Foodstuffs Rules, 2005

L.N. 97 of 2005

VETERINARY SERVICES ACT

(CAP. 437)

Sampling Methods and Methods of Analysis for the Official

Control of the Levels for Certain Contaminants in

Foodstuffs Rules, 2005

IN exercise of the powers conferred by article 25 of the Veterinary

Services Act, the Minister for Rural Affairs and the Environment has

made the following rules>-

(1) The title to these rules is the Sampling Methods and Title and scope.

Methods of Analysis for the Official Control of the Levels for Certain

Contaminants in Foodstuffs Rules, 2005.

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

under European Union Council Directive 98#53#EC establishing methods

of analysis for the official control of feedingstuffs.

Definitions.

For the purposes of these rules -

Methods of sampling for official checking control of the levels of aflatoxins

in certain foodstuffs

1. Purpose and scope

Samples intended for official checking of the levels of aflatoxin content 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 limits laid down in European Commission

Regulation 98/1525/EC 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 determined by the official to have

common characteristics, such as origin, variety, type of

packing, packer, consignor or markings.

Sublot

designated part of a large 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 ( = subsample).

3. General provisions

Personnel

Sampling shall be performed by an authorised person as specified by the

competent authority.

Material to be sampled

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

with the specific provisions in point 5 of this Schedule, large lots should be

subdivided into sublots to be sampled separately.

Precautions to be taken

In the course of sampling and preparation of the laboratory samples, precautions

must be taken to avoid any changes which would affect the aflatoxin content,

adversely affect the analytical determination or make the aggregate samples

unrepresentative.

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 provided for in 3.8.

Preparation of the aggregate sample and the laboratory samples (subsamples)

The aggregate sample is made up by uniting and sufficiently mixing the

incremental samples. After mixing, the aggregate sample must be divided into

equal subsamples in accordance with the specific provisions of point 5 of this

Schedule.

The mixing is necessary to ensure that each subsample contains Portions of the

whole lot or sublot.

Replicate samples

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

to be taken from the homogenised laboratory sample, unless this conflicts with

Member States' rules on sampling.

Packaging and transmission of laboratory samples

Each laboratory 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

laboratory sample which might arise during transportation or storage.

Sealing and labelling of laboratory samples

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

identified following the Member State's 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.

4. Explanatory provisions

Different types of lots

Food commodities may be traded in bulk, containers, or individual packings

(sacks, bags, retail packings, etc.). The sampling procedure can be applied to all

the different forms in which the commodities are put on the market.

Without prejudice to the specific provisions as laid down in point 5 of this

Schedule, the following formula can be used as a guide for the sampling of lots

traded in individual packings (sacks, bags, retail packings, etc.)

Sampling frequency (SF) = Weight of the lot x weight of the incremental sample

Weight of the aggregate sample x weight of individual packing

—

Weight: in kg

Sampling frequency (SF): every nth sack or bag from which an

incremental sample must be taken (decimal figures should be rounded to

the nearest whole number).

Weight of the incremental sample

The weight of the incremental sample should be about 300 grams unless

otherwise defined in point 5 of this Schedule and with the exception of spices in

which case the weight of the incremental sample is about 100 grams. In the case

of retail packings, the weight of the incremental sample depends on the weight

of the retail packing.

Number of incremental samples for lots of less than 15 tonnes

The number of incremental samples to be taken depends on the weight of the

lot, with a minimum of 10 and a maximum of 100, unless otherwise defined in

point 5 of this Schedule. The figures in the following table may be used to

determine the number of incremental samples to be taken.

Table 1

Number of incremental samples to be taken depending on the

weight of the lot

Lot weight

No of incremental samples

(tonnes)

≤ 0,1

> 0,1 - ≤ 0,2

> 0,2 - ≤ 0,5

> 0,5 - ≤ 1,0

> 1,0 - ≤ 2,0

> 2,0 - ≤ 5,0

> 5,0 - ≤ 10,0

> 10,0 - ≤ 15,0

“the competent authority” means the Veterinary Services

within Malta as provided under article 2 of the Veterinary Services

Act, or any other authority to which such responsibility has been

delegated by the Veterinary Services.

Sample preparation and criteria for methods of analysis used in official

checking of the levels of aflatoxins in certain foodstuffs

1. Introduction

Precautions

Daylight should be excluded as much as possible during the procedure, since

aflatoxin gradually breaks down under the influence of ultra-violet light. As the

distribution of aflatoxin is extremely non-homogeneous, samples should be

prepared — and especially homogenised — with extreme care.

All the material received by the laboratory is to be used for the preparation of

test material.

Calculation of proportion of shell/kernel of whole nuts

The limits fixed for aflatoxins in European Union Commission Regulation (EC)

No 1525/98 apply to the edible part.

The level of aflatoxins in the edible part can be determined by

shelling samples of nuts ‘in shell’ and the level of aflatoxins is directly

determined in the edible part,

homogenise the nuts ‘in shell’ by taking them through the sample

preparation procedure. The sampling and analytical procedure must

estimate the weight of nut kernel in the aggregate sample. The weight of

nut kernel in the aggregate sample is estimated after establishing a suitable

factor for the proportion of nut shell to nut kernel in whole nuts. This

proportion is used to ascertain the amount of kernel in the bulk sample

taken

through

the

sample

preparation

and

analysis

procedure.

Approximately 100 whole nuts are taken at random separately from the lot

or are to be put aside from each aggregate sample. The ratio may, for each

laboratory sample, be obtained by weighing the whole nuts, shelling and

re-weighing the shell and kernel portions. However, the proportion of shell

to kernel may be established by the laboratory from a number of samples

and so can be assumed for future analytical work. But if a particular

laboratory sample is found to be in contravention of any limit, the

proportion should be determined for that sample using the approximately

100 nuts that have been set aside.

2. Treatment of the sample as received in the laboratory

Finely grind and thoroughly mix each laboratory sample using a process that

has been demonstrated to achieve complete homogenisation. In case the

maximum level applies to the dry matter, the dry matter content shall be

determined on a part of the homogenised sample, using a procedure that

hasbeen demonstrated to determine accurately the dry matter content.

3. Subdivision of samples for enforcement and defence purposes

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

shall be taken from the homogenised material unless this conflicts with Member

States' rules on sampling.

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

requirements

Definitions

A number of the most commonly used definitions that the laboratory will be

required to use are given below

The most commonly quoted precision parameters are repeatability and

reproducibility.

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 × s r

sr

= Standard deviation, calculated from results generated under

repeatability conditions

= relative standard deviation, calculated from results generated under

repeatability conditions [(S r/x) × 100], where x is the average of

results over all laboratories and samples

= 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

= standard deviation, calculated from results under reproducibility

conditions

= relative standard deviation calculated from results generated under

reproducibility conditions [(S R/x) × 100]

General requirements

Methods of analysis used for food control purposes must comply whenever

possible with the provisions of points 1 and 2 of the Annex to European Union

Council Directive 85/591/EEC.

4.3. Specific requirements

Where no specific methods for the determination of aflatoxin levels in

foodstuffs are prescribed at European Community level, laboratories may select

any method provided the selected method meets the following criteria

Concentration

Recommended value

Maximum permitted

range

value

All

Negligible

Recovery — Aflatoxin

0,01-0,05 µg/kg

60 to 120 %

>0,05 µg/kg

70 to 110 %

Recovery — Aflatoxins

< 1,0 µg/kg

50 to 120 %

1-10 µg/kg

70 to 110 %

>10 µg/kg

80 to 110 %

All

As derived from

2 × value derived

Horwitz equation

from Horwitz equation

Precision RSD r may be calculated as 0,66 times precision RSD R at the concentration of interest.

Notes

—

Values to apply to both B 1 and sum of B 1 + B 2 + G 1 + G 2 ,

—

if sum of individual aflatoxins B 1 + B 2 + G 1 + G 2 are to be reported, then

response of each to the analytical system must be either known or

equivalent,

—

the detection limits of the methods used are not stated as the precision

values are given at the concentrations of interest,

—

the precision values are calculated from the Horwitz equation, i. e.: RSD R

= 2 (1-0,5 logC) where

—

RSD R is the relative standard deviation calculated from results

generated under reproducibility conditions [(S R /x) × 100]

—

C is the concentration ratio (i. e. 1 = 100 g/100 g, 0,001 = 1 000

mg/kg).

This is a generalised precision equation which has been found to be independent

of analyte and matrix but solely dependent on concentration for most routine

methods of analysis.

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 Schedule I,

points 5.2.2, 5.3.2, 5.4.2, 5.5.1.2 and 5.5.2.3).

The analytical result has to 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 %.

Laboratory quality standards

Laboratories must comply with European Council Directive 93/99/EEC.

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

The competent authority shall take all measures necessary to Necessary measures

to ensure sampling

ensure that the sampling for the official control of the levels of aflatoxins for the official

in foodstuffs is carried out in accordance with the methods described in control

of aflatoxins in

Schedule I to these rules.

foodstuffs.

The competent authority shall take all measures necessary to Necessary measures

ensure that sample preparation and methods of analyses used for the to

preparation and

official control of the levels of aflatoxins in foodstuffs comply with the methods of analyses

used for the official

criteria described in Schedule II to these rules.

control of the levels

of aflatoxins in

foodstuffs.

Specific provisions

General survey of the sampling procedure for groundnuts, nuts, dried fruit,

spices and cereals

Table 2

Subdivision of lots into sublots depending on product and lot weight

Commodity

Lot weight

Weight or

Number of

Aggregate

(tonnes)

number of

incremental

sample

sublots

samples

Weight (kg)

Dried figs and other

≥ 15

15-30 tonnes

dried fruit

< 15

—

10-100 ( )

≤ 30

Groundnuts,

≥ 500

100 tonnes

pistachios,

> 125 and < 500

5 sublots

Brazil nuts and other

≥ 15 and ≤ 125

25 tonnes

10-100 ( 1 )

< 15

—

≤ 30

≥ 1 500

500 tonnes

> 300 and < 1 500

3 sublots

≥ 50 and ≤ 300

100 tonnes

< 50

—

10-100 ( )

1-10

≥ 15

25 tonnes

< 15

—

10-100 ( )

1-10

( ) Depending on the lot weight — see point 4.3 or 5.3 of this Schedule.

Groundnuts, pistachios and Brazil nuts

Dried figs

Cereals (lots ≥ 50 tonnes)

Spices

Sampling procedure

On condition that the sublot can be separated physically, each lot must be

subdivided into sublots following Table 2 at point 5.1. 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 %,

each sublot must be sampled separately,

number of incremental samples: 100. In the case of lots under 15 tonnes,

the number of incremental samples to be taken depends on the weight of

the lot, with a minimum of 10 and a maximum of 100 (see point 4.3),

weight of the aggregate sample = 30 kg which has to be mixed and to be

divided into three equal subsamples of 10 kg before grinding (this division

into three subsamples is not necessary in the case of groundnuts, nuts,

dried fruit and maize intended for further sorting or other physical

treatment, however, this will depend upon the availability of equipment

which is able to homogenise a 30 kg sample). In cases where the aggregate

sample weights are under 10 kg, the aggregate sample must not be divided

into three subsamples. In the case of spices the aggregate sample weighs

not more than 10 kg and therefore no division in subsamples is necessary,

laboratory sample: a subsample of 10 kg (each subsample must be

separately ground finely and mixed thoroughly to achieve complete

homogenisation, in accordance with the provisions laid down in Schedule

II),

if it is not possible to carry out the method of sampling described above

because of the commercial consequences resulting from damage to the lot

(because of packaging forms, means of transport, etc.) an alternative

method of sampling may be applied provided that it is as representative as

possible and is fully described and documented.

Acceptance of a lot or sublot

For groundnuts, nuts, dried fruit and maize subjected to a sorting or other

physical treatment and spices

— acceptance if the aggregate sample or the average of the subsamples

conforms to the maximum limit, taking into account the measurement

uncertainty and correction for recovery,

— rejection if the aggregate sample or the average of the subsamples

exceeds the maximum limit beyond reasonable doubt taking into

account the measurement uncertainty and correction for recovery,

for groundnuts, nuts, dried fruit and cereals intended for direct human

consumption and cereals, with the exception of maize, to be subjected to a

sorting or other physical treatment

— acceptance if none of the subsamples exceeds the maximum limit,

taking into account the measurement uncertainty and correction for

recovery,

— rejection if one or more of the subsamples exceeds the maximum limit

beyond reasonable doubt taking into account the measurement

uncertainty and correction for recovery,

— where the aggregate sample is under 10 kg

— acceptance if the aggregate sample conforms to the maximum

limit, taking into account the measurement uncertainty and

correction for recovery,

— rejection if the aggregate sample exceeds the maximum limit

beyond reasonable doubt taking into account analytical uncertainty

and correction for recovery.

Nuts other than groundnuts, pistachios and Brazil nuts

Dried fruit other than figs

Cereals (lots under 50 tonnes)

Sampling procedure

For these products, the sampling procedure laid down in point 5.2.1 may be

applied. However, taking into account the low incidence of contamination for

these products and/or the newer forms of packaging in which products can be

traded, simpler sampling methods may be applied.

For cereal lots under 50 tonnes, a sampling plan consisting of, depending on the

lot weight, 10 to 100 incremental samples each of 100 grams, resulting in an

aggregate sample of 1 to 10 kg may be used. The figures in the following table

can be used to determine the number of incremental samples to be taken.

Table 3

Number of incremental samples to be taken depending on the

weight of the lot of cereals

Lot weight

Number of incremental samples

(tonnes)

≤1

> 1 - ≤3

> 3 - ≤10

> 10 - ≤20

> 20 - ≤50

Acceptance of a lot or sublot

See point 5.2.2.

Milk

Sampling procedure

Sampling in accordance with European Union Commission Decision

91/180/EEC of 14 February 1991 laying down certain methods of analysis and

testing of raw milk and heat-treated milk

number of incremental samples: minimum 5,

weight of aggregate sample: minimum 0,5 kg or litres.

Acceptance of a lot or sublot

Acceptance if the aggregate sample conforms to the maximum limit,

taking into account the measurement uncertainty and correction for

recovery,

rejection if the aggregate sample exceeds the maximum limit beyond

reasonable doubt taking into account the measurement uncertainty and

correction for recovery.

Derived products and compound foods

Milk products

5.5.1.1. Sampling procedure

Sampling in accordance with European Union Commission Directive

87/524/EEC of 6 October 1987 laying down European Community methods of

sampling for chemical analysis for the monitoring of preserved milk products.

Number of incremental samples: minimum 5.

For the other milk products an equivalent method of sampling is used.

5.5.1.2. Acceptance of a lot or sublot

Acceptance if the aggregate sample conforms to the maximum limit,

taking into account the measurement uncertainty and correction for

recovery,

rejection if the aggregate sample exceeds the maximum limit beyond

reasonable doubt taking into account the measurement uncertainty and

correction for recovery.

Other derived products with very small particle weight, i.e. flour, fig paste,

peanut butter (homogeneous distribution of aflatoxin contamination).

5.5.2.1. Sampling procedure

Number of incremental samples: 100. For lots of under 50 tonnes the

number of incremental samples should be 10 to 100, depending on the lot

weight (see Table 3 at point 5.3.1 of this Schedule),

the weight of the incremental sample should be about 100 grams. In the

case of lots in retail packing, the weight of the incremental sample

depends on the weight of the retail packing,

weight of aggregate sample = 1-10 kg sufficiently mixed.

5.5.2.2. Number of samples to be taken

The number of aggregate samples to be taken depends on the lot weight.

The division of large lots into sublots must be done as defined for cereals

in Table 2 under point 5.1,

each sublot must be sampled separately.

Acceptance of a lot or sublot

Acceptance if the aggregate sample conforms to the maximum limit,

taking into account the measurement uncertainty and correction for

recovery,

rejection if the aggregate sample exceeds the maximum limit beyond

reasonable doubt taking into account the measurement uncertainty and

correction for recovery.

Other derived products with a relatively large particle size (heterogeneous

distribution of aflatoxin contamination)

Sampling procedure and acceptance as defined at points 5.2 and 5.3 of

This Schedule for the raw agricultural product.

Foods intended for infants and young children

Sampling procedure

The sampling procedure as mentioned for milk and derived products as well as

for compound food in points 5.4, 5.5 and 5.6 applies.

Acceptance of a lot

Acceptance if the aggregate sample conforms to the maximum limit,

taking into account the measurement uncertainty and correction for

recovery,

—

Rejection if the aggregate sample exceeds the maximum limit beyond

reasonable doubt, taking into account the measurement uncertainty and

correction for recovery.

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.