Commission Regulation (EC) No 333/2007Show full title

ANNEX U.K.

PART A U.K. DEFINITIONS

For the purposes of this Annex, the following definitions shall apply:

‘lot’

:

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;

‘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; aggregate samples shall be considered as representative of the lots or sublots from which they are taken;

‘laboratory sample’

:

a sample intended for the laboratory.

PART B U.K. SAMPLING METHODS

B.1. GENERAL PROVISIONS U.K.

B.1.1. Personnel U.K.

Sampling shall be performed by an authorised person as designated by the Member State.

B.1.2. Material to be sampled U.K.

Each lot or sublot which is to be examined shall be sampled separately.

B.1.3. Precautions to be taken U.K.

In the course of sampling, precautions shall be taken to avoid any changes which would affect the levels of contaminants, adversely affect the analytical determination or make the aggregate samples unrepresentative.

B.1.4. Incremental samples U.K.

As far as possible, incremental samples shall be taken at various places distributed throughout the lot or sublot. Departure from such procedure shall be recorded in the record provided for under point B.1.8. of this Annex.

B.1.5. Preparation of the aggregate sample U.K.

The aggregate sample shall be made up by combining the incremental samples.

B.1.6. Samples for enforcement, defence and referee purposes U.K.

The samples for enforcement, defence and referee purposes shall be taken from the homogenised aggregate sample unless this conflicts with the rules of the Member States as regards the rights of the food business operator.

B.1.7. Packaging and transmission of samples U.K.

Each 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 any change in composition of the sample which might arise during transportation or storage.

[F1 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.]

Textual Amendments

F1 Inserted by 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).

B.1.8. Sealing and labelling of samples U.K.

Each sample taken for official use shall be sealed at the place of sampling and identified following the rules of the Member States.

A record shall be kept of each sampling, permitting each lot or sublot to be identified unambiguously (reference to the lot number shall be given) and giving the date and place of sampling together with any additional information likely to be of assistance to the analyst.

[F2 B.2. SAMPLING PLANS U.K.

B.2.1. Division of lots into sublots U.K.

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 U.K.

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

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 U.K.

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.

Textual Amendments

F2 Substituted by 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).

B.3. SAMPLING AT RETAIL STAGE U.K.

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 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.]

PART C U.K. SAMPLE PREPARATION AND ANALYSIS

C.1. LABORATORY QUALITY STANDARDS U.K.

Laboratories shall comply with the provisions of Article 12 of Regulation (EC) No 882/2004.

Laboratories shall participate in appropriate proficiency testing schemes which comply with the ‘International Harmonised Protocol for the Proficiency Testing of (Chemical) Analytical Laboratories’(1) developed under the auspices of IUPAC/ISO/AOAC.

Laboratories shall be able to demonstrate that they have internal quality control procedures in place. Examples of these are the ‘ISO/AOAC/IUPAC Guidelines on Internal Quality Control in Analytical Chemistry Laboratories’(2).

Wherever possible the trueness of analysis shall be estimated by including suitable certified reference materials in the analysis.

C.2. SAMPLE PREPARATION U.K.

C.2.1. Precautions and general considerations U.K.

The basic requirement is to obtain a representative and homogeneous laboratory sample without introducing secondary contamination.

All of the sample material received by the laboratory shall be used for the preparation of the laboratory sample.

Compliance with maximum levels laid down in Regulation (EC) No 1881/2006 shall be established on the basis of the levels determined in the laboratory samples.

C.2.2. Specific sample preparation procedures U.K.

C.2.2.1. Specific procedures for lead, cadmium, mercury and inorganic tin U.K.

The analyst shall ensure that samples do not become contaminated during sample preparation. Wherever possible, apparatus and equipment coming into contact with the sample shall not contain those metals to be determined and be made of inert materials e.g. plastics such as polypropylene, polytetrafluoroethylene (PTFE) etc. These should be acid cleaned to minimise the risk of contamination. High quality stainless steel may be used for cutting edges.

[F2 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 - Determination of trace elements – Performance criteria, general considerations and sample preparation’(3) has been found to be satisfactory but other sample preparation methods may be equally valid.]

In the case of inorganic tin, care shall be taken to ensure that all the material is taken into solution as losses are known to occur readily, particularly because of hydrolysis to insoluble hydrated Sn(IV) oxide species.

[F2 C.2.2.2. Specific procedures for polycyclic aromatic hydrocarbons U.K.

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.]

C.2.3. Treatment of the sample as received in the laboratory U.K.

The complete aggregate sample shall be finely ground (where relevant) and thoroughly mixed using a process that has been demonstrated to achieve complete homogenisation.

C.2.4. Samples for enforcement, defence and referee purposes U.K.

The samples for enforcement, defence and referee purposes shall be taken from the homogenised material unless this conflicts with the rules of the Member States on sampling as regards the rights of the food business operator.

C.3. METHODS OF ANALYSIS U.K.

C.3.1. Definitions U.K.

The following definitions shall apply:

‘r’

=

Repeatability the value below which the absolute difference between 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 × s_r.

‘s_r’

=

Standard deviation calculated from results generated under repeatability conditions.

‘RSD_r’

=

Relative standard deviation calculated from results generated under repeatability conditions [(s_r/) × 100].

‘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 × s_R.

‘s_R’

=

Standard deviation, calculated from results under reproducibility conditions.

‘RSD_R’

=

Relative standard deviation calculated from results generated under reproducibility conditions [(s_R/) × 100].

‘LOD’

=

Limit of detection, smallest measured content, from which it is possible to deduce the presence of the analyte with reasonable statistical certainty. The limit of detection is numerically equal to three times the standard deviation of the mean of blank determinations (n > 20).

‘LOQ’

=

Limit of quantification, lowest content of the analyte which can be measured with reasonable statistical certainty. If both accuracy and precision are constant over a concentration range around the limit of detection, then the limit of quantification is numerically equal to six or 10 times the standard deviation of the mean of blank determinations (n > 20).

‘’[F2 HORRAT (4) _r

=

The observed RSD _r divided by the RSD _r value estimated from the (modified) Horwitz equation (5) (cf. point C.3.3.1 (‘Notes to the performance criteria’)) using the assumption r = 0,66 R.]

‘[F2 HORRAT (6) _R ’

=

The observed RSD _R divided by the RSD _R value estimated from the (modified) Horwitz equation (7) (cf. point C.3.3.1 (‘Notes to the performance criteria’)).]

‘[F2 u’

=

Combined standard measurement uncertainty obtained using the individual standard measurement uncertainties associated with the input quantities in a measurement model] (8)

‘U’

=

The expanded measurement uncertainty, using a coverage factor of 2 which gives a level of confidence of approximately 95 % (U = 2u).

‘Uf’

=

Maximum standard measurement uncertainty.

[F2 C.3.2. General requirements U.K.

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 (9) apply in accordance with Article 31 of Council Regulation (EC) No 479/2008 (10) .]

C.3.3. Specific requirements U.K.

[F2 C.3.3.1. Performance criteria U.K.

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.

(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
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 (11) (for concentrations 1,2 × 10 ^–7 ≤ C ≤ 0,138) and the modified Horwitz equation (12) (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.]

[F2 C.3.3.2. ‘Fitness-for-purpose’ approach U.K.

For in-house validated methods, as an alternative a ‘fitness-for-purpose’ approach (13) 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 uncertainty calculated using the formula below:

where:

• 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
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’(14) .]

PART D U.K. REPORTING AND INTERPRETATION OF RESULTS

D.1. REPORTING U.K.

D.1.1. Expression of results U.K.

The results shall be expressed in the same units and with the same number of significant figures as the maximum levels laid down in Regulation (EC) No 1881/2006.

D.1.2. Recovery calculations U.K.

If an extraction step is applied in the analytical method, the analytical result shall be corrected for recovery. In this case the level of recovery must be reported.

[F2 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.]

D.1.3. Measurement uncertainty U.K.

The analytical result shall be reported as x +/– U whereby x is the analytical result and U is the expanded measurement uncertainty, using a coverage factor of 2 which gives a level of confidence of approximately 95 % (U = 2u).

[F2 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’(15) .]

D.2. INTERPRETATION OF RESULTS U.K.

D.2.1. Acceptance of a lot/sublot U.K.

The lot or sublot is accepted if the analytical result of the laboratory sample does not exceed the respective maximum level as laid down in Regulation (EC) No 1881/2006 taking into account the expanded measurement uncertainty and correction of the result for recovery if an extraction step has been applied in the analytical method used.

D.2.2. Rejection of a lot/sublot U.K.

The lot or sublot is rejected if the analytical result of the laboratory sample exceeds beyond reasonable doubt the respective maximum level as laid down in Regulation (EC) No 1881/2006 taking into account the expanded measurement uncertainty and correction of the result for recovery if an extraction step has been applied in the analytical method used.

D.2.3. Applicability U.K.

The present interpretation rules shall apply for the analytical result obtained on the sample for enforcement. In case of analysis for defence or reference purposes, the national rules shall apply.

(1)

‘The international harmonized protocol for the proficiency testing of analytical chemistry laboratories’ by M. Thompson, S.L.R. Ellison and R. Wood, Pure Appl. Chem., 2006, 78, 145-96.

(2)

Edited by M. Thompson and R. Wood, Pure Appl. Chem., 1995, 67, 649-666.

(3)

[F2 Standard EN 13804:2002, ‘Foodstuffs — Determination of trace elements — Performance criteria, general considerations and sample preparation’, CEN, Rue de Stassart 36, B-1050 Brussels .]

(4)

[F2 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.]

(5)

[F2 M. Thompson, Analyst, 2000, p. 125 and 385-386.]

(6)

[F2 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.]

(7)

[F2 M. Thompson, Analyst, 2000, p. 125 and 385-386.]

(8)

[F2 International vocabulary of metrology – Basic and general concepts and associated terms (VIM), JCGM 200:2008.]

(9)

[F2 Organisation internationale de la vigne et du vin.]

(10)

[F2 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 ).]

(11)

[F2 W. Horwitz, L.R. Kamps, K.W. Boyer, J.Assoc.Off.Analy.Chem.,1980, 63, 1344.]

(12)

[F2 M. Thompson, Analyst, 2000, p. 125 and 385-386.]

(13)

[F2 M. Thompson and R. Wood, Accred. Qual. Assur., 2006, p. 10 and 471-478.]

(14)

[F2 http://ec.europa.eu/food/food/chemicalsafety/contaminants/report-sampling_analysis_2004_en.pdf]

(15)

[F2 http://ec.europa.eu/food/food/chemicalsafety/contaminants/report-sampling_analysis_2004_en.pdf]

Textual Amendments

F2 Substituted by 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).