Contaminants in Food (Sampling and Analysis Methods)

L.N. 107 of 2006

FOOD SAFETY ACT

(CAP. 449)

Contaminants in Food (Sampling and Analysis Methods)

(Amendment) (No. 2) Regulations, 2006

IN exercise of the powers conferred by article 10 of the Food Safety

Act, the Minister of Health, the Elderly and Community Care has made

the following regulations>-

The title of these regulations is the Contaminants in Food Citation.

(Sampling and Analysis Methods) (Amendment) (No. 2) Regulations,

2006, and they shall be read and construed as one with the Contaminants

in Food (Sampling and Analysis Methods) Regulations, 2004, L.N. 488 of 2004.

hereinafter referred to as “the principal regulations”.

These regulations implement the provisions of Commission Scope.

Directive 2005#10#EC of 4 February, 2005.

For regulation 7 of the principal regulations there shall be Amends regulation

7 of the principal

substituted by the following>-

regulations.

“7.1. The sampling for the official control of the levels of

benzo(a)pyrene in foodstuffs shall be carried out in accordance

with the methods described in the Eleventh Schedule.

2. The sampling preparation and methods of analysis used

for the official control of the levels of benzo(a)pyrene in foodstuffs

shall comply with the criteria described in the Twelfth Schedule.”.

4. Immediately after the Tenth Schedule to the principal Adds Eleventh

Schedule to the

regulations there shall be added the following Eleventh Schedule>-

principal

regulations.

“ELEVENTH SCHEDULE

(Equivalent to Annex I of Commission Directive 2005#10#EC)

METHODS OF SAMPLING FOR OFFICIAL CONTROL OF

THE LEVELS OF BENZO(A)PYRENE IN FOODSTUFFS

1. Purpose and Scope

Samples intended for official checking of the levels of

benzo(a)pyrene in foodstuffs shall be taken according to the methods

described below. Aggregate samples thus obtained shall be considered

as representative of the lots. 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 a food commodity delivered at

one time and having been determined by the official to have common

characteristics, such as origin, variety, type of packing, packer, consignor

or markings.

‘Sublot’> designated part of a lot in order to apply the sampling

method on that designated part< each sublot must be physically separate

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 person as specified

by the Food Safety Commission.

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 the samples

precautions must be taken to avoid any changes, which would affect

the benzo(a)pyrene content, adversely affect the analytical determination

or make the aggregate samples unrepresentative.

3.4. Incremental samples

As far as possible incremental samples should be taken at various

places distributed throughout the lot or sublot. Departure from this

procedure must be recorded in the record.

3.5. Preparation of the aggregate sample

The aggregate sample is made up by uniting all incremental

samples. This aggregate sample is homogenised in the laboratory unless

this is incompatible with implementation of point 3.6.

3.6. Replicate laboratory samples

Replicate laboratory samples for enforcement, trade (defence) and

referee purposes shall be taken from the homogenized aggregate sample

unless this conflicts with national rules on sampling.

3.7. Packaging and transmission of samples

Each sample shall be placed in a clean, inert container offering

adequate protection from contamination 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.

3.8.

Sealing and labelling of samples

Each sample taken for official use shall be sealed at the place of

sampling and identified following the national rules.

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

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 oils, for which a homogeneous distribution of

benzo(a)pyrene can be assumed within a given lot, it is sufficient to

take three incremental samples per lot to form the aggregate sample.

Reference to the lot number shall be given. For olive oil and olive pomace

oil further information on sampling is given in Commission Regulation

(EC) No 1989#2003.

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, no less than 100g each, resulting in

an aggregate sample of no less than 300g (see point 3.5).

TABLE 1

Minimum number of incremental samples to be taken

from the lot

Weight of lot (in kg)

Minimum number of

incremental samples to be taken

‹ 50

50 to 500

› 500

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

Number of packages or units

in the lot or sublot

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

4.2.

Sampling at retail stage

Sampling of foodstuffs at the retail stage should be done where

possible in accordance with the above sampling provisions. Where this

is not possible, other effective sampling procedures at retail stage can

be used provided that they ensure sufficient representativeness for the

sampled lot.

5. Compliance of the lot or sublot with the specification

The control laboratory shall analyse the laboratory sample for

enforcement in duplicate analyses in cases where the obtained result of

the first analysis is less than 20 % below or above the maximum level,

and in these cases shall calculate the mean of the results.

The lot is accepted if the result of the first analysis or, where

duplicate analysis is necessary, if the mean does not exceed the respective

maximum level (as laid down in Regulation (EC) No 466#2001) taking

into account the measurement uncertainty and correction for recovery.

The lot is non-compliant with the maximum level (as laid down in

Regulation (EC) 466#2001) if the result of the first analysis or, where

duplicate analysis is necessary, if the mean exceeds the maximum level

beyond reasonable doubt taking into account the measurement

uncertainty and correction for recovery.”

5. Immediately after the new Eleventh Schedule to the principal Adds Twelfth

Schedule to the

regulations, there shall be added the following Twelfth Schedule>-

principal

regulations.

“TWELFTH SCHEDULE

(Equivalent to Annex II of Commission Directive 2005#10#EC)

SAMPLE PREPARATION AND CRITERIA FOR METHODS

OF ANALYSIS USED IN OFFICIAL CHECKING OF THE

LEVELS OF BENZO(A)PYRENE IN FOODSTUFFS

1. Precautions and general considerations for benzo(a)pyrene

in food samples

The basic requirement is to obtain a representative and

homogeneous laboratory sample without introducing secondary

contamination.

The analyst should ensure that samples do not become

contaminated during sample preparation. Containers should be rinsed

with high purity acetone or hexane (p.A., HLPC grade or equivalent)

before use to minimize the risk of contamination. Wherever possible,

apparatus coming into contact with the sample should be made of inert

materials e.g. aluminium, glass or polished stainless steel. Plastics such

as polypropylene, PTFE etc. should 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. Treatment of the sample as received in the laboratory

Finely grind (where relevant) and mix thoroughly the complete

aggregate sample using a process that has been demonstrated to achieve

complete homogenisation.

3. Subdivision of samples for enforcement and defence purposes

The replicate samples for enforcement, trade (defence) and referee

purposes shall be taken from the homogenized material unless this

conflicts with national rules on sampling.

4. Method of analysis to be used by the laboratory and laboratory

control requirements

4.1. 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 interval of time) may be expected to lie within a specific

probability (typically 95 %) and hence r = 2.8 x 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 # –x ) x 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 x 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 # –x ) x 100], where –x is

the average of results over all laboratories and samples.

HORRAT r = the observed RSD r divided by the RSD r value

estimated from the Horwitz equation (1) using the assumption r = 0.66R.

HORRAT R = the observed RSD R value divided by the RSD R value

calculated from the Horwitz equation.

U = the expanded uncertainty, using a coverage factor of 2 which

gives a level of confidence of approximately 95 %.

4.2.

General requirements

Methods of analysis used for food control purposes must comply

with points 1 and 2 of the Annex to Council Directive 85#591#EEC.

4.3.

Specific requirements

Where no specific methods for the determination of benzo(a)pyrene

in food are prescribed at Community level, laboratories may select any

validated method provided the selected method meets the performance

criteria indicated in the Table. The validation should ideally include a

certified reference material.

TABLE

Performance criteria for methods of analysis for benzo(a)pyrene

Parameter

Value#comment

Applicability

Food specified in Regulation

(EC) No 208#2005

Detection limit

Not more than 0,3 µg#kg

Limit of quantification

Not more than 0,9 µg#kg

Precision

HORRAT r or HORRAT R values

of less than 1.5 in the validation

collaborative trial

Recovery

50% – 120%

Specificity

Free from matrix or spectral

interferences, verification of

positive detection

4.3.1.

Performance Criteria — Uncertainty Function Approach

However, an uncertainty approach may also be used to assess the

suitability of the method of analysis to be used by the laboratory. The

laboratory may use a method which will produce results within a

maximum standard uncertainty. The maximum standard uncertainty can

be calculated using the following formula>

√ [(LOD/2) +(0.2C) ]

Uƒ =

Where>

Uf

is the maximum standard uncertainty

LOD

is the limit of detection of the method

C

is the concentration of interest

If an analytical method provides results with uncertainty

measurements less than the maximum standard uncertainty, the method

will be equally suitable to one which meets the performance

characteristics given in the Table.

4.4.

Recovery calculation and reporting of results

The analytical result is to be reported corrected or uncorrected for

recovery. The manner of reporting and the level of recovery must be

reported. The analytical result corrected for recovery is used for checking

compliance (see the Eleventh Schedule, point 5).

The analyst should note the ‘European Commission Report on the

relationship between analytical results, the measurement of uncertainty,

recovery factors and the provisions in EU food legislation’ (2).

The analytical result has to be reported as x +#– U whereby x is the

analytical result and U is the measurement uncertainty.

4.5.

Laboratory quality standards

Laboratories must comply with Directive 93#99#EEC.

4.6.

Other considerations for the analysis

Proficiency testing

Participation in appropriate proficiency testing schemes which

comply with the ‘International Harmonised Protocol for the Proficiency

Testing of (Chemical) Analytical Laboratories’ (3) developed under

the auspices of IUPAC# ISO#AOAC.

Internal quality control

Laboratories should 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’ (4).

REFERENCES

1. W. Horwitz, ‘Evaluation of Analytical Methods for

Regulation of Foods and Drugs’, Anal. Chem., 1982, 54, 67A-76A.

2. European Commission Report on the relationship between

analytical results, the measurement of uncertainty, recovery factors and

the provisions in EU food legislation, 2004.

3. ISO#AOAC#IUPAC International Harmonised Protocol for

Proficiency Testing of (Chemical) Analytical Laboratories, Edited by

M. Thompson and R. Wood, Pure Appl. Chem., 1993, 65, 2123-2144

(Also published in J. AOAC International, 1993, 76, 926).

4. ISO#AOAC#IUPAC International Harmonised Guidelines for

Internal Quality Control in Analytical Chemistry Laboratories, Edited

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

Mitbug[ fl-Istamperija tal-Gvern — Printed at the Government Printing Press