Regulations, 2004

L.N. 488 of 2004

FOOD SAFETY ACT

(CAP. 449)

Contaminants in Food (Sampling and Analysis Methods)

Regulations, 2004

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

1 The title of these regulations is the Contaminants in Food Title

(Sampling and Analysis Methods) Regulations, 2004.

1.2

These regulations implement the provisions of

(a) Commission Directive 98/53/EC of the 16 th July, 1998

laying down the sampling methods and the methods of analysis

for the official control of the levels for certain contaminants in

foodstuffs;

(b) Commission Directive 2002/26/EC of the 13 th March,

2002 amending Directive 98/53/EC laying down the sampling

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

levels for certain contaminants in foodstuffs;

(c) Commission Directive 2002/27/EC of the 13 th March,

2002 amending Directive 98/53/EC laying down the sampling

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

levels for certain contaminants in foodstuffs;

(d) Commission Directive 2003/121/EC of 15 th December,

2003 amending Directive 98/53/EC laying down the sampling

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

levels for certain contaminants in foodstuffs;

(e) Commission Directive 2004/43/EC of 13 th April, 2004

amending Directive 98/53/EC and Directive 2002/26/EC as regards

sampling methods and methods of analysis for the official control

of the levels of aflatoxin and ochratoxin A in food for infants and

young children;

(f) Commission Directive 2001/22/EC of 8 th March, 2001

laying down the sampling methods and the methods of analysis

for the official control of the levels of lead, cadmium, mercury

and 3-MCPD in foodstuffs;

(g) Commission Directive 2002/69/EC of 26 th July, 2002

laying down the sampling methods and the methods of analysis

for the official control of dioxins and the determination of dioxin-

like PCBs in foodstuffs;

(h) Commission Directive 2004/44/EC of 13 th April, 2004

amending Directive 2002/69/EC laying down the sampling

methods and the methods of analysis for the official control of

dioxins and the determination of dioxin-like PCBs in foodstuffs

(i) Commission Directive 2002/26/EC of 13 th March, 2002

laying down the sampling methods and the methods of analysis

for the official control of the levels of ochratoxin A in foodstuffs;

(j) Commission Directive 2003/78/EC of 11 th August, 2003

laying down the sampling methods and the methods of analysis

for the official control of the levels of patulin in foodstuffs.

(Equivalent to Annex I of Commission Directive 98/53/EC)

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 Commission Regulation (EC) No

1525/98 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 official analyst as specified by the Act.

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

B

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.

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. 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

5. 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 weight

sublots

samples

(kg)

≥ 15

Dried figs and other dried fruit

15-30 tonnes

10-100 ( * )

≤ 30

-

< 15

≥ 500

Groundnuts, pistachios, Brazil

100 tonnes

nuts and other nuts

5 sublots

> 125 & < 500

25 tonnes

≥ 15 & ≤ 125

10-100 ( * )

≤ 30

-

< 15

≥ 1500

Cereals

500 tonnes

3 sublots

> 300 & < 1500

100 tonnes

≥ 50 & ≤ 300

10-100 ( * )

-

1-10

< 50

Depending on the lot weight – see point 4.3 or 5.3 of this Schedule

B

Commodity

Lot weight

Weight or

Number of

Aggregate

(tonnes)

number of

incremental

sample weight

sublots

samples

(kg)

≥ 15

25 tonnes

-

10-100 (*)

1-10

< 15

Groundnuts, pistachios and Brazil nuts

Dried figs

Cereals (lots ≥ 50 tonnes)

Spices

5.2.1. 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 the

Second Schedule),

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.

5.2.2. 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 the measurement

uncertainty and correction for recovery.

Nuts other than groundnuts, pistachios and Brazil nuts

Dried fruit other than figs

Cereals (lots under 50 tonnes)

5.3.1. 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

> 3 - ≤ 10

> 10 - ≤ 20

> 20 - ≤ 50

B

5.3.2. Acceptance of a lot or sublot

See point 5.2.2.

5.4.1. Sampling procedure

Sampling in accordance with Commission Decision 91/180/EEC of 14 February

1991 laying down certain methods of analysis and testing of raw milk and heat-

treated milk 1

number of incremental samples: minimum 5,

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

5.4.2. 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.

Derived products and compound foods

5.5.1. Milk products

5.5.1.1. Sampling procedure

Sampling in accordance with Commission Directive 87/524/EEC of 6 October

1987 laying down Community methods of sampling for chemical analysis for the

monitoring of preserved milk products 2 .

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.

OJ L 93, 13. 4. 1991, p. 1.

OJ L 306, 28. 10. 1987, p. 24.

5.5.2. 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.

5.5.2.3 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

compounded 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.

B

6. 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.

1 The sampling for the official control of the levels of aflatoxins

in foodstuffs shall be carried out in accordance with the methods

described in the First Schedule to these regulations.

2.2 The sample preparation and methods of analyses used for

the official control of the levels of aflatoxins in foodstuffs shall comply

with the criteria described in the Second Schedule to these regulations.

(Equivalent to Annex II of Commission Directive 98/53/EC)

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 the Contaminants in Food Regulations 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 mix thoroughly each laboratory sample using a process that has

been demonstrated to achieve complete homogenisation.

B

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 has

been 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 homogenized material.

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

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) . 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 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).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 Council Directive

85/591/EEC.

Specific requirements

Where no specific methods for the determination of aflatoxin levels in foodstuffs

are prescribed at Community level, laboratories may select any method provided

the selected method meets the following criteria

Criterion

Concentration range

Recommended value

Maximum permitted

value

All

Negligible

0.01 – 0.05 µg/kg

Recovery – Aflatoxin

60 to120 %

70 to 110 %

> 0.05 µg/kg

< 1.0 µg/kg

Recovery – Aflatoxins

50 to 120 %

70 to110 %

1-10 µg/kg

80 to 110 %

> 10 µg/kg

Precision RSD R

All

As derived from

2 x value derived from

Horwitz equation

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

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

B

result corrected for recovery is used for checking compliance (see First Schedule,

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 confidence of approximately 95 %.

Laboratory quality standards

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

1 The sampling for the official control of the levels of lead,

cadmium, mercury and 3-MCPD in foodstuffs shall be carried out in

accordance with the methods described in the Third Schedule to these

regulations.

3.2 The sample preparation and methods of analyses used for

the official control of the levels of lead, cadmium, mercury and 3-MCPD

in foodstuffs shall comply with the criteria described in the Fourth

Schedule to these regulations.

(Equivalent to Annex I of Commission Directive 2001/22/EC)

Methods Of Sampling For Offical Control Of The Levels Of Lead, Cadmium,

Mercury And 3-MPCD 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 the Contaminants in Food Regulations shall be

established on the basis of the levels determined in the laboratory samples.

2. DEFINITIONS

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.

Laboratory sample: sample intended for the laboratory

3. GENERAL PROVISIONS

Personnel

Sampling shall be performed by an authorised analyst as specified by the Act.

Material to be sampled

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

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.

B

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 3.8.

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.

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. The size of the laboratory

samples for enforcement shall be sufficient to allow at least for duplicate

analyses.

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.

Sealing and labelling of aggregate and laboratory samples

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

identified. 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

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.

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 3.8.

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

5. 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

the Contaminants in Food Regulations. It is rejected if the mean exceeds the

respective maximum level.

B

1 The sampling for the official control of the levels of

ochratoxin A in foodstuffs shall be carried out in accordance with the

methods described in the Fifth Schedule to these regulations.

4.2 The sample preparation and methods of analyses used for

the official control of the levels of ochratoxin A in foodstuffs shall

comply with the criteria described in the Sixth Schedule to these

regulations.

(Equivalent to Annex II of Commission Directive 2001/22/EC)

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 ( 3 ) 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 Contaminants in Food Regulations.

3. 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

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 .

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 ) × 100 ] , where x is the average of results over all

laboratories and samples.

Draft Standard prEN 13804, ‘Foodstuffs — Determination of Trace Elements — Performance Criteria

and General Considerations’, CEN, Rue de Stassart 36, B-1050 Brussels.

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 / x ) × 100 ]

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

Horwitz equation using the assumption r = 0,66R

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

from the Horwitz equation ( 4 ).

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 of the European Community. For the analysis of lead in wine,

Commission Regulation (EEC) No 2676/90( 5 ) determining Community methods

for the analysis of wines lays down the method to be used in Chapter 35 of its

Annex.

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 the Contaminants in Food

Regulations

Detection limit

No more than one tenth of the value of the

specification in the Contaminants in Food

Regulations, except if the value of the specification

W Horwitz, ‘Evaluation of Analytical Methods for Regulation of Foods and Drugs’, Anal. Chem., 1982,

No 54, 67A-76A

OJ L 272, 3.10.1990, p. 1.

B

Parameter

Value/comment

for lead is less than 0.1 mg/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 the Contaminants in Food

Regulations, 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

HORRAT r or HORRAT R 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 ( 6 ).

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

10 (or less) µg on a dry matter

Limit of quantification

-

basis

Less than 4 µg/kg

Standard deviation of the field

-

blank signal

< 4 µg/kg

20 µg/kg

In-house precision estimates –

standard deviation of replicate

< 6 µg/kg

30 µg/kg

measurements at different

< 7 µg/kg

40 µg/kg

concentrations

< 8 µg/kg

50 µg/kg

< 15 µg/kg

100 µg/kg

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’ ( 7 )

Method of Analysis to determine 3-Monochloropropane-1,2-Diol in Food and Food Ingredients using

Mass Spectrometric Detection, submitted to CEN TC 275 and AOAC International (also available as

‘Report of the Scientific Cooperation task 3.2.6: Provision of validated methods to support the Scientific

Committee on Food’s recommendations regarding 3-MCPD in hydrolysed protein and other foods’).

ISO/AOAC/IUPAC Harmonised Guidelines for the Use of Recovery Information in Analytical

Measurement. Edited Michael Thompson, Steven L R Ellison, Ales Fajgelj, Paul Willetts and Roger Wood,

Pure Appl. Chem., 1999, No 71, 337-348

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.

Laboratory quality standards

Laboratories must comply with Directive 93/99/EEC.

Expression of results

The results shall be expressed in the same units as the maximum levels laid down

in the Contaminants in Foods Regulations.

B

1 The sampling for the official control of the levels of dioxins Sampling and

and furans and the determination of the levels of dioxin-like PCBs in analytical

for dioxins and

foodstuffs shall be carried out in accordance with the methods described dioxin-like PCBs in

foodstuffs.

in the Seventh Schedule to these regulations.

5.2 The sample preparation and methods of analyses used for

the official control of the levels of dioxins and furans and the

determination of the levels of dioxin-like PCBs in foodstuffs shall

comply with the criteria described in the Eighth Schedule to these

regulations.

(Equivalent to Annex I of Commission Directive 2002/26/EC)

Methods of Sampling for Official Control of the Levels of Ochratoxin A in certain

foodstuffs

1. Purpose and scope

Samples intended for official checking of the levels of ochratoxin A 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 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 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.

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. In accordance with the

specific provisions of this Schedule, large lots should be subdivided into sublots to 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 ochratoxin A 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 the incremental samples.

3.6. Replicate samples

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

taken from the homogenised sample, unless this conflicts with other applicable 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 appropriate procedures established by the Food Safety Commission. 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. Specific provisions

4.1. 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 points 4.3, 4.4 and 4.5 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) n = Weight of the lot . Weight of the incremental sample

Weight of the aggregate sample . Weight of individual packaging

—

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).

4.2. Weight of the aggregate sample

B

The weight of the incremental sample should be about 100 grams, unless otherwise

defined in this Schedule. In the case of lots in retail packings, the weight of the

incremental sample depends on the weight of the retail packing.

4.3. General survey of the sampling procedure for cereals and dried vine fruit

Table 1: 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)

Cereals

and

cereal ≥ 1500

500 tonnes

products

> 300 and <

3 sublots

≥ 50 and ≤

100 tonnes

10-100 ( 8 )

< 50

-

1-10

vine

fruit ≥ 15

15–30 tonnes

(currants, raisins and

10-100 ( 9 )

< 15

-

1-10

sultanas)

4.4. Sampling procedure for cereals and cereal products (lots ≥ 50 tonnes) and dried

vine fruit (lots ≥ 15 tonnes)

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

subdivided into sublots following Table 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 of cereals under 50

tonnes and lots of dried vine fruit under 15 tonnes, see point 4.5. Weight of the

aggregate sample = 10 kg.

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.

4.5. Sampling provisions for cereals and cereal products (lots < 50 tonnes) and for dried

vine fruit (lots < 15 tonnes)

Depending on the lot weight – See Table 2 of this Schedule.

Depending on the lot weight – See Table 3 of this Schedule.

For cereal lots under 50 tonnes and for dried vine fruit lots under 15 tonnes, the sampling

plan has to be used with 10 to 100 incremental samples, depending on the lot weight,

resulting in an aggregate sample of 1 to 10 kg.

The figures in the following table can be used to determine the number of incremental

samples to be taken.

Table 2: Number of incremental samples to be taken depending on the weight of the lot of

cereals

Lot weight

Number of incremental samples

(tonnes)

≤ 1

>3 - ≤ 10

> 10 - ≤ 20

> 20 - ≤ 50

Table 3: Number of incremental samples to be taken depending on the weight of the lot of

dried vine fruit

Lot weight

Number 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

4.6 Sampling procedure for foods intended for infants and young children

The sampling procedure as mentioned for cereals and cereal products in point 4.5 of this

Schedule applies. This means that 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, in

accordance with Table 2 at point 4.5.

-

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

in retail packing, the weight of the incremental sample depends on the weight of

the retail packing.

-

Weight of aggregate sampling = 1 to 10 kg sufficiently mixed.

B

4.7. 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. 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.

1 The sampling for the official control of the levels of patulin Sampling and

analytical methods

in foodstuffs shall be carried out in accordance with the methods for patulin in

foodstuffs.

described in the Ninth Schedule to these regulations.

6.2 The sample preparation and methods of analyses used for

the official control of the levels of patulin in foodstuffs shall comply

with the criteria described in the Tenth Schedule to these regulations.

(Equivalent to Annex II of Commission Directive 2002/26/EC)

Sample Preparation and Criteria for Methods of Analysis used in Official Checking

of the Levels of Ochratoxin A in certain foodstuffs

1. Precautions

As the distribution of ochratoxin A is 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.

2. Treatment of the sample as received in the laboratory

Finely grind and mix thoroughly the complete aggregate 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 has been

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 other applicable 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

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 × sr

sr= 1

Standard deviation, calculated from results generated under repeatability

conditions

B

Relative standard deviation, calculated from results generated under

s

−

repeatability conditions [ − r . 100 ] where x is the average of results over

x

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 × sR

Standard deviation, calculated from results under reproducibility

conditions

Relative standard deviation calculated from results generated under

S

reproducibility conditions [ r − . 100 ].

x

4.2. General requirements

Methods of analysis used for food control purposes must comply with the provisions of

items 1 and 2 of the Annex to Directive 85/591/EEC concerning the introduction of

Community methods of sampling and analysis for the monitoring of foodstuffs intended

for human consumption.

4.3. Specific requirements

Where no specific methods for the determination of ochratoxin A levels in foodstuffs are

prescribed at Community level, laboratories may select any method provided the selected

method meets the following criteria

Performance characteristics for ochratoxin A

Ochratoxin A

(µg/kg)

RSD r

RSD R

Recovery

(%)

(%)

(%)

≤ 40

≤ 60

50 to120

≤ 20

≤ 30

70 to110

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

RSD R = 2 ( 1 − 0 . 5 log C )

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.

4.4. Recovery calculation

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 shall be used for checking compliance (see Fifth Schedule, point 5).

The analytical result has to be reported as x ± U, whereby x is the analytical result and U

is the expanded measurement uncertainty.

U is the expanded uncertainty, using a coverage factor of 2 which gives a level of

confidence of approximately 95 %.

4.5. Laboratory quality standards

Laboratories must comply with Directive 93/99/EEC on the subject of additional

measures concerning the official control of foodstuffs.

B

1 The Contaminants (Sampling and Analysis Methods) Repeal of L.N. 240

of 2003.

Regulations, 2003 are hereby repealed.

(Equivalent to Annex I of Commission Directive 2002/69/EC)

Methods of Sampling for Official Control of the Levels of Dioxins (PCDD/PCDF)

and the Determination of Dioxin-like PCBs in certain foodstuffs

1. Purpose and scope

Samples intended for the official control of the levels of dioxins (PCDD/PCDF) content,

as well for the determination of the content of dioxin-like PCBs ( 10 ) 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 Commission Regulation (EC) No

466/2001 setting maximum levels for certain contaminants in foodstuffs shall be

established on the basis of the levels determined in the laboratory samples.

2. Definitions

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 and fishery products, 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.

Laboratory sample: a representative part/quantity of the aggregate sample intended for

the laboratory.

Table WHO TEFs for human risk assessment based on the conclusions of the World Health Organisation

meeting in Stockholm, Sweden, 15-18 June 1997 (Van den Berg et al., (1998) Toxic Equivalency Factors

(TEFs) for PCBs, PCDDs, PCDFs for Humans and for Wildlife. Environmental Health Perspectives,

106(12), 775).

Congener

TEF value

Dibenzo-p-dioxins (PCDDs)

2,3,7,8-TCDD

1,2,3,7,8-PeCDD

1,2,3,4,7,8-HxCDD

0.1

1,2,3,6,7,8-HxCDD

0.1

1,2,3,7,8,9-HxCDD

0.1

1,2,3,4,6,7,8-HpCDD

0.01

OCDD

0.0001

Dibenzofurans (PCDFs)

2,3,7,8-TCDF

0.1

1,2,3,7,8-PeCDF

0.05

2,3,4,7,8-PeCDF

0.5

1,2,3,4,7,8-HxCDF

0.1

1,2,3,6,7,8-HxCDF

0.1

1,2,3,7,8,9-HxCDF

0.1

2,3,4,6,7,8-HxCDF

0.1

1,2,3,4,6,7,8-HpCDF

0.01

1,2,3,4,7,8,9-HpCDF

0.01

OCDF

0.0001

‘Dioxin-like’ PCBs

Non-ortho PCBs + Mono-ortho PCBs

Non-ortho PCBs

PCB 77

0.0001

PCB 81

0.0001

PCB 126

0.1

PCB 169

0.01

Mono-ortho PCBs

PCB 105

0.0001

PCB 114

0.0005

PCB 118

0.0001

PCB 123

0.0001

PCB 156

0.0005

PCB 157

0.0005

PCB 167

0.00001

PCB 189

0.0001

Abbreviations used: T = tetra; Pe = penta; Hx = hexa; Hp = hepta; O = octa; CDD = chlorodibenzodioxin;

CDF = chlorodibenzofuran; CB = chlorobiphenyl

B

3. General provisions

3.1. Personnel

Sampling shall be performed by an authorised qualified 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 laboratory samples precautions must be

taken to avoid any changes, which would affect the content of dioxins and dioxin-like

PCBs, adversely affect the analytical determination or make the aggregate samples

unrepresentative.

3.4. Incremental samples

As far as practical 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 3.8.

3.5. 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.

3.6. 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 other provisions

on sampling. The size of the laboratory samples for enforcement shall be sufficient to

allow at least for duplicate analyses.

3.7. 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.

3.8. 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 procedures established by the Food Safety Commission. 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.

Number of incremental samples

In the case of milk and oils, for which a homogeneous distribution of the contaminants in

question can be assumed within a given lot, it is sufficient to take three incremental

samples per lot which forms the aggregate sample. Reference to the lot number shall be

given. For other products, the minimum number of incremental samples to be taken from

the lot shall be as given in Table 1. The aggregate sample uniting all incremental samples

shall be at least 1 kg (see point 3.5). The incremental samples shall be of similar weight.

The weight of an incremental sample should be at least 100 grams. The weight of the

incremental sample is dependent on the size of the particles in the lot. Departure from this

procedure must be recorded in the record provided for under 3.8. In accordance with the

provisions of Commission Decision 97/747/EC of the 27 th October, 1997 fixing the levels

and frequencies of sampling provided for by Council Directive 96/23/EC for the

monitoring of certain substances and residues thereof in certain animal products ( 11 ), the

sample size for hen eggs is at least 12 eggs (for bulk lots as well for lots consisting of

individual packages, Tables 1 and 2).

TABLE 1

Minimum number of incremental samples to be taken from the lot

Weight of the 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 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

OJ L 303, 6.11.1997, p. 12.

B

Specific provisions for the sampling of lots containing whole fishes

The number of incremental samples to be taken from the lot is defined in Table 1. The

aggregate sample uniting all incremental samples shall be at least 1 kg (see point 3.5).

In case the lot to be sampled contains small fish (individual fish weighing < 1 kg),

the whole fish is taken as incremental sample to form the aggregate sample. In

case the resulting aggregate sample weighs more than 3 kg, the incremental

samples can consist of the middle part, weighing each at least 100 grams, of the

fish forming the aggregate sample. The whole part to which the maximum level is

applicable is used for homogenisation of the sample.

In case the lot to be sampled contains larger fish (individual fish weighing more

than 1 kg), the incremental sample consists of the middle part of the fish. Each

incremental sample weighs at least 100 grams. In case the lot to be sampled

consist of very large fish (e.g. > 6 kg) and taking a piece of the middle part of the

fish would result in significant economic damage, taking three incremental

samples of at least 350 grams each can be considered sufficient, independently of

the size of the lot.

5. Compliance of the lot or sublot with the specification

The lot is accepted if the analytical result of a single analysis does not exceed the

respective maximum level as laid down in Regulation (EC) No 466/2001, taking into

account the measurement uncertainty.

The lot is non-compliant with the maximum level as laid down in Regulation (EC) No

466/2001, if the analytical result confirmed by duplicate analysis and calculated as the

mean of at least two separate determinations exceeds the maximum level beyond

reasonable doubt, taking into account the measurement uncertainty.

The taking into account of the measurement uncertainty can be done according to one of

the following approaches

by calculating the expanded uncertainty, using a coverage factor of 2, which gives

a level of confidence of approximately 95 %,

by establishing the decision limit (CCα) according to the provisions of

Commission Decision 2002/657/EC of the 12 th August, 2002 implementing

Council Directive 96/23/EC concerning the performance of analytical methods

and the interpretation of results ( 12 ) (point 3.1.2.5 of the Annex — the case of

substances with established permitted levels).

OJ L 221, 17.8.2002, p. 8. Decision as last amended by Decision 2004/25/EC (OJ L 6, 10.1.2004, p. 38).

The present interpretation rules apply for the analytical result obtained on the sample for

official control. In case of analysis for defence or referee purposes, the national rules

apply.

B

Reporting of the result

Insofar as the used analytical procedure makes it possible, the analytical results should

contain the levels of the individual PCDD/F and PCB congeners and be reported as

lowerbound, upperbound and mediumbound in order to include a maximum of

information in the reporting of the results and thereby enabling the interpretation of the

results according to specific requirements.

The report should also include the lipid content of the sample as well the method used for

lipid extraction.

The recoveries of the individual internal standards must be made available in case the

recoveries are outside the range mentioned in point 6, in case the maximum level is

exceeded and in other cases upon request.

B

Sample Preparation and Requirements for Methods of Analysis used in Official

Control of the Levels of Dioxins (PCDD/PCDF) and the Determination of Dioxin-

like PCBs in certain foodstuffs

1. Objective and field of application

These requirements should be applied where foodstuffs are analysed for the official

control of the levels of dioxins (polychlorinated dibenzo-p-dioxins (PCDD) and

polychlorinated dibenzofurans (PCDF)) and the determination of dioxin-like PCBs.

Monitoring for the presence of dioxins in foodstuffs can be performed by a strategy

involving a screening method in order to select those samples with levels of dioxins and

dioxin-like PCBs that are less than 30-40 % below or exceed the level of interest. The

concentration of dioxins in those samples with significant levels needs to be

determined/confirmed by a confirmatory method.

Screening methods are methods that are used to detect the presence of dioxins and

dioxin-like PCBs at the level of interest. These methods have a capacity for a high sample

throughput and are used to sift large numbers of samples for potential positives. They are

specifically designed to avoid false negatives.

Confirmatory methods are methods that provide full or complementary information

enabling the dioxins and dioxin-like PCBs to be identified and quantified unequivocally

at the level of interest.

2. Background

Because environmental and biological samples (including samples of foodstuffs) in

general contain complex mixtures of different dioxin congeners, the concept of Toxic

Equivalency Factors (TEFs) has been developed to facilitate risk assessment. These TEFs

have been established to express concentrations of mixtures of 2,3,7,8-substituted PCDDs

and PCDFs, and more recently, some non-ortho and mono-ortho chlorine substituted

PCBs which possesses dioxin-like activity in toxic equivalents (TEQs) of 2,3,7,8-TCDD

(see Seventh Schedule, footnote 1).

The concentrations of the individual substances in a given sample are multiplied by their

respective TEF and subsequently summed to give the total concentration of dioxin-like

compounds expressed as TEQs.

The concept of ‘upperbound’ requires using the limit of quantification for the

contribution of each non-quantified congener to the TEQ.

The concept of ‘lowerbound’ requires using zero for the contribution of each non-

quantified congener to the TEQ.

The concept of ‘mediumbound’ requires using half of the limit of quantification

calculating the contribution of each non-quantified congener to the TEQ.

For the purposes of this Schedule only, the accepted specific limit of quantification of an

individual congener is the concentration of an analyte in the extract of a sample which

produces an instrumental response at two different ions, to be monitored with an S/N

(signal/noise) ratio of 3:1 for the less sensitive signal and fulfilment of the basic

requirements such as, e.g., retention time, isotope ratio according to the determination

procedure as described in EPA method 1613 revision B.

3. Quality assurance requirements to be complied with for sample preparation

Measures must be taken to avoid cross-contamination at each stage of the

sampling and analysis procedure.

The samples must be stored and transported in glass, aluminium, polypropylene

or polyethylene containers. Traces of paper dust must be removed from the

sample container. Glassware should be rinsed with solvents previously controlled

for the presence of dioxins.

The sample storage and transportation has to be performed in a way that

maintains the integrity of the foodstuff sample.

Insofar as relevant, finely grind and mix thoroughly each laboratory sample using

a process that has been demonstrated to achieve complete homogenisation (e.g.

ground to pass a 1 mm sieve); samples have to be dried before grinding if

moisture content is too high.

Perform a blank analysis by carrying out the entire analytical procedure omitting

only the sample.

Sample weight used for the extraction must be sufficient to fulfil the requirements

with respect to sensitivity.

There are many satisfactory specific sample preparation procedures, which may

be used for the products under consideration. The procedures have to be validated

according to internationally accepted guidelines.

4. Requirements for laboratories

Laboratories shall demonstrate the performance of a method in the range of the

level of interest, e.g. 0,5 ×, 1 × and 2 × the level of interest with an acceptable

coefficient of variation for repeated analysis. For details of acceptance criteria,

see point 5.

B

Limit of quantification for a confirmatory method should be in the range of about

one fifth of the level of interest, to make sure that acceptable coefficients of

variations are met in the range of the level of interest.

Regular blank controls and spiking experiments or analysis of control samples

(preferably, if available, certified reference material) should be performed as

internal quality control measures.

Successful participation in interlaboratory studies that assess laboratory

proficiency is the best way to prove the competence in specific analyses. However

successful participation in interlaboratory studies for, e.g. soil or sewage samples,

does not necessarily prove the competence also in the field of food or feedingstuff

samples, which present lower contamination levels. Therefore, the continuous

participation in interlaboratory studies for the determination of dioxins and

dioxin-like PCBs in the relevant feed/food matrices is mandatory.

In accordance with the provisions of Directive 93/99/EEC, laboratories should be

accredited by a recognised body operating in accordance with ISO Guide 58 to

ensure that they are applying analytical quality assurance. Laboratories should be

accredited following the ISO/IEC/17025:1999 standard.

5. Requirements to be met by analytical procedure for dioxinsand dioxin-like PCBs

Basic requirements for acceptance of analytical procedures

High sensitivity and low limits of detection. For PCDDs and PCDFs, detectable

quantities have to be in the picogram TEQ (10-12 g) range because of extreme

toxicity of some of these compounds. PCBs are known to occur at higher levels

than the PCDDs and PCDFs. For most PCB congeners sensitivity in the nanogram

(10-9 g) range is already sufficient. However, for the measurement of the more

toxic dioxin-like PCB congeners (in particular non-ortho substituted congeners),

the same sensitivity must be reached as for the PCDDs and PCDFs.

High selectivity (specificity). A distinction is required for PCDDs, PCDFs and

dioxin-like PCBs from a multitude of other, coextracted and possibly interfering

compounds present at concentrations up to several orders of magnitude higher

than those of the analytes of interest. For gas chromatography/mass spectrometry

(GC/MS) methods a differentiation among various congeners is necessary, such

as between toxic (e.g. the seventeen 2,3,7,8-substituted PCDDs and PCDFs and

dioxin-like PCBs) and other congeners. Bioassays should be able to determine

TEQ values selectively as the sum of PCDDs, PCDFs and dioxin-like PCBs.

High accuracy (trueness and precision). The determination should provide a valid

estimate of the true concentration in a sample. High accuracy (accuracy of the

measurement: the closeness of the agreement between the result of a measurement

with the true or assigned value of the measurement) is necessary to avoid the

rejection of a sample analysis result on the basis of poor reliability of the estimate

of TEQ. Accuracy is expressed as trueness (difference between the mean value

measured for an analyte in a certified material and its certified value, expressed as

percentage of this value) and precision (precision is usually calculated as a

standard deviation including repeatability and reproducibility, and indicates the

closeness of agreement between the results obtained by applying the experimental

procedure several times under prescribed conditions).

Screening methods can comprise bioassays and GC/MS methods; confirmatory

methods are high-resolution gas chromatography/high resolution mass

spectrometry (HRGC/HRMS) methods. Following criteria have to be complied

with on total TEQ value

Screening methods

Confirmatory methods

False negative rate

< 1 %

Trueness

-20 % to + 20 %

< 30 %

< 15 %

6. Specific requirements for GC/MS methods to be complied with for screening or

confirmatory purposes

Addition of 13 C-labelled 2,3,7,8-chlorine substituted internal PCDD/F standards

(and of 13 C-labelled internal dioxin-like PCB standards, if dioxin-like PCBs have

to be determined) must be carried out at the very beginning or start of the

analytical method e.g. prior to extraction in order to validate the analytical

procedure. At least one congener for each of the tetra to octa-chlorinated

homologous groups for PCDD/F (and at least one congener for each of the

homologous groups for dioxin-like PCBs, if dioxin-like PCBs have to be

determined) must be added (alternatively, at least one congener for each mass

spectrometric selected ion recording function used for monitoring PCDD/F and

dioxin-like PCBs). There is a clear preference, certainly in case of confirmatory

methods, of using all 17 13 C-labelled 2,3,7,8-substituted internal PCDD/F

standards and all 12 13 C-labelled internal dioxin-like PCB standard (if dioxin-like

PCBs have to be determined).

Relative response factors should also be determined for those congeners for which

no 13 C-labelled analogue is added by using appropriate calibration solutions.

For foodstuffs of plant origin and foodstuffs of animal origin containing less than

10 % fat, the addition of the internal standards is mandatory prior to extraction.

For foodstuffs of animal origin containing more than 10 % fat, the internal

standards can be added either before extraction or after fat extraction. An

appropriate validation of the extraction efficiency should be carried out,

depending on the stage at which internal standards are introduced and on whether

results are reported on product or fat basis.

B

Prior to GC/MS analysis, 1 or 2 recovery (surrogate) standard(s) must be added.

Control of recovery is necessary. For confirmatory methods, the recoveries of the

individual internal standards should be in the range of 60 % to 120 %. Lower or

higher recoveries for individual congeners, in particular for some hepta- and octa-

chlorinated dibenzodioxins and dibenzofurans, are acceptable on the condition

that their contribution to the TEQ value does not exceed 10 % of the total TEQ

value (based on PCDD/F only). For screening methods, the recoveries should be

in the range of 30 % to 140 %.

Separation of dioxins from interfering chlorinated compounds such as PCBs and

chlorinated diphenyl ethers should be carried out by suitable chromatographic

techniques (preferably with a florisil, alumina and/or carbon column).

Gas chromatographic separation of isomers should be sufficient (< 25 % peak to

peak between 1,2,3,4,7,8-HxCDF and 1,2,3,6,7,8-HxCDF).

Determination should be performed according to EPA Method 1613 revision B

Tetra- through octa-chlorinated dioxins and furans by isotope dilution

HRGC/HRMS or another with equivalent performance criteria.

The difference between upperbound level and lower bound level should not

exceed 20 % for foodstuffs with a dioxin contamination of about 1 pg WHO-

TEQ/g fat (based on PCDD/PCDF only). For foodstuffs with a low fat content,

the same requirements for contamination levels of about 1 pg WHO-TEQ/g

product have to be applied. For lower contamination levels, for example 0,50 pg

WHO-TEQ/g product, the difference between upperbound and lowerbound level

may be in the range of 25 to 40 %.

7. Screening methods of analysis

7.1. Introduction

Different analytical approaches can be performed using a screening method: a pure

screening approach and a quantitative approach.

Screening approach

The response of samples is compared to that of a reference sample at the level of interest.

Samples with a response less than the reference are declared negative, those with a higher

response are suspected positives. Requirements

A blank and a reference sample(s) have to be included in each test series, which is

extracted and tested at the same time under identical conditions. The reference

sample must show a clearly elevated response in comparison to a blank.

Extra reference samples 0,5 × and 2 × the level of interest should be included to

demonstrate the proper performance of the test in the range of interest for the

control of the level of interest.

When testing other matrices, the suitability of the reference sample(s) has to be

demonstrated, preferentially by including samples shown by HRGC/HRMS to

contain a TEQ level around that of the reference sample or else a blank spiked at

this level.

Since no internal standards can be used in bioassays, tests on repeatability are

very important to obtain information on the standard deviation within one test

series. The coefficient of variation should be below 30 %.

For bioassays, the target compounds, possible interferences and maximum

tolerable blank levels should be defined.

Quantitative approach

The quantitative approach requires standard dilution series, duplicate or triplicate clean

up and measuring as well as blank and recovery controls. The result may be expressed as

TEQ, thereby assuming that the compounds responsible for the signal correspond to the

TEQ principle. This can be performed by using TCDD (or a dioxin/furan standard

mixture) to produce a calibration curve to calculate the TEQ level in the extract and thus

in the sample. This is subsequently corrected for the TEQ level calculated for a blank

sample (to account for impurities from solvents and chemicals used), and a recovery

(calculated from the TEQ level in a quality control sample around the level of interest). It

is essential to note that part of the apparent recovery loss may be due to matrix effects

and/or differences between the TEF values in the bioassays and the official TEF values

set by WHO.

7.2. Requirements for methods of analysis used for screening

GC/MS methods of analysis and bioassays may be used for screening. For

GC/MS methods the requirements as laid down in point 6 are to be used. For cell

based bioassays specific requirements are laid down in point 7.3 and for kit-based

bioassays in point 7.4.

Information on the number of false-positive and false-negative results of a large

set of samples below and above the maximum level or action level is necessary, in

comparison to the TEQ content as determined by a confirmatory method of

analysis. Actual false negative rates should be under 1 %. The rate of false

positive samples should be low enough to make the use of a screening tool

advantageous.

Positive results have always to be confirmed by a confirmatory method of

analysis (HRGC/HRMS). In addition, samples from a wide TEQ-range should be

B

confirmed by HRGC/HRMS (approximately 2 % to 10 % of the negative

samples). Information on correspondence between bioassay and HRGC/HRMS

results should be made available.

7.3. Specific requirements for cell-based bioassays

When performing a bioassay, every test run requires a series of reference

concentrations of TCDD or a dioxin/furan mixture (full dose-response curve with

a R2 > 0,95). However, for screening purposes an expanded low level curve for

analysing low level samples could be used.

A TCDD reference concentration (about 3 × limit of quantification) on a quality

control sheet should be used for the outcome of the bioassay over a constant time

period. An alternative could be the relative response of a reference sample in

comparison to the TCDD calibration line since the response of the cells may

depend on many factors.

Quality control (QC) charts for each type of reference material should be recorded

and checked to make sure the outcome is in accordance with the stated guidelines.

In particular for quantitative calculations, the induction of the sample dilution

used must be within the linear portion of the response curve. Samples above the

linear portion of the response curve must be diluted and re-tested. Therefore, at

least three or more dilutions at one time are recommended to be tested.

The percent standard deviation should not be above 15 % in a triplicate

determination for each sample dilution and not above 30 % between three

independent experiments.

The limit of detection may be set as 3 × the standard deviation of the solvent

blank or of the background response. Another approach is to apply a response that

is above the background (induction factor 5 × the solvent blank) calculated from

the calibration curve of the day. The limit of quantification may be set as 5 × to 6

× the standard deviation of the solvent blank or of the background response or to

apply a response that is above the background (induction factor 10 × the solvent

blank) calculated from the calibration curve of the day.

7.4. Specific requirements for kit-based bioassays ( 13 )

Manufacturer's instructions for sample preparation and analyses have to be

followed.

No evidence have yet been submitted of commercially available kit-based bioassays having sufficient

sensitivity and reliability to be used for screening for the presence of dioxins at the required levels in

samples of foodstuffs and feedingstuffs.

Test kits should not be used after the expiration date.

Materials or components designed for use with other kits should not be used.

Test kits should be kept within the specified range of storage temperature and

used at the specified operating temperature.

The limit of detection for immunoassays is determined as 3 × the standard

deviation, based on 10 replicate analysis of the blank, to be divided by the slope

value of the linear regression equation.

Reference standards should be used for tests at the laboratory to make sure that

the responsiveness to the standard is within an acceptable range.

(Equivalent to Annex I of Commission Directive 2003/78/EC)

Methods of Sampling for Official Control of the Levels of Patulin in certain

foodstuffs

1. Purpose and scope

Samples intended for official checking of the levels of patulin 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

Commission 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.

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 patulin 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 the incremental samples. It shall be at least 1

kg unless not practical e.g. when a single package has been sampled.

3.6. Replicate samples

Replicate samples for enforcement, trade (defence) and referee purposes shall be taken

from the homogenised aggregate sample unless this conflicts with other provisions 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 procedures established by the Food Safety Commission.

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.

Number of incremental samples

The aggregate sample shall be at least 1 kg (see point 3.5), except where it is not possible

e.g. when sampling a single package.

The minimum number of incremental samples to be taken from the lot shall be as given

in Table 1. In the case of liquid products the lot shall be thoroughly mixed insofar as

possible by either manual or mechanical means immediately prior to sampling. In this

B

case, a homogeneous distribution of patulin can be assumed within a given lot. It is

therefore sufficient to take three incremental samples from a lot to form the aggregate

sample.

The incremental samples shall be of similar weight. The weight of an incremental sample

should be at least 100 grams, resulting in an aggregate sample of at least 1 kg. Departure

from this procedure must be recorded in the record provided for under 3.8.

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 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

5. Compliance of the lot or sublot with the specification

The control laboratory shall analyse the laboratory sample for enforcement in duplicate

analysis in case the obtained result of the first analysis is less than 20 % below or above

the maximum level, and calculate the mean of the results.

The lot is accepted if the result of the first analysis is more than 20 % below the

maximum level 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) No

466/2001, if the mean, corrected for recovery exceeds the maximum level beyond

reasonable doubt taking into account the measurement uncertainty.

Sample Preparation and Criteria for Methods of Analysis used in Official Checking

of the Levels of Patulin in certain foodstuffs

1. Precautions

As the distribution of patulin in certain foodstuffs could be 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.

2. Treatment of the sample as received in the laboratory

Finely grind (insofar 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 homogenised material unless this conflicts with other provisions 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.

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 x s r .

s r =

Standard deviation, calculated from results generated under repeatability

conditions.

B

Relative standard deviation, calculated from results generated under

s

−

repeatability conditions [ − r . 100 ] where x is the average of results over

x

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 x s R .

Standard deviation, calculated from results under reproducibility

conditions.

Relative standard deviation calculated from results generated under

s

reproducibility conditions [ − r . 100 ].

x

4.2. General requirements

Methods of analysis used for food control purposes must comply with the provisions of

items 1 and 2 of the Annex to Council Directive 85/591/EEC of the 20 th December, 1985

concerning the introduction of Community methods of sampling and analysis for the

monitoring of foodstuffs intended for human consumption ( 14 ).

4.3. Specific requirements

Where no specific methods for the determination of patulin in foodstuffs are prescribed at

Community level, laboratories may select any method provided the selected method

meets the following criteria

Patulin

RSD r %

RSD R %

Recovery %

≤ 30

≤ 40

50 to120

≤ 20

≤ 30

70 to105

≤ 15

≤ 25

75 to 105

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

OJ L 372, 31.12.1985, p. 50.

RSD R = 2 ( 1 − 0 . 5 log C )

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 = 100g/100g, 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.

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 Annex I, point 5).

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 Council Directive 93/99/EEC of 29 th October, 1993 on

the subject of additional measures concerning the official control of foodstuffs.