L.S. 437.66 Regoli dwar Metodi għat-Teħid ta’ Kampjuni u Metodi ta’ Analiżi għall-Kontroll Uffiċjali tal-Livelli taċ-Ċomb, Kadmju, Merkurju u 3-MCPD f

(1)The title of these rules is the Sampling Methods and Methods of Analysis for the Official Control of the Levels of Lead, Cadmium, Mercury and 3-MCPD in Foodstuffs Rules. Citation and scope.

(2)The scope of these rules is to implement the rules found under European Union Council Directive 2001/22/EC on the sampling methods and the methods of analysis for the official control of the levels of lead, cadmium, mercury and 3-MCPD in foodstuffs. 2. For the purposes of these rules, and unless context otherwise requires - Definitions. "aggregate sample" means the combined total of all the incremental samples taken from the lot or sublot; "the Commission" means the European Commission; "the Community" means the European Community as established under the Treaty establishing the European Community; "the competent authority" means the Veterinary Services within Malta as provided under article 2 of the Veterinary Services Act; "incremental sample" means a quantity of material taken from a single place in the lot or sublot; "laboratory sample" means the sample intended for the laboratory; "lot" means an identifiable quantity of food delivered at one time a n d d e t e r m i n e d b y th e v e t e r i n ary official to ha ve common characteristics, such as origin, variety, type of packing, packer, consignor or markings. In the case of fish, also the size of fish shall be comparable; "Member State" means a State which is a Member within the European Community; "sublot" means a designated part of a large lot in order to apply the sampling method on that designated part. Each sublot must be physically separated and identifiable; "third country" means a State which is not a Member within the European Community; Cap. 437. 2 [ S.L.437.66 Cap. 437. SAMPLING METHODS AND METHODS OF ANALYSIS FOR THE OFFICIAL CONTROL OF THE LEVELS OF LEAD, CADMIUM, MERCURY AND 3-MCPD IN FOODSTUFFS "Veterinary Services" means the competent authority within the territory of Malta as established under article 2 of the Veterinary Services Act. Sampling for official controls. 3. Malta shall take all measures necessary to ensure that the sampling for the official controls of the levels of lead, cadium, mercury and 3-MCPD in foodstuffs is carried out in accordance with the methods described in Schedule I. Sample preparation and methods of analyses. 4. Malta shall take all measures necessary to ensure that sample preparation and methods of analyses used for the official control of the levels of lead, cadmium, mercury and 3- MCPD in foodstuffs comply with the criteria described in Schedule II to these rules. Reference of procedure and applicability. 5. When Malta adopts these provisions, the provisions shall contain a reference to these rules or shall be accompanied by such reference at the time of their official publication. The procedure for such reference shall be that applicable in Malta. SAMPLING METHODS AND METHODS OF ANALYSIS FOR THE OFFICIAL CONTROL OF THE LEVELS OF LEAD, CADMIUM, MERCURY AND 3-MCPD IN FOODSTUFFS [ S.L.437.66 3 SCHEDULE I METHODS OF SAMPLING FOR OFFICAL CONTROL OF THE LEVELS OF LEAD, CADMIUM, MERCURY AND 3-MCPD IN CERTAIN FOODSTUFFS 1. PURPOSE AND SCOPE Samples intended for the official control of the levels of lead, cadmium, mercury and 3-MCPD contents in foodstuffs shall be taken according to the methods des c r i bed b e l ow. A gg re ga t e s a mp l e s t hus obtained shall be considered as representative of the lots or sublots from which they are taken. Compliance with maximum levels laid down in Regulation (EC) No 466/2001 shall be established on the basis of the levels determined in the laboratory samples. 2. GENERAL PROVISIONS 2.1. Personnel Sampling shall be performed by an authorised qualified person as specified by Malta. 2.2. Material to be sampled Each lot which is to be examined must be sampled separately. 2.3. Precautions to be taken In the course of sampling and preparation of laboratory samples precautions must be taken to avoid any changes which would affect the lead, cadmium, mercury and 3MCPD contents, adversely affect the analytical determination or make the aggregate samples unrepresentative. 2.4. Incremental samples As far as possible incremental samples shall be taken at various places distributed throughout the lot or sublot. Departure from this procedure must be recorded in the record provided for under 2.8. 2.5. Preparation of the aggregate sample The aggregate sample is made up by uniting all incremental samples. It shall be at least 1 kg unless not practical, e.g. when a single package has been sampled. 2.6. Subdivision of aggregate sample in laboratory samples for enforcement, defence and referee purposes The laboratory samples for enforcement, trade (defence) and referee purposes shall be taken from the homogenised aggregate sample unless this conflicts with Veterinary Services’ regulations on sampling. The size of the laboratory samples for enforcement shall be sufficient to allow at least for duplicate analyses. 2.7. Packaging and transmission of aggregate and laboratory samples Each aggregate and laboratory sample shall be placed in a clean, inert container offering adequate protection from contamination, from loss of analytes by adsorption to the internal wall of the container and against damage in transit. All necessary precautions shall be taken to avoid change of composition of the aggregate and laboratory samples which might arise during transportation or storage. 2.8. Sealing and labelling of aggregate and laboratory samples Each sample taken for official use shall be sealed at the place of sampling and identified following the Veterinary Services’ regulations. A record must be kept of each sampling, permitting each lot to be identified unambiguously and giving the 4 [ S.L.437.66 SAMPLING METHODS AND METHODS OF ANALYSIS FOR THE OFFICIAL CONTROL OF THE LEVELS OF LEAD, CADMIUM, MERCURY AND 3-MCPD IN FOODSTUFFS date and place of sampling together with any additional information likely to be of assistance to the analyst. 3. SAMPLING PLANS Sampling should ideally take place at the point where the commodity enters the food chain and a discrete lot becomes identifiable. The sampling method applied shall ensure that the aggregate sample is representative for the lot that is to be controlled. 3.1. Number of incremental samples In the case of liquid products for which a homogeneous distribution of the contaminant in question can be assumed within a given lot, it is sufficient to take one incremental sample per lot which forms the aggregate sample. Reference to the lot number shall be given. Liquid products containing hydrolysed vegetable protein (HVP) or liquid soya sauce shall be shaken well, or homogenised by other suitable means, before the incremental sample is taken. For other products, the minimum number of incremental samples to be taken from the lot shall be as given in Table 1. The incremental samples shall be of similar weight. Departure from this procedure must be recorded in the record provided for under 2.8. Table 1: Minimum number of incremental samples to be taken from the lot Weight of lot (

1. kg)< 50 Minimum number of incremental samples to be taken 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 1 to 25 Number of packages or units to be taken 1 package or unit 26 to 100 About 5%, at least 2 packages or units > 100 About 5%, at maximum 10 packages or units 4. COMPLIANCE OF THE LOT OR SUBLOT WITH THE SPECIFICATION The control laboratory shall analyse the laboratory sample for enforcement at least in two independent analyses, and calculate the mean of the results. The lot is accepted if the mean conforms to the respective maximum level as laid down in Regulation (EC) No 466/2001. It is rejected if the mean exceeds the respective maximum level. SAMPLING METHODS AND METHODS OF ANALYSIS FOR THE OFFICIAL CONTROL OF THE LEVELS OF LEAD, CADMIUM, MERCURY AND 3-MCPD IN FOODSTUFFS [ S.L.437.66 5 SCHEDULE II 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 CADMIUM AND MERCURY PREPARATION PROCEDURES FOR LEAD, 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 (
2. a)but others may be equally valid. The following points must be noted for any procedure used: - bivalve molluscs, crustaceans and small fish: where these are normally eaten whole, the viscera are to be included in the material to be analysed, - vegetables: only the edible portion of is to be tested, with note to be taken of the requirements of the Regulation (EC) No 466/2001. 3. METHOD OF ANALYSIS TO BE USED BY THE LABORATORY AND LABORATORY CONTROL REQUIREMENTS 3.1. Definitions A number of the most commonly used definitions that the laboratory will be required to use are given below: r = repeatability, the value below which the absolute difference between two single test results obtained under repeatability conditions (i.e., same sample, same operator, same apparatus, same laboratory, and short interval of time) may be expected to lie within a specific probability (typically 95%) and hence r = 2,8 × sr. sr = standard deviation, calculated from results generated under repeatability conditions. RSDr = relative standard deviation, calculated from results generated under repeatability conditions [(sr / x -) × 100], where x - is the average of results over all laboratories and samples. R = reproducibility, the value below which the absolute difference between single test results obtained under reproducibility conditions (i.e., on identical material obtained by operators in different laboratories, using the standardised test method), may be expected to lie within a certain probability (typically 95%); R = 2,8 × sR. sR = standard deviation, calculated from results under reproducibility conditions. RSDR = relative standard deviation calculated from results generated under reproducibility conditions [(sR / x-) x 100] HORRATr = the observed RSDr divided by the RSDr value estimated from the Horwitz equation using the assumption r = 0,66R HORRATR = the observed RSDR value divided by the RSDR value calculated from the Horwitz equation (b). 6 [ S.L.437.66 SAMPLING METHODS AND METHODS OF ANALYSIS FOR THE OFFICIAL CONTROL OF THE LEVELS OF LEAD, CADMIUM, MERCURY AND 3-MCPD IN FOODSTUFFS 3.2. General requirements Methods of analysis used for food control purposes must comply whenever possible with the provisions of paragraphs 1 and 2 of the Annex to Directive 85/591/ EEC. For the analysis of lead in wine, Commission Regulation (EEC) No 2676/90 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 Applicability Detection limit Value / comment Foods specified in Regulation (EC) No 466/2001 No more than one tenth of the value of the specification in Regulation (EC) No 466/2001, except if the value of the specification for lead is less than 0,1mg/kg. For the latter, no more than one fifth of the value of the specification Limit of quantification No more than one fifth of the value of the specification in Regulation (EC) No 466/2001, except if the value of the specification for lead is less than 0,1 mg`kg. For the latter, no more than two fifths of the value of the specification Precision HORRATr or HORRATR values of less than 1,5 in the validation collaborative trial Recovery 80 - 120% (as indicated in the collaborative trial) Specificity Free from matrix or spectral interferences 3.3.2. 3-MCPD analysis Specific methods for the determination of 3-MCPD contents are not prescribed. Laboratories shall use a validated method that fulfils the performance criteria indicated in Table 4. Where possible, the validation shall include a certified reference material in the collaborative trial test materials. A specific method has been validated by collaborative trial and has been shown to meet the requirements of Table 4 (c). Table 4: Performance criteria of methods for 3-MCPD analysis Criterion Field blanks Recovery Limit of quantification Recommended value Less than the detection limit 75 - 110% 10 (or less) ìg/kg on a dry matter basis Standard deviation of the field Less than 4 ìg/kg blank signal Concentration All - SAMPLING METHODS AND METHODS OF ANALYSIS FOR THE OFFICIAL CONTROL OF THE LEVELS OF LEAD, CADMIUM, MERCURY AND 3-MCPD IN FOODSTUFFS In-house precision estimates standard deviation of replicate m e a s u r e m e n t s a t d i ff e r e n t concentrations < 4 ìg/kg < 6 ìg/kg < 7 ìg/kg < 8 ìg/kg < 15 ìg/kg [ S.L.437.66 7 20 ìg/kg 30 ìg/g 40 ìg/kg 50 ìg/kg 100 ìg/kg 3.4. Estimation of the analytical trueness and recovery calculations Wherever possible the trueness of the analysis shall be estimated by including suitable certified reference materials in the analytical run. The ‘Harmonised Guidelines for the Use of Recovery Information in Analytical Measurement’ (
3. d)developed under the auspices of IUPAC/ISO/AOAC shall be taken into account. The analytical result shall be reported corrected or uncorrected. The manner of reporting and the level of recovery must be reported. 3.5. Laboratory quality standards Laboratories must comply with Directive 93/99/EEC. 3.6. Expression of results The results shall be expressed in the same units as the maximum levels laid down in Regulation (EC) No 466/2001.