol. 89, 1095-1109.
(**) M. Thompson, Analyst, 2000, p. 125 and 385-386.’
(c) the definition for ‘u’ is replaced by the following:
‘u = Combined standard measurement uncertainty obtained using the individual standard measurement uncer
tainties associated with the input quantities in a measurement model (*)
___________
(*) International vocabulary of metrology – Basic and general concepts and associated terms (VIM), JCGM
200:2008.’;
(7) point
C.3.2
is
replaced
by
the
following:
‘C.3.2 General requirements
Methods of analysis used for food control purposes shall comply with the provisions of Annex III to
Regulation (EC) No 882/2004.
Methods for analysis for total tin are appropriate for official control on inorganic tin levels.
For the analysis of lead in wine, the methods and rules established by the OIV (*) apply in accordance with
Article 31 of Council Regulation (EC) No 479/2008 (**).
___________
(*) Organisation internationale de la vigne et du vin.
(**) Council Regulation (EC) No 479/2008 of 29 April 2008 on the common organisation of the market in
wine amending Regulations (EC) No 1493/1999, (EC) No 1782/2003, (EC) No 1290/2005, (EC) No
3/2008 and repealing Regulations (EEC) No 2392/86 and (EC) No 1493/1999 (OJ L 148, 6.6.2008,
p. 1).’;
(8) point
C.3.3.1
is
replaced
by
the
following:
‘C.3.3.1. P e r f o r m a n c e c r i t e r i a
Where no specific methods for the determination of contaminants in foodstuffs are prescribed at European
Union level, laboratories may select any validated method of analysis for the respective matrix provided
that the selected method meets the specific performance criteria set out in Tables 5, 6 and 7.
It is recommended that fully validated methods (i.e. methods validated by collaborative trial for the
respective matrix) are used where appropriate and available. Other suitable validated methods (e.g. in-
house validated methods for the respective matrix) may also be used provided that they fulfil the
performance criteria set out in Tables 5, 6 and 7.
Where possible, the validation of in-house validated methods shall include a certified reference material.

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L 215/14
EN
Official Journal of the European Union
20.8.2011
(a) Performance criteria for methods of analysis for lead, cadmium, mercury and inorganic tin:
Table 5
Parameter Criterion
Applicability Foods
specified
in
Regulation
(EC)
No
1881/2006
Specificity Free
from
matrix
or
spectral
interferences
Repeatability (RSD r ) HORRAT r less than 2
Reproducibility (RSD R ) HORRAT R less than 2
Recovery The
provisions
of
point
D.1.2
apply
Inorganic tin Lead,
cadmium,
mercury
ML is < 0,100 mg/kg ML
is
≥ 0,100 mg/kg
LOD
≤ 5 mg/kg
≤ one fifth of the ML
≤ one tenth of the ML
LOQ
≤ 10 mg/kg
≤ two fifths of the ML
≤ one fifth of the ML
(b) Performance criteria for methods of analysis for 3-MCPD:
Table 6
Parameter Criterion
Applicability Foods
specified
in
Regulation
(EC)
No
1881/2006
Specificity Free
from
matrix
or
spectral
interferences
Field blanks Less
than
LOD
Repeatability (RSD r ) 0,66
times
RSD R as derived from (modified) Horwitz equation
Reproducibility (RSD R ) as
derived
from
(modified)
Horwitz
equation
Recovery 75-110
%
LOD
≤ 5 μg/kg (on dry matter basis)
LOQ
≤ 10 μg/kg (on dry matter basis)
(c) Performance criteria for methods of analysis for polycyclic aromatic hydrocarbons:
The four polycyclic aromatic hydrocarbons to which these criteria apply are benzo(a)pyrene,
benz(a)anthracene, benzo(b)fluoranthene and chrysene.
Table 7
Parameter Criterion
Applicability Foods
specified
in
Regulation
(EC)
No
1881/2006
Specificity Free
from
matrix
or
spectral
interferences,
verification
of
positive
detection
Repeatability (RSD r ) HORRAT r less than 2
Reproducibility (RSD R ) HORRAT R less than 2

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EN
20.8.2011 Official
Journal
of
the
European
Union L
215/15
Parameter Criterion
Recovery 50-120
%
LOD
≤ 0,30 μg/kg for each of the four substances
LOQ
≤ 0,90 μg/kg for each of the four substances
(d) Notes to the performance criteria:
The Horwitz equation (*) (for concentrations 1,2 × 10 –7 ≤ C ≤ 0,138) and the modified Horwitz
equation (**) (for concentrations C < 1,2 × 10 –7 ) are generalised precision equations which are independent
of analyte and matrix but solely dependent on concentration for most routine methods of analysis.
Modified Horwitz equation for concentrations C < 1,2 × 10 –7 :
RSD R = 22 %
where:
— RSD R is the relative standard deviation calculated from results generated under reproducibility conditions
[(s R / ) × 100]
— C is the concentration ratio (i.e. 1 = 100 g/100 g, 0,001 = 1 000 mg/kg). The modified Horwitz equation
applies to concentrations C < 1,2 × 10 –7 .
Horwitz equation for concentrations 1,2 × 10 –7 ≤ C ≤ 0,138:
RSD R = 2C (–0,15)
where:
— RSD R is the relative standard deviation calculated from results generated under reproducibility conditions
[(s R / ) × 100]
— C is the concentration ratio (i.e. 1 = 100 g/100 g, 0,001 = 1 000 mg/kg). The Horwitz equation applies
to concentrations 1,2 × 10 –7 ≤ C ≤ 0,138.
___________
(*) W. Horwitz, L.R. Kamps, K.W. Boyer, J.Assoc.Off.Analy.Chem.,1980, 63, 1344.
(**) M. Thompson, Analyst, 2000, p. 125 and 385-386.’;
(9) point
C.3.3.2
is
replaced
by
the
following:
‘C.3.3.2. “Fitness-for-purpose” approach
For in-house validated methods, as an alternative a “fitness-for-purpose” approach (*) may be used to assess
their suitability for official control. Methods suitable for official control must produce results with a
combined standard measurement uncertainty (u) less than the maximum standard measurement uncer
tainty calculated using the formula below:

Uf
where:
q2
αC2
LOD=2

— Uf is the maximum standard measurement uncertainty (μg/kg).
— LOD is the limit of detection of the method (μg/kg). The LOD must meet the performance criteria set
in point C.3.3.1 for the concentration of interest.
— C is the concentration of interest (μg/kg);
— α is a numeric factor to be used depending on the value of C. The values to be used are given in
Table 8.
Table 8
Numeric values to be used for α as constant in formula set out in this point, depending on the
concentration of interest
C (μg/kg)
α
≤ 50 0,2
51-500 0,18

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L 215/16
EN
Official Journal of the European Union
20.8.2011
C (μg/kg)
α
501-1 000 0,15
1 001-10 000 0,12
> 10 000 0,1
The analyst shall note the “Report on the relationship between analytical results, measurement uncertainty,
recovery factors and the provisions of EU food and feed legislation” (**).
___________
(*) M. Thompson and R. Wood, Accred. Qual. Assur., 2006, p. 10 and 471-478.
(**) http://ec.europa.eu/food/food/chemicalsafety/contaminants/report-sampling_analysis_2004_en.pdf’;
(10) in point D.1.2 ‘Recovery calculations’, the second paragraph is replaced by the following:
‘In case no extraction step is applied in the analytical method (e.g. in case of metals), the result may be reported
uncorrected for recovery if evidence is provided by ideally making use of suitable certified reference material that the
certified concentration allowing for the measurement uncertainty is achieved (i.e. high accuracy of the measurement),
and thus that the method is not biased. In case the result is reported uncorrected for recovery this shall be
mentioned.’;
(11) in point D.1.3 ‘Measurement uncertainty’, the second paragraph is replaced by the following:
‘The analyst shall note the “Report on the relationship between analytical results, measurement uncertainty, recovery
factors and the provisions of EU food and feed legislation” (*).
___________
(*) http://ec.europa.eu/food/food/chemicalsafety/contaminants/report-sampling_analysis_2004_en.pdf’.

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