Foodstuffs Rules, 2005

VETERINARY SERVICES ACT

(CAP. 437)

Sampling Methods and the methods of analysis for the official

control of thelevels of lead, cadmium, mercury and 3-MCPD in

Foodstuffs Rules, 2005

IN exercise of the powers conferred under article 25 of the

Veterinary Services Act, the Minister for Rural Affairs and the

Environment, in agreement with the Minister of Health, the Elderly

and Community Care, has made the following rules>-

(1) The title of these rules is the Sampling Methods and the

methods of analysis for the official control of the levels of lead, cadmium,

mercury and 3-MCPD in Foodstuffs Rules, 2005.

(2) The scope of these rules is to implement the rules found

under European Union Council Directive 2001#22#EC on the sampling

methods and the methods of analysis for the official control of the levels

of lead, cadmium, mercury and 3-MCPD in foodstuffs.

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. GENERAL PROVISIONS

2.1. Personnel

Sampling shall be performed by an authorised qualified person as specified by Malta.

2.2. Material to be sampled

Each lot which is to be examined must be sampled separately.

2.3. 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.

2.4. 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 2.8.

2.5. 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.

2.6. 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 Veterinary Services’ regulations on sampling. The

size of the laboratory samples for enforcement shall be sufficient to allow at least for duplicate analyses.

2.7. 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.

2.8. 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

Veterinary Services’ 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.

3. 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.

3.1. 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 2.8.

Table 1: Minimum number of incremental samples to be taken from the lot

Weight of lot

Minimum number of incremental samples to be

(kg)

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 in the lot

Number of packages or units 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. 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.

For the purposes of these rules, and unless context otherwise

requires -

“aggregate sample” means the combined total of all the

incremental samples taken from the lot or sublot<

“the Commission” means the European Commission<

“the Community” means the European Community as

established under the Treaty establishing the European Community<

“the competent authority” means the Veterinary Services

within Malta as provided under article 2 of the Veterinary Services

Act<

“incremental sample” means a quantity of material taken from

a single place in the lot or sublot<

“laboratory sample” means the sample intended for the

laboratory<

“lot” means an identifiable quantity of food delivered at one

time and determined by the veterinary 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<

“Member State” means a State which is a Member within the

European Community<

“sublot” means a 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<

“third country” means a State which is not a Member within

the European Community<

“Veterinary Services” means the competent authority within

the territory of Malta as established under article 2 of the Veterinary

Services Act.

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 REQUIREMENTS

3.1. 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 × sr.

sr = standard deviation, calculated from results generated under repeatability conditions.

RSDr = 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.

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 × sR.

sR = standard deviation, calculated from results under reproducibility conditions.

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

0,1mg/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

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

collaborative trial

Recovery

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

Specificity

Free from matrix or spectral interferences

3.3.2. 3-MCPD analysis

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).

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

Criterion

Recommended value

Concentration

Field blanks

Less than the detection limit

—

Recovery

75-110 %

All

Limit of quantification

10 (or less) ìg/kg on a dry matter

—

basis

Standard deviation of the field

blank signal

Less than 4 ìg/kg

—

In-house precision estimates —

< 4 ìg/kg

20 ìg/kg

standard deviation of replicate

< 6 ìg/kg

30 ìg/kg

measurements at different

< 7 ìg/kg

40 ìg/kg

concentrations

< 8 ìg/kg

50 ìg/kg

< 15 ìg/kg

100 ìg/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.

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

Malta shall take all measures necessary to ensure that the Sampling for

official controls.

sampling for the official controls of the levels of lead, cadium, mercury

and 3-MCPD in foodstuffs is carried out in accordance with the methods

described in Schedule I to these rules.

Malta shall take all measures necessary to ensure that sample Sample preparation

and methods of

preparation and methods of analyses used for the official control of the analyses.

levels of lead, cadmium, mercury and 3- MCPD in foodstuffs comply

with the criteria described in Schedule II to these rules.

When Malta adopts these provisions, the provisions shall Reference of

procedure and

contain a reference to these rules or shall be accompanied by such applicability.

reference at the time of their official publication. The procedure for

such reference shall be that applicable in Malta.