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FOOD SAFETY ACT, 2002 (ACT No. XIV of 2002)Contaminants in Food (Sampling and Analysis Methods) Regulations, 2003
IN exercise of the powers conferred by article 10 of the Food Safety Act, the Minister of
Health has made the following regulations:
(Sampling and Analysis Methods) Regulations, 2003.
2.1 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.
3.1 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.
Title
Sampling Methods for aflatoxins in foodstuffs
Sampling Methods for lead, cadmium, mercury and 3- MPCD in foodstuffs
FIRST SCHEDULE
(Equivalent to Annex I of Commission Directive 98/53/EC)
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
3.1. Personnel
Sampling shall be performed by an official analyst as specified by the Act.
3.2. 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.
3.3. 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.
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 provided for in 3.8.
3.5. 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.
3.6. Replicate samples
The replicate samples for enforcement, trade (defence) and referee purposes are to be taken from the homogenised laboratory sample.
3.7. 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.
3.8. 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
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 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).
4.2. 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.
4.3. 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 (tonnes) | No of incremental samples |
≤ 0.1 | 10 |
> 0.1 - ≤ 0.2 | 15 |
> 0.2 - ≤ 0.5 | 20 |
> 0.5 - ≤ 1.0 | 30 |
> 1.0 - ≤ 2.0 | 40 |
> 2.0 - ≤ 5.0 | 60 |
> 5.0 - ≤ 10.0 | 80 |
> 10.0 - ≤ 15.0 | 100 |
5. Specific provisions
5.1. 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 (tonnes) | Weight or number of sublots | Number of incremental samples | Aggregate sample weight (kg) |
Dried figs and other dried fruit | ≥ 15 < 15 | 15-30 tonnes - | 100 10-100 (*) | 30 ≤ 30 |
Groundnuts, pistachios, Brazil nuts and other nuts | ≥ 500 > 125 & < 500 ≥ 15 & ≤ 125 < 15 | 100 tonnes 5 sublots 25 tonnes - | 100 100 100 10-100 (*) | 30 30 30 ≤ 30 |
Cereals | ≥ 1500 > 300 & < 1500 ≥ 50 & ≤ 300 < 50 | 500 tonnes 3 sublots 100 tonnes - | 100 100 100 10-100 (*) | 30 30 30 1-10 |
* Depending on the lot weight – see point 4.3 or 5.3 of this Schedule
Commodity | Lot weight (tonnes) | Weight or number of sublots | Number of incremental samples | Aggregate sample weight (kg) |
Spices | ≥ 15 < 15 | 25 tonnes - | 100 10-100 (*) | 10 1-10 |
5.2. 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 and dried fruit 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 and dried fruit 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,
– rejection if the aggregate sample or the average of the subsamples exceeds the maximum limit,
– for groundnuts, nuts, dried fruit and cereals intended for direct human consumption:
– acceptance if none of the subsamples exceeds the maximum limit,
– rejection if one or more of the subsamples exceeds the maximum limit,
– where the aggregate sample is under 10 kg:
– acceptance if the aggregate sample conforms to the maximum limit,
– rejection if the aggregate sample exceeds the maximum limit.
5.3. 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 (tonnes) | Number of incremental samples |
≤ 1 | 10 |
> 1 - ≤ 3 | 20 |
> 3 - ≤ 10 | 40 |
> 10 - ≤ 20 | 60 |
> 20 - ≤ 50 | 100 |
5.3.2. Acceptance of a lot or sublot
See point 5.2.2.
5.4. Milk
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,
– rejection if the aggregate sample exceeds the maximum limit.
5.5. 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,
– rejection if the aggregate sample exceeds the maximum limit.
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.
1 OJ L 93, 13. 4. 1991, p. 1.
2 OJ L 306, 28. 10. 1987, p. 24.
5.5.2.3 Acceptance of a lot or sublot
– Acceptance if the aggregate sample conforms to the maximum limit,
– rejection if the aggregate sample exceeds the maximum limit.
5.6. 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.
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.
SECOND SCHEDULE
(Equivalent to Annex II of Commission Directive 98/53/EC)
1. Introduction
1.1. 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.
1.2. 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.
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
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 = Standard deviation, calculated from results generated under repeatability conditions
RSDr = relative standard deviation, calculated from results generated under repeatability conditions [(Sr/x) . 100], where x is the average of results over all laboratories and samples
R = reproducibility, the value below which the absolute difference between single test results obtained under reproducibility conditions
(i.e. on identical material obtained by operators in different laboratories, using the standardised test method) may be expected
to lie within a certain probability (typically 95 %); R = 2.8 sR
sR = standard deviation, calculated from results under reproducibility conditions
RSDR = relative standard deviation calculated from results generated under reproducibility conditions [(SR/x).100]
4.2. 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.
4.3. 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 |
Blanks | All | Negligible | |
Recovery – Aflatoxin M1 | 0.01 – 0.05 µg/kg > 0.05 µg/kg | 60 to120 % 70 to 110 % | |
Recovery – Aflatoxins B1, B2, G1, G2 | < 1.0 µg/kg 1-10 µg/kg > 10 µg/kg | 50 to 120 % 70 to110 % 80 to 110 % | |
Precision RSDR | All | As derived from Horwitz equation | 2 x value derived from Horwitz equation |
Precision RSDR may be calculated as 0.66 times precision RSDR at the concentration of interest.
Notes:
– Values to apply to both B1 and sum of B1+B2+G1+G2,
– if sum of individual aflatoxins B1+B2+G1+G2 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.: RSDR = 2 (1-0,5 logC)
where:
– RSDR is the relative standard deviation calculated from results generated under reproducibility conditions [(SR/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.
4.5. Laboratory quality standards
Laboratories must comply with Council Directive 93/99/EEC.
THIRD SCHEDULE
(Equivalent to Annex I of Commission Directive 2001/22/EC)
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
3.1. Personnel
Sampling shall be performed by an authorised analyst as specified by the Act.
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 lead, cadmium, mercury and 3-MCPD contents, adversely affect the analytical determination or make the aggregate samples unrepresentative.
3.4. Incremental samples
As far as possible incremental samples shall be taken at various places distributed throughout the lot or sublot. Departure from this
procedure must be recorded in the record provided for under 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. 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. 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.
4.1. Number of incremental samples
In the case of liquid products for which a homogeneous distribution of the contaminant in question can be assumed within a given lot,
it is sufficient to take one incremental sample per lot which forms the aggregate sample. Reference to the lot number shall be given.
Liquid products containing hydrolysed vegetable protein (HVP) or liquid soya sauce shall be shaken well, or homogenised by other
suitable means, before the incremental sample is taken. For other products, the minimum number of incremental samples to be taken
from the lot shall be as
given in Table 1. The incremental samples shall be of similar weight. Departure from this procedure must be recorded in the record
provided for under 3.8.
Table 1: Minimum number of incremental samples to be taken from the lot
Weight of lot (kg) | Minimum number of incremental samples to be taken |
< 50 | 3 |
50 to 500 | 5 |
> 500 | 10 |
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.
FOURTH SCHEDULE
(Equivalent to Annex II of Commission Directive 2001/22/EC)
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
3.1. Definitions
A number of the most commonly used definitions that the laboratory will be required to use are given below:
r = repeatability, the value below which the absolute difference between two single test results obtained under repeatability conditions
(i.e., same sample, same operator, same apparatus, same laboratory, and short interval of time) may be expected to lie within a specific
probability (typically 95 %) and hence r = 2.8 . sr.
sr = standard deviation, calculated from results generated under repeatability conditions.
RSDr = relative standard deviation, calculated from results generated under repeatability conditions [(sr / x ) × 100] , where x is the average of results over all laboratories and samples.
3 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 . sR.
sR = standard deviation, calculated from results under reproducibility conditions. RSDR = relative standard deviation calculated from results generated under
reproducibility conditions [(sR / x ) × 100]
HORRATr = the observed RSDr divided by the RSDr value estimated from the
Horwitz equation using the assumption r = 0,66R
HORRATR = the observed RSDR value divided by the RSDR value calculated from the Horwitz equation (4).
3.2. General requirements
Methods of analysis used for food control purposes must comply whenever possible with the provisions of paragraphs 1 and 2 of the
Annex to Directive
85/591/EEC 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.
3.3. Specific requirements
3.3.1. Lead, cadmium and mercury analyses
Specific methods for the determination of lead, cadmium and mercury contents are not prescribed. Laboratories shall use a validated
method that fulfils the performance criteria indicated in Table 3. Where possible, the validation shall include a certified reference
material in the collaborative trial test materials.
Table 3: Performance criteria of methods for lead, cadmium and mercury analyses
Parameter | Value/comment |
Applicability | Foods specified in 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 |
4 W Horwitz, ‘Evaluation of Analytical Methods for Regulation of Foods and Drugs’, Anal. Chem., 1982, No 54, 67A-76A
5 OJ L 272, 3.10.1990, p. 1.
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 | HORRATr or HORRATR values of less than 1.5 in the validation collaborative trial |
Recovery | 80-120 % (as indicated in the collaborative trial) |
Specificity | Free from matrix or spectral interferences |
3.3.2. 3-MCPD analysis
Specific methods for the determination of 3-MCPD contents are not prescribed. Laboratories shall use a validated method that fulfils
the performance criteria indicated in Table 4. Where possible, the validation shall include a certified reference material
in the collaborative trial test materials. A specific method has been validated by collaborative trial and has been shown to meet
the requirements of Table 4 (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 |
Limit of quantification | 10 (or less) µg on a dry matter basis | - |
Standard deviation of the field blank signal | Less than 4 µg/kg | - |
In-house precision estimates – standard deviation of replicate measurements at different concentrations | < 4 µg/kg < 6 µg/kg < 7 µg/kg < 8 µg/kg < 15 µg/kg | 20 µg/kg 30 µg/kg 40 µg/kg 50 µg/kg 100 µg/kg |
3.4. Estimation of the analytical trueness and recovery calculations
Wherever possible the trueness of the analysis shall be estimated by including suitable certified reference materials in the analytical
run. The ‘Harmonised Guidelines for the Use of Recovery Information in Analytical Measurement’ (7)
6 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’).
7 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.
3.5. Laboratory quality standards
Laboratories must comply with Directive 93/99/EEC.
3.6. Expression of results
The results shall be expressed in the same units as the maximum levels laid down in the Contaminants in Foods Regulations.
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