(1) "lot" means an identifiable quantity of a food commodity delivered at one time and determined by the competent authority to have common characteristics, such as origin, variety, type of package, packer, consignor or markings; (2) "sublot" means a physically separate and identifiable part of a large lot designated to apply the sampling method; (3) "incremental sample" means a quantity of material taken from a single place in the lot or sublot; (4) "aggregate sample" means the combined total of all the incremental samples taken from the lot or sublot; (5) "subsample" means a quantity of material taken from the aggregate sample for control of ergot sclerotia by visual examination; (6) "laboratory sample" means a representative part or quantity of the aggregate sample intended for the laboratory; (7) "recovery (Rec, %)" means the percentage obtained by applying the following formula x/xref × 100 % where: x measured concentration (for spiked samples corrected for background concentration if not blank), and xref reference concentration (concentration of a Certified Reference Material (CRM), Proficiency Test material, or spiked sample); (8) "bias" means the difference between the measured value and the reference concentration; (9) "repeatability relative standard deviation (RSDr)" means the relative standard deviation (%) calculated from results generated under repeatability conditions (repeatability precision): using the same method on the same sample material in one laboratory by the same operator, with the same instrument, within a short interval of time (1 day or 1 sequence); (10) "within-laboratory reproducibility relative standard deviation (RSDw R )" means the relative standard deviation (%) calculated from results generated under within-laboratory reproducibility conditions (intermediate precision): using the same method on the same sample material in one laboratory but different days (preferably a longer time interval), and may include other conditions, such as involving different operators and/or different (equivalent) instruments;(11) "reproducibility relative standard deviation (RSD R )" means the relative standard deviation (%) calculated from results generated under reproducibility conditions (interlaboratory precision), meaning the same material is analysed by different laboratories. The RSDR may be derived from, in particular, collaborative studies and proficiency tests;(12) "limit of Quantification (LOQ)" means the lowest content of the analyte which can be measured with reasonable statistical certainty. In the context of this regulation this means the lowest successfully validated level: the lowest tested concentration of analyte in a sample material, for which it has been demonstrated that the criteria for recovery, precision, and identification are met For risk assessment, fit-for-purpose LOQs are generally lower compared to what is required for official control for checking compliance with a ML, as the aim is to generate numerical data for the major part of the samples analysed (i.e. avoid left-censored data) in order to be able to perform accurate exposure assessments. For monitoring purposes, it can be acceptable to report levels below the LOQ as defined in the context of this Regulation. (13) "screening target concentration (STC)" means the concentration of interest for detection of the mycotoxin in a sample. When the aim is to test compliance with regulatory limits, the STC is equal to the applicable maximum level. For other purposes or in case no maximum level has been established, the STC is predefined by the laboratory; (14) "screening method" means the method used for selection of those samples with levels of mycotoxins that exceed the screening target concentration (STC), with a given certainty. For the purpose of mycotoxin screening, a certainty of 95 % is considered fit-for-purpose. The result of the screening analysis is either "negative" or "suspect". Screening methods shall allow a cost-effective high sample-throughput, thus increasing the chance to discover new incidents with high exposure and health risks to consumers. These methods shall be based on bio-analytical, LC-MS or HPLC methods. Results from samples exceeding the cut-off value shall be verified by a full re-analysis from the original sample by a confirmatory method; (15) "negative sample" means the mycotoxin content in the sample is < STC with a certainty of 95 % (i.e. there is a 5 % chance that samples will be incorrectly reported as negative); (16) "false negative sample" means the mycotoxin content in the sample is >STC but it has been identified as negative; (17) "suspect sample" (screen positive) means the sample exceeds the cut-off value and may contain the mycotoxin at a level higher than the STC; (18) "false suspect sample" means a negative sample that has been identified as suspect; (19) "confirmatory methods" means methods that provide full or complementary information enabling the mycotoxin to be identified and quantified unequivocally at the level of interest; (20) "cut-off value" means the response, signal, or concentration, obtained with the screening method, above which the sample is classified as "suspect". The cut-off value is determined during the validation and takes the variability of the measurement into account; (21) "negative control (blank matrix) sample" means a sample known to be free of the mycotoxin to be screened for, by previous determination using a confirmatory method of sufficient sensitivity or by other method or, where such sample cannot be obtained, material with the lowest obtainable level as long as the level allows the conclusion that the screening method is fit for that purpose; (22) "sample known to be free" means a sample where the amount present of the analyte does not exceed 1/5 of the STC. If the level can be quantified with a confirmatory method, the level shall be taken into consideration for the validation assessment; (23) "positive control sample" means a sample containing the mycotoxin at the screening target concentration, such as a certified reference material, a material of known content (e.g. test material of proficiency tests) or otherwise sufficiently characterised by a confirmatory method. In the absence of any of the above, a blend of samples with different levels of contamination or a spiked sample prepared within laboratory and sufficiently characterised can be used, provided it can be proven that the contamination level has been verified.
Commission Implementing Regulation (EU) 2023/2782 of 14 December 2023 laying down the methods of sampling and analysis for the control of the levels of mycotoxins in food and repealing Regulation (EC) No 401/2006
Modified by
- Commission Implementing Regulation (EU) 2024/885of 20 March 2024amending Implementing Regulation (EU) 2023/2782 laying down the methods of sampling and analysis for the control of the levels of mycotoxins in food as regards the method of sampling for dried herbs, herbal infusions (dried product), teas (dried product) and powdered spices(Text with EEA relevance), 32024R0885, March 21, 2024
affect the mycotoxin content, adversely affect the analytical determination or make the aggregate samples unrepresentative; affect the food safety of the lots to be sampled.
| Sampling frequency (SF) n = | Weight of the lot x Weight of the incremental sample |
| Weight of the aggregate sample x Weight of individual package |
weight: in kg sampling frequency (SF): every n th individual package from which an incremental sample shall be taken (decimal figures shall be rounded to the nearest whole number).
A. Cereals, oilseeds other than groundnuts, cereal and oilseed products other than groundnut products B. Dried fruit and derived/processed products with the exception of dried figs C. Dried figs and derived/processed products D. Groundnuts (peanuts), apricot kernels, tree nuts and dried spices with large particle size and derived/processed products E. Dried spices except dried spices with large particle size and powdered spices F. Milk and milk products, infant formula, follow-on formula, foods for special medical purposes intended for infants and young children and young child formula G. Coffee, coffee products, cocoa, cocoa products, liquorice root and liquorice products H. Beverages I. Solid processed fruit and vegetable products J. Baby foods and processed cereal-based food for infants and young children K. Vegetable oils L. Food supplements, pollen and pollen products M. Dried herbs, herbal infusions (dried product), teas (dried product) and powdered spices N. Very large lots or lots stored or transported in a way whereby sampling throughout the lot is not feasible
| Commodity | Lot weight (tonne) | Weight or number of sublots | No incremental samples | Aggregate sample weight (kg) |
|---|---|---|---|---|
| Cereals, oilseeds other than groundnuts, cereal products and oilseed products, other than groundnut products | > | 3 sublots | ||
| ≥ | 100 tonnes | |||
| < | — |
On condition that the sublot can be separated physically, each lot shall be subdivided into sublots according to 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 %. In case the lot is not or cannot be physically separated into sublots, a minimum of 100 incremental samples is taken from the lot. For lots > 500 tonnes, the number of incremental samples is provided for in point N.2. Each sublot shall be sampled separately. Number of incremental samples: 100. Weight of the aggregate sample = 10 kg (or 2,5 kg in the case of small particle cereals and oilseeds). If it is not possible to carry out the method of sampling set out in this point because of the unacceptable 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. An alternative method of sampling may also be applied in cases where it is practically impossible to apply the abovementioned method of sampling. This is the case where large lots of cereals are stored in warehouses or where cereals are stored in silos The sampling of such lots shall be performed in accordance with the rules set out in part N. Guidance for sampling large lots shall be provided in a guidance document available on the following website: https://food.ec.europa.eu/system/files/2016-10/cs_contaminants_sampling_guidance-sampling-final_en.pdf
| Lot weight (tonnes) | Number of incremental samples | Aggregate sample weight(kg) | Aggregate sample weight(kg) |
|---|---|---|---|
| ≤ | |||
| > | |||
| > | |||
| > | |||
| > | |||
| > | |||
| > |
acceptance if the first subsample contains less than 50 % of the maximum level of ergot sclerotia or if the average of two subsamples conforms to the maximum level; rejection if the average of two subsamples exceeds the maximum level.
acceptance if the laboratory sample conforms to the maximum level, taking into account the correction for recovery and measurement uncertainty; rejection if the laboratory sample exceeds the maximum level beyond reasonable doubt taking into account the correction for recovery and measurement uncertainty. This is the case when the analytical result (corrected for recovery if applicable) minus the expanded measurement uncertainty arising from the analysis is above the maximum level.
| Commodity | Lot weight (tonnes) | Weight or number of sublots | Number of incremental samples | Aggregate sample weight (kg) |
|---|---|---|---|---|
| Dried fruit, except dried figs | ≥ | |||
| < | — |
On condition that the sublot can be separated physically, each lot shall be subdivided into sublots according to 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 shall be sampled separately. Number of incremental samples: 100. 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.
| Lot weight (tonnes) | Number of incremental samples | Aggregate sample weight (kg) |
|---|---|---|
| ≤ | ||
| > | ||
| > | ||
| > | ||
| > | ||
| > | ||
| > | ||
| > |
acceptance if the laboratory sample conforms to the maximum level, taking into account the correction for recovery and measurement uncertainty; rejection if the laboratory sample exceeds the maximum level beyond reasonable doubt taking into account the correction for recovery and measurement uncertainty. This is the case when the analytical result (corrected for recovery if applicable) minus the expanded measurement uncertainty arising from the analysis is above the maximum level.
| Commodity | Lot weight (tonne) | Weight or number of sublots | No incremental samples | Aggregate sample weight (kg) |
|---|---|---|---|---|
| Dried figs | ≥ | |||
| < | — | ≤ |
On condition that the sublot can be separated physically, each lot shall be subdivided into sublots according to 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 shall be sampled separately. Number of incremental samples: 100 Weight of the aggregate sample = 30 kg, which shall be mixed and divided into three equal laboratory samples of 10 kg before grinding (this division into three laboratory samples is not necessary in case of dried figs subjected to further sorting or other physical treatment and availability of equipment which is able to homogenise a 30 kg sample). Each laboratory sample of 10 kg shall be separately ground finely and mixed thoroughly to achieve complete homogenisation, in accordance with the provisions laid down in Annex II. If it is not possible to carry out the method of sampling described above because of the unacceptable 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 fully described and documented.
| Lot weight (tonnes) | Aggregate sample weight (kg) (in case of retail/individual packages, weight of aggregate sample can diverge – see point C.1) | No of laboratory samples from aggregate sample | |
|---|---|---|---|
| ≤ | |||
| > | |||
| > | |||
| > | |||
| > | |||
| > | |||
| > | |||
| > |
Weight of the aggregate sample ≤ 30 kg which shall be mixed and divided into two or three equal laboratory samples of ≤ 10 kg before grinding (this division into two or three laboratory samples is not necessary in case of dried figs, subjected to further sorting or other physical treatment and availability of equipment which is able to homogenise up to 30 kg samples). In cases where the aggregate sample weights are less than 30 kg, the aggregate sample shall be divided into laboratory samples according to the following guidance: < 12 kg: no division into laboratory samples; ≥ 12 – < 24 kg: division into two laboratory samples; ≥ 24 kg: division into three laboratory samples.
Each laboratory sample shall be separately ground finely and mixed thoroughly to achieve complete homogenisation, in accordance with the provisions laid down in Annex II. If it is not possible to carry out the method of sampling described in the previous indent, because of the unacceptable 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 fully described and documented.
In many cases, lots of fig pastes have no homogenous distribution of mycotoxin contamination and therefore in the case of fig paste, the method of sampling and acceptance as for dried figs (under points C.3 and C.4) shall be applied. Number of incremental samples: 100. For lots of under 50 tons the number of incremental samples shall be 10 to 100, depending on the lot weight (see following Table 3). Table 3 Number of incremental samples to be taken depending on the weight of the lot Lot weight (tonnes) No of incremental samples Aggregate sample weight (kg) ≤ 1 10 1 > 1 – ≤3 20 2 > 3 – ≤10 40 4 > 10 – ≤20 60 6 > 20 – ≤50 100 10 The weight of the incremental sample shall be about 100 g. In the case of lots in retail/individual packages, the weight of the incremental sample depends on the weight of the retail/individual package. Weight of aggregate sample = 1-10 kg sufficiently mixed.
acceptance if none of the laboratory samples exceeds the maximum level, taking into account the correction for recovery and measurement uncertainty; rejection if one or more of the laboratory samples exceed(s) the maximum level beyond reasonable doubt taking into account the correction for recovery and measurement uncertainty. This is the case when the analytical result (corrected for recovery if applicable) minus the expanded measurement uncertainty arising from the analysis is above the maximum level.
acceptance if the laboratory sample conforms to the maximum level, taking into account the correction for recovery and measurement uncertainty, rejection if the laboratory sample exceeds the maximum level beyond reasonable doubt taking into account the correction for recovery and measurement uncertainty. This is the case when the analytical result (corrected for recovery if applicable) minus the expanded measurement uncertainty arising from the analysis is above the maximum level.
| Commodity | Lot weight (tonne) | Weight or number of sublots | No incremental samples | Aggregate sample weight (kg) |
|---|---|---|---|---|
| Groundnuts (peanuts), apricot kernels, tree nuts and dried spices with large particle size | ≥ | |||
| > | ||||
| ≥ | ||||
| < | — | ≤ |
On condition that the sublot can be separated physically, each lot shall 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 shall be sampled separately. Number of incremental samples: 100. Weight of the aggregate sample = 20 kg which shall be mixed and divided into two equal laboratory samples of 10 kg before grinding (this division into two laboratory samples is not necessary in case of groundnuts (peanuts), apricot kernels, tree nuts and dried spices with large particle size subjected to further sorting or other physical treatment and of the availability of equipment which is able to homogenise a 20 kg sample). Each laboratory sample of 10 kg shall be separately ground finely and mixed thoroughly to achieve complete homogenisation, in accordance with the provisions laid down in Annex II. If it is not possible to carry out the method of sampling described above because of the commercial consequences resulting from damage to the lot (because of packaging forms, means of transport, etc.) an alternative method of sampling may be applied provided that it is as representative as possible and is fully described and documented.
| Lot weight (tonnes) | Aggregate sample weight (kg) (in case of retail/individual packages, weight of aggregate sample can diverge – see point D.1) | No of laboratory samples from aggregate sample | |
|---|---|---|---|
| ≤ | |||
| > | |||
| > | |||
| > | |||
| > | |||
| > | |||
| > | |||
| > |
Weight of the aggregate sample ≤ 20 kg which shall be mixed and if necessary divided into two equal laboratory samples of ≤ 10 kg before grinding (this division into two laboratory samples is not necessary in case of groundnuts (peanuts), apricot kernels, tree nuts and dried spices with large particle size subjected to further sorting or other physical treatment and of the availability of equipment which is able to homogenise up to 20 kg samples). In cases where the aggregate sample weights are less than 20 kg, the aggregate sample shall be divided into laboratory samples according to following guidance: < 12 kg: no division into laboratory samples; ≥ 12 kg: division into two laboratory samples.
Each laboratory sample shall be separately ground finely and mixed thoroughly to achieve complete homogenisation, in accordance with the provisions laid down in Annex II. If it is not possible to carry out the method of sampling described above because of the unacceptable 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.
Number of incremental samples: 100; for lots of under 50 tons the number of incremental samples shall be 10 to 100, depending on the lot weight (see Table 3), Table 3 Number of incremental samples to be taken depending on the weight of the lot Lot weight (tonnes) No of incremental samples Aggregate sample weight (kg) ≤ 1 10 1 > 1 – ≤3 20 2 > 3 – ≤10 40 4 > 10 – ≤20 60 6 > 20 – ≤50 100 10 The weight of the incremental sample shall be about 100 g. In the case of lots in retail/individual packages, the weight of the incremental sample depends on the weight of the retail/individual package, Weight of aggregate sample = 1-10 kg sufficiently mixed,
acceptance if the aggregate sample or the average of the laboratory samples conforms to the maximum level, taking into account the correction for recovery and measurement uncertainty, rejection if the aggregate sample or the average of the laboratory samples exceeds the maximum level beyond reasonable doubt taking into account the correction for recovery and measurement uncertainty. This is the case when the analytical result (corrected for recovery if applicable) minus the expanded measurement uncertainty arising from the analysis is above the maximum level.
acceptance if none of the laboratory samples exceeds the maximum level, taking into account the correction for recovery and measurement uncertainty, rejection if one or both of the laboratory samples exceeds the maximum level beyond reasonable doubt taking into account the correction for recovery and measurement uncertainty. This is the case when the analytical result (corrected for recovery if applicable) minus the expanded measurement uncertainty arising from the analysis is above the maximum level.
acceptance if the laboratory sample conforms to the maximum level, taking into account the correction for recovery and measurement uncertainty, rejection if the laboratory sample exceeds the maximum level beyond reasonable doubt taking into account the correction for recovery and measurement uncertainty. This is the case when the analytical result (corrected for recovery if applicable) minus the expanded measurement uncertainty arising from the analysis is above the maximum level.
| Commodity | Lot weight (tonnes) | Weight or number of sublots | Number of incremental samples | Aggregate sample weight (kg) |
|---|---|---|---|---|
| Dried spices | ≥ | |||
| < | — |
On condition that the sublot can be separated physically, each lot shall 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 shall be sampled separately. Number of incremental samples: 100. Weight of the aggregate sample = 10 kg. If it is not possible to carry out the method of sampling described above because of the unacceptable 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.
| Lot weight (tonnes) | Number of incremental samples | Aggregate sample weight (kg) |
|---|---|---|
| ≤ | ||
| > | ||
| > | ||
| > | ||
| > | ||
| > | ||
| > | ||
| > | ||
| > |
acceptance if the laboratory sample conforms to the maximum level, taking into account the correction for recovery and measurement uncertainty; rejection if the laboratory sample exceeds the maximum level beyond reasonable doubt taking into account the correction for recovery and measurement uncertainty. This is the case when the analytical result (corrected for recovery if applicable) minus the expanded measurement uncertainty arising from the analysis is above the maximum level.
| Form of commercialisation | Volume or weight of lot (in litre or kg) | Minimum number of incremental samples to be taken | Minimum volume or weight of aggregate sample (in litre or kg) |
|---|---|---|---|
| Bulk | — | ||
| Bottles/packages | ≤ | ||
| Bottles/packages | |||
| Bottles/packages | > |
acceptance if the laboratory sample conforms to the maximum level, taking into account the correction for recovery and measurement uncertainty; rejection if the laboratory sample exceeds the maximum level beyond reasonable doubt taking into account the correction for recovery and measurement uncertainty. This is the case when the analytical result (corrected for recovery if applicable) minus the expanded measurement uncertainty arising from the analysis is above the maximum level.
| Commodity | Lot weight (ton) | Weight or number of sublots | No incremental samples | Aggregate sample weight (kg) |
|---|---|---|---|---|
| Coffee, coffee products, cocoa, cocoa products, liquorice root and liquorice products | ≥ | |||
| < | — |
On condition that the sublot can be separated physically, each lot shall 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 vary from the mentioned weight by a maximum of 20 %. Each sublot shall be sampled separately, Number of incremental samples: 100, Weight of the aggregate sample = 10 kg, If it is not possible to carry out the method of sampling described above because of the unacceptable 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.
| Lot weight (tonnes) | No of incremental samples | Aggregate sample weight (kg) |
|---|---|---|
| ≤ | ||
| > | ||
| > | ||
| > | ||
| > | ||
| > | ||
| > | ||
| > |
acceptance if the laboratory sample conforms to the maximum level, taking into account the correction for recovery and measurement uncertainty, rejection if the laboratory sample exceeds the maximum level beyond reasonable doubt taking into account the correction for recovery and measurement uncertainty. This is the case when the analytical result (corrected for recovery if applicable) minus the expanded measurement uncertainty arising from the analysis is above the maximum level.
| Form of commercialisation | Volume of lot (in litres) | Minimum number of incremental samples to be taken | Minimum volume of the aggregate sample (in litres) |
|---|---|---|---|
| Bulk | — | ||
| Bottles/packages (beverages other than wine) | ≤ | ||
| Bottles/packages (beverages other than wine) | |||
| Bottles/packages (beverages other than wine) | > | ||
| Bottles/packages wine | ≤ | ||
| Bottles/packages wine | |||
| Bottles/packages wine | > |
acceptance if the laboratory sample conforms to the maximum level, taking into account the correction for recovery and measurement uncertainty, rejection if the laboratory sample exceeds the maximum level beyond reasonable doubt taking into account the correction for recovery and measurement uncertainty. This is the case when the analytical result (corrected for recovery if applicable) minus the expanded measurement uncertainty arising from the analysis is above the maximum level.
| Weight of lot (in kg) | Minimum number of incremental samples to be taken | Aggregate sample weight(kg) |
|---|---|---|
| < | ||
| > |
| Number of packages or units in the lot | Number of packages or units to be taken | Aggregate sample weight(kg) |
|---|---|---|
| about | ||
| > | about |
acceptance if the laboratory sample conforms to the maximum level, taking into account the measurement uncertainty and correction for recovery, rejection if the laboratory sample exceeds the maximum level beyond reasonable doubt taking into account the measurement uncertainty and correction for recovery. This is the case when the analytical result (corrected for recovery if applicable) minus the expanded measurement uncertainty arising from the analysis is above the maximum level.
The method of sampling for cereals and cereal products as set out in point A.4 in part II of this Annex shall apply to food intended for infants and young children. Accordingly, the number of incremental samples to be taken shall depend on the weight of the lot, with a minimum of 10 and a maximum of 100, in accordance with Table 2 at point A.4 in part II of this Annex. For very small lots (≤ 0,5 tonnes) a lower number of incremental samples may be taken, but the aggregate sample uniting all incremental samples shall be also in that case at least 1 kg. weight of the incremental sample shall be about 100 g. In the case of lots in retail/individual packages, the weight of the incremental sample shall depend on the weight of the retail/individual package and in case of very small lots (≤ 0,5 tonnes) the incremental samples shall have a weight as such that uniting the incremental samples results in an aggregate sample of at least 1 kg. Departure from this method shall be recorded in the record provided for under part I point A.1.8 of this Annex. weight of aggregate sample = 1-10 kg sufficiently mixed.
acceptance if the laboratory sample conforms to the maximum level, taking into account the correction for recovery and measurement uncertainty; rejection if the laboratory sample exceeds the maximum level beyond reasonable doubt taking into account the correction for recovery and measurement uncertainty. This is the case when the analytical result (corrected for recovery if applicable) minus the expanded measurement uncertainty arising from the analysis is above the maximum level.
The weight of the incremental sample shall be at least about 100 g (ml) (depending of the nature of the lot e.g. vegetable oil in bulk, at least 3 incremental samples of about 350 ml have to be taken), resulting in an aggregate sample of at least 1 kg (litre). On condition that the sublot can be separated physically, each lot shall 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 %. In case the lot is not or cannot be physically separated into sublots, a minimum of 3 incremental samples is taken from the lot. The minimum number of incremental samples to be taken from the lot shall be as given in Table 2. The lot shall be thoroughly mixed insofar possible by either manual or mechanical means immediately prior to sampling. In this case, a homogeneous distribution of mycotoxins can be assumed within a given lot, it is therefore sufficient to take three incremental samples from a lot to form the aggregate sample. Table 1 Subdivision of lots into sublots depending on lot weight Commodity Lot weight (tonne) Weight or number of sublots Minimum No incremental samples Minimum aggregate sample weight (kg) Vegetable oils ≥ 1500 500 tonnes3 1 > 300 and <1500 3 sublots3 1 ≥ 50 and ≤300 100 tonnes3 1 < 50 — 3 1 Table 2 Minimum number of incremental samples to be taken from the lot On condition that the sublot can be separated physically, large bulk lots of vegetable oils shall be subdivided into sublots as foreseen in Table 2 of this part K Form of commercialisation Weight of lot (in kg) Volume of lot (in litres) Minimum number of incremental samples to be taken Bulk — 3 packages ≤ 50 3 packages > 50 to500 5 packages > 500 10
acceptance if the laboratory sample conforms to the maximum level, taking into account the correction for recovery and measurement uncertainty, rejection if the laboratory sample exceeds the maximum level beyond reasonable doubt taking into account the correction for recovery and measurement uncertainty. This is the case when the analytical result (corrected for recovery if applicable) minus the expanded measurement uncertainty arising from the analysis is above the maximum level.
| Lot size (number of retail/individual packages) | Number of retail/individual packages to be taken for sample | Sample size (minimum amount of the aggregate sample) |
|---|---|---|
| Food supplements as capsules/pills: Total content of the retail/individual package | ||
| ||
| Food supplements as capsules/pills: total content of the two retail/individual packages | ||
| ||
| Food supplements as capsules/pills: from each retail/individual package taken for sample, half of the capsules/pills | ||
| ||
| > | ||
| ||
| Unknown (only applicable for e-commerce) | Food supplements as capsules/pills: total content of the package |
acceptance if the laboratory sample conforms to the maximum level, taking into account the correction for recovery and measurement uncertainty; rejection if the laboratory sample exceeds the maximum level beyond reasonable doubt taking into account the correction for recovery and measurement uncertainty. This is the case when the analytical result (corrected for recovery if applicable) minus the expanded measurement uncertainty arising from the analysis is above the maximum level.
| Commodity | Lot weight (tonnes) | Weight of sublots | Number of incremental samples | Aggregate sample weight (kg) |
|---|---|---|---|---|
| dried herbs, herbal infusions (dried product) teas (dried product), powdered spices | ≥ 15 | 25 tonnes | 50 | 4 |
| < 15 | — | 3 – 50 | 0,2 – 4,0 |
| Lot weight (tonnes) | Minimum number of incremental samples | Minimum aggregate sample weight (kg) |
|---|---|---|
| ≤ 0,1 | ||
| > 0,1 – ≤ 0,5 | ||
| > 0,5 – ≤ 5,0 | ||
| > 5,0 – ≤ 10,0 | ||
| > 10,0 – ≤ 15,0 |
samples of nuts and oilseeds "in shell" can be shelled and the level of mycotoxins is determined in the edible part; the nuts and oilseeds "in shell" can be taken through the sample preparation procedure. The method of sampling and analysis shall estimate the weight of kernel in the aggregate sample. The weight of kernel in the aggregate sample shall be estimated after establishing a suitable factor for the proportion of shell to kernel in whole nuts and oilseeds. This proportion is used to ascertain the amount of kernel in the aggregate sample taken through the sample preparation and method of analysis.
| Mycotoxin | Food | LOQ requirement (μg/kg) |
|---|---|---|
| Aflatoxin B1 | ≤ | |
| Aflatoxin B1, B2, G1, G2, each of the aflatoxins | All other foods | ≤ |
| Liquorice confectionary containing < 97 % liquorice extract on dry basis | ≤ | |
| Cocoa powder | ≤ | |
| Cereals and cereal-based foods | ≤ | |
| Processed cereal-based food for infants and young children | ≤ |
quality control for the batch of samples screened; providing information on robustness of the method at conditions in the laboratory that applies the method; justification of applicability of the method to different commodities; allowing to adjust cut-off values in case of gradual drifts over time.
a statement on the STC; a statement on the determined cut-off value; Note: The cut-off value shall have the same number of significant figures as the STC. Numerical values used to calculate the cut-off value need at least one more significant figure than the STC.a statement on calculated false suspected rate; a statement on how the false suspected rate was generated. Note: The statement on the calculated false suspected rate indicates if the method is fit-for-purpose as it indicates the number of blank (or low level contamination) samples that will be subject to verification.Table 2 Commodity groups for the validation of confirmatory and screening methods If a buffer is used to stabilise the pH changes in the extraction step, then this commodity group can be merged into one commodity group "High water content". "Difficult or unique commodities" needs only to be fully validated if they are frequently analysed. If they are only analysed occasionally, validation may be reduced to just checking the reporting levels using spiked blank extracts. Commodity groups Commodity categories Typical representative commodities included in the category High water content Fruit Juices Alcoholic beverages Root and tuber vegetables Cereal or fruit based purees Apple juice, grape juice Wine, beer, cider Fresh ginger, herbal infusions (liquid) Purees intended for infants and small children High oil content Tree nuts Oil seeds and products thereof Oily fruits and products thereof Walnuts, hazelnuts, chestnuts rapeseed, sunflower, cottonseeds, soybeans, peanuts, sesame seeds etc. Oils and pastes (e.g. peanut butter, tahina) High starch and/or protein content and low water and fat content Cereal grain and products thereof Dietary products Wheat, rye, barley, maize, rice, oats Wholemeal bread, white bread, crackers, breakfast cereals, pasta Dried powders for the preparation of food for infants and small children High acid content and high water content Citrus products "Difficult or unique commodities" Cocoa beans and products thereof, copra and products thereof, coffee, tea (dried product) Spices, liquorice root, herbal infusions (dried product), food supplements, pollen, and pollen products High sugar low water content Dried fruits Figs, raisins, currants, sultanas Milk and milk products Milk Cheese Dairy products (e.g. milk powder) Cow, goat and buffalo milk Cow, goat cheese Yogurt, cream Meat (tissue) Edible offals Muscle, processed meat products Kidney, liver ham Table 3 One tailed t-value for a false negative rate of 5 % Degrees of Freedom Number of replicates t-value (5 %) 10 11 1,812 11 12 1,796 12 13 1,782 13 14 1,771 14 15 1,761 15 16 1,753 16 17 1,746 17 18 1,74 18 19 1,734 19 20 1,729 20 21 1,725 21 22 1,721 22 23 1,717 23 24 1,714 24 25 1,711 25 26 1,708 26 27 1,706 27 28 1,703 28 29 1,701 29 30 1,699 30 31 1,697 40 41 1,684 60 61 1,671 120 121 1,658 ∞ ∞ 1,645
(a) Corrected for recovery, where appropriate and relevant, and when corrected it shall be stated. The recovery rate is to be quoted unless intrinsic correction for bias is part of the procedure. The correction for recovery is not necessary in case the recovery rate is between 90-110 %. (b) As x +/– U whereby x is the analytical result and U is the expanded analytical measurement uncertainty, using a coverage factor of 2 which gives a level of confidence of approximately 95 %.
(1) "lot" means an identifiable quantity of a food commodity delivered at one time and determined by the competent authority to have common characteristics, such as origin, variety, type of package, packer, consignor or markings; (2) "sublot" means a physically separate and identifiable part of a large lot designated to apply the sampling method; (3) "incremental sample" means a quantity of material taken from a single place in the lot or sublot; (4) "aggregate sample" means the combined total of all the incremental samples taken from the lot or sublot; (5) "subsample" means a quantity of material taken from the aggregate sample for control of ergot sclerotia by visual examination; (6) "laboratory sample" means a representative part or quantity of the aggregate sample intended for the laboratory; (7) "recovery (Rec, %)" means the percentage obtained by applying the following formula x/xref × 100 % where: x measured concentration (for spiked samples corrected for background concentration if not blank), and xref reference concentration (concentration of a Certified Reference Material (CRM), Proficiency Test material, or spiked sample); (8) "bias" means the difference between the measured value and the reference concentration; (9) "repeatability relative standard deviation (RSDr)" means the relative standard deviation (%) calculated from results generated under repeatability conditions (repeatability precision): using the same method on the same sample material in one laboratory by the same operator, with the same instrument, within a short interval of time (1 day or 1 sequence); (10) "within-laboratory reproducibility relative standard deviation (RSDw R )" means the relative standard deviation (%) calculated from results generated under within-laboratory reproducibility conditions (intermediate precision): using the same method on the same sample material in one laboratory but different days (preferably a longer time interval), and may include other conditions, such as involving different operators and/or different (equivalent) instruments;(11) "reproducibility relative standard deviation (RSD R )" means the relative standard deviation (%) calculated from results generated under reproducibility conditions (interlaboratory precision), meaning the same material is analysed by different laboratories. The RSDR may be derived from, in particular, collaborative studies and proficiency tests;(12) "limit of Quantification (LOQ)" means the lowest content of the analyte which can be measured with reasonable statistical certainty. In the context of this regulation this means the lowest successfully validated level: the lowest tested concentration of analyte in a sample material, for which it has been demonstrated that the criteria for recovery, precision, and identification are met For risk assessment, fit-for-purpose LOQs are generally lower compared to what is required for official control for checking compliance with a ML, as the aim is to generate numerical data for the major part of the samples analysed (i.e. avoid left-censored data) in order to be able to perform accurate exposure assessments. For monitoring purposes, it can be acceptable to report levels below the LOQ as defined in the context of this Regulation. (13) "screening target concentration (STC)" means the concentration of interest for detection of the mycotoxin in a sample. When the aim is to test compliance with regulatory limits, the STC is equal to the applicable maximum level. For other purposes or in case no maximum level has been established, the STC is predefined by the laboratory; (14) "screening method" means the method used for selection of those samples with levels of mycotoxins that exceed the screening target concentration (STC), with a given certainty. For the purpose of mycotoxin screening, a certainty of 95 % is considered fit-for-purpose. The result of the screening analysis is either "negative" or "suspect". Screening methods shall allow a cost-effective high sample-throughput, thus increasing the chance to discover new incidents with high exposure and health risks to consumers. These methods shall be based on bio-analytical, LC-MS or HPLC methods. Results from samples exceeding the cut-off value shall be verified by a full re-analysis from the original sample by a confirmatory method; (15) "negative sample" means the mycotoxin content in the sample is < STC with a certainty of 95 % (i.e. there is a 5 % chance that samples will be incorrectly reported as negative); (16) "false negative sample" means the mycotoxin content in the sample is >STC but it has been identified as negative; (17) "suspect sample" (screen positive) means the sample exceeds the cut-off value and may contain the mycotoxin at a level higher than the STC; (18) "false suspect sample" means a negative sample that has been identified as suspect; (19) "confirmatory methods" means methods that provide full or complementary information enabling the mycotoxin to be identified and quantified unequivocally at the level of interest; (20) "cut-off value" means the response, signal, or concentration, obtained with the screening method, above which the sample is classified as "suspect". The cut-off value is determined during the validation and takes the variability of the measurement into account; (21) "negative control (blank matrix) sample" means a sample known to be free of the mycotoxin to be screened for, by previous determination using a confirmatory method of sufficient sensitivity or by other method or, where such sample cannot be obtained, material with the lowest obtainable level as long as the level allows the conclusion that the screening method is fit for that purpose; (22) "sample known to be free" means a sample where the amount present of the analyte does not exceed 1/5 of the STC. If the level can be quantified with a confirmatory method, the level shall be taken into consideration for the validation assessment; (23) "positive control sample" means a sample containing the mycotoxin at the screening target concentration, such as a certified reference material, a material of known content (e.g. test material of proficiency tests) or otherwise sufficiently characterised by a confirmatory method. In the absence of any of the above, a blend of samples with different levels of contamination or a spiked sample prepared within laboratory and sufficiently characterised can be used, provided it can be proven that the contamination level has been verified.
affect the mycotoxin content, adversely affect the analytical determination or make the aggregate samples unrepresentative; affect the food safety of the lots to be sampled.
| Sampling frequency (SF) n = | Weight of the lot x Weight of the incremental sample |
| Weight of the aggregate sample x Weight of individual package |
weight: in kg sampling frequency (SF): every n th individual package from which an incremental sample shall be taken (decimal figures shall be rounded to the nearest whole number).
A. Cereals, oilseeds other than groundnuts, cereal and oilseed products other than groundnut products B. Dried fruit and derived/processed products with the exception of dried figs C. Dried figs and derived/processed products D. Groundnuts (peanuts), apricot kernels, tree nuts and dried spices with large particle size and derived/processed products E. Dried spices except dried spices with large particle size and powdered spices F. Milk and milk products, infant formula, follow-on formula, foods for special medical purposes intended for infants and young children and young child formula G. Coffee, coffee products, cocoa, cocoa products, liquorice root and liquorice products H. Beverages I. Solid processed fruit and vegetable products J. Baby foods and processed cereal-based food for infants and young children K. Vegetable oils L. Food supplements, pollen and pollen products M. Dried herbs, herbal infusions (dried product), teas (dried product) and powdered spices N. Very large lots or lots stored or transported in a way whereby sampling throughout the lot is not feasible
| Commodity | Lot weight (tonne) | Weight or number of sublots | No incremental samples | Aggregate sample weight (kg) |
|---|---|---|---|---|
| Cereals, oilseeds other than groundnuts, cereal products and oilseed products, other than groundnut products | > | 3 sublots | ||
| ≥ | 100 tonnes | |||
| < | — |
On condition that the sublot can be separated physically, each lot shall be subdivided into sublots according to 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 %. In case the lot is not or cannot be physically separated into sublots, a minimum of 100 incremental samples is taken from the lot. For lots > 500 tonnes, the number of incremental samples is provided for in point N.2. Each sublot shall be sampled separately. Number of incremental samples: 100. Weight of the aggregate sample = 10 kg (or 2,5 kg in the case of small particle cereals and oilseeds). If it is not possible to carry out the method of sampling set out in this point because of the unacceptable 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. An alternative method of sampling may also be applied in cases where it is practically impossible to apply the abovementioned method of sampling. This is the case where large lots of cereals are stored in warehouses or where cereals are stored in silos The sampling of such lots shall be performed in accordance with the rules set out in part N. Guidance for sampling large lots shall be provided in a guidance document available on the following website: https://food.ec.europa.eu/system/files/2016-10/cs_contaminants_sampling_guidance-sampling-final_en.pdf
| Lot weight (tonnes) | Number of incremental samples | Aggregate sample weight(kg) | Aggregate sample weight(kg) |
|---|---|---|---|
| ≤ | |||
| > | |||
| > | |||
| > | |||
| > | |||
| > | |||
| > |
acceptance if the first subsample contains less than 50 % of the maximum level of ergot sclerotia or if the average of two subsamples conforms to the maximum level; rejection if the average of two subsamples exceeds the maximum level.
acceptance if the laboratory sample conforms to the maximum level, taking into account the correction for recovery and measurement uncertainty; rejection if the laboratory sample exceeds the maximum level beyond reasonable doubt taking into account the correction for recovery and measurement uncertainty. This is the case when the analytical result (corrected for recovery if applicable) minus the expanded measurement uncertainty arising from the analysis is above the maximum level.
| Commodity | Lot weight (tonnes) | Weight or number of sublots | Number of incremental samples | Aggregate sample weight (kg) |
|---|---|---|---|---|
| Dried fruit, except dried figs | ≥ | |||
| < | — |
On condition that the sublot can be separated physically, each lot shall be subdivided into sublots according to 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 shall be sampled separately. Number of incremental samples: 100. 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.
| Lot weight (tonnes) | Number of incremental samples | Aggregate sample weight (kg) |
|---|---|---|
| ≤ | ||
| > | ||
| > | ||
| > | ||
| > | ||
| > | ||
| > | ||
| > |
acceptance if the laboratory sample conforms to the maximum level, taking into account the correction for recovery and measurement uncertainty; rejection if the laboratory sample exceeds the maximum level beyond reasonable doubt taking into account the correction for recovery and measurement uncertainty. This is the case when the analytical result (corrected for recovery if applicable) minus the expanded measurement uncertainty arising from the analysis is above the maximum level.
| Commodity | Lot weight (tonne) | Weight or number of sublots | No incremental samples | Aggregate sample weight (kg) |
|---|---|---|---|---|
| Dried figs | ≥ | |||
| < | — | ≤ |
On condition that the sublot can be separated physically, each lot shall be subdivided into sublots according to 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 shall be sampled separately. Number of incremental samples: 100 Weight of the aggregate sample = 30 kg, which shall be mixed and divided into three equal laboratory samples of 10 kg before grinding (this division into three laboratory samples is not necessary in case of dried figs subjected to further sorting or other physical treatment and availability of equipment which is able to homogenise a 30 kg sample). Each laboratory sample of 10 kg shall be separately ground finely and mixed thoroughly to achieve complete homogenisation, in accordance with the provisions laid down in Annex II. If it is not possible to carry out the method of sampling described above because of the unacceptable 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 fully described and documented.
| Lot weight (tonnes) | Aggregate sample weight (kg) (in case of retail/individual packages, weight of aggregate sample can diverge – see point C.1) | No of laboratory samples from aggregate sample | |
|---|---|---|---|
| ≤ | |||
| > | |||
| > | |||
| > | |||
| > | |||
| > | |||
| > | |||
| > |
Weight of the aggregate sample ≤ 30 kg which shall be mixed and divided into two or three equal laboratory samples of ≤ 10 kg before grinding (this division into two or three laboratory samples is not necessary in case of dried figs, subjected to further sorting or other physical treatment and availability of equipment which is able to homogenise up to 30 kg samples). In cases where the aggregate sample weights are less than 30 kg, the aggregate sample shall be divided into laboratory samples according to the following guidance: < 12 kg: no division into laboratory samples; ≥ 12 – < 24 kg: division into two laboratory samples; ≥ 24 kg: division into three laboratory samples.
Each laboratory sample shall be separately ground finely and mixed thoroughly to achieve complete homogenisation, in accordance with the provisions laid down in Annex II. If it is not possible to carry out the method of sampling described in the previous indent, because of the unacceptable 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 fully described and documented.
In many cases, lots of fig pastes have no homogenous distribution of mycotoxin contamination and therefore in the case of fig paste, the method of sampling and acceptance as for dried figs (under points C.3 and C.4) shall be applied. Number of incremental samples: 100. For lots of under 50 tons the number of incremental samples shall be 10 to 100, depending on the lot weight (see following Table 3). Table 3 Number of incremental samples to be taken depending on the weight of the lot Lot weight (tonnes) No of incremental samples Aggregate sample weight (kg) ≤ 1 10 1 > 1 – ≤3 20 2 > 3 – ≤10 40 4 > 10 – ≤20 60 6 > 20 – ≤50 100 10 The weight of the incremental sample shall be about 100 g. In the case of lots in retail/individual packages, the weight of the incremental sample depends on the weight of the retail/individual package. Weight of aggregate sample = 1-10 kg sufficiently mixed.
acceptance if none of the laboratory samples exceeds the maximum level, taking into account the correction for recovery and measurement uncertainty; rejection if one or more of the laboratory samples exceed(s) the maximum level beyond reasonable doubt taking into account the correction for recovery and measurement uncertainty. This is the case when the analytical result (corrected for recovery if applicable) minus the expanded measurement uncertainty arising from the analysis is above the maximum level.
acceptance if the laboratory sample conforms to the maximum level, taking into account the correction for recovery and measurement uncertainty, rejection if the laboratory sample exceeds the maximum level beyond reasonable doubt taking into account the correction for recovery and measurement uncertainty. This is the case when the analytical result (corrected for recovery if applicable) minus the expanded measurement uncertainty arising from the analysis is above the maximum level.
| Commodity | Lot weight (tonne) | Weight or number of sublots | No incremental samples | Aggregate sample weight (kg) |
|---|---|---|---|---|
| Groundnuts (peanuts), apricot kernels, tree nuts and dried spices with large particle size | ≥ | |||
| > | ||||
| ≥ | ||||
| < | — | ≤ |
On condition that the sublot can be separated physically, each lot shall 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 shall be sampled separately. Number of incremental samples: 100. Weight of the aggregate sample = 20 kg which shall be mixed and divided into two equal laboratory samples of 10 kg before grinding (this division into two laboratory samples is not necessary in case of groundnuts (peanuts), apricot kernels, tree nuts and dried spices with large particle size subjected to further sorting or other physical treatment and of the availability of equipment which is able to homogenise a 20 kg sample). Each laboratory sample of 10 kg shall be separately ground finely and mixed thoroughly to achieve complete homogenisation, in accordance with the provisions laid down in Annex II. If it is not possible to carry out the method of sampling described above because of the commercial consequences resulting from damage to the lot (because of packaging forms, means of transport, etc.) an alternative method of sampling may be applied provided that it is as representative as possible and is fully described and documented.
| Lot weight (tonnes) | Aggregate sample weight (kg) (in case of retail/individual packages, weight of aggregate sample can diverge – see point D.1) | No of laboratory samples from aggregate sample | |
|---|---|---|---|
| ≤ | |||
| > | |||
| > | |||
| > | |||
| > | |||
| > | |||
| > | |||
| > |
Weight of the aggregate sample ≤ 20 kg which shall be mixed and if necessary divided into two equal laboratory samples of ≤ 10 kg before grinding (this division into two laboratory samples is not necessary in case of groundnuts (peanuts), apricot kernels, tree nuts and dried spices with large particle size subjected to further sorting or other physical treatment and of the availability of equipment which is able to homogenise up to 20 kg samples). In cases where the aggregate sample weights are less than 20 kg, the aggregate sample shall be divided into laboratory samples according to following guidance: < 12 kg: no division into laboratory samples; ≥ 12 kg: division into two laboratory samples.
Each laboratory sample shall be separately ground finely and mixed thoroughly to achieve complete homogenisation, in accordance with the provisions laid down in Annex II. If it is not possible to carry out the method of sampling described above because of the unacceptable 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.
Number of incremental samples: 100; for lots of under 50 tons the number of incremental samples shall be 10 to 100, depending on the lot weight (see Table 3), Table 3 Number of incremental samples to be taken depending on the weight of the lot Lot weight (tonnes) No of incremental samples Aggregate sample weight (kg) ≤ 1 10 1 > 1 – ≤3 20 2 > 3 – ≤10 40 4 > 10 – ≤20 60 6 > 20 – ≤50 100 10 The weight of the incremental sample shall be about 100 g. In the case of lots in retail/individual packages, the weight of the incremental sample depends on the weight of the retail/individual package, Weight of aggregate sample = 1-10 kg sufficiently mixed,
acceptance if the aggregate sample or the average of the laboratory samples conforms to the maximum level, taking into account the correction for recovery and measurement uncertainty, rejection if the aggregate sample or the average of the laboratory samples exceeds the maximum level beyond reasonable doubt taking into account the correction for recovery and measurement uncertainty. This is the case when the analytical result (corrected for recovery if applicable) minus the expanded measurement uncertainty arising from the analysis is above the maximum level.
acceptance if none of the laboratory samples exceeds the maximum level, taking into account the correction for recovery and measurement uncertainty, rejection if one or both of the laboratory samples exceeds the maximum level beyond reasonable doubt taking into account the correction for recovery and measurement uncertainty. This is the case when the analytical result (corrected for recovery if applicable) minus the expanded measurement uncertainty arising from the analysis is above the maximum level.
acceptance if the laboratory sample conforms to the maximum level, taking into account the correction for recovery and measurement uncertainty, rejection if the laboratory sample exceeds the maximum level beyond reasonable doubt taking into account the correction for recovery and measurement uncertainty. This is the case when the analytical result (corrected for recovery if applicable) minus the expanded measurement uncertainty arising from the analysis is above the maximum level.
| Commodity | Lot weight (tonnes) | Weight or number of sublots | Number of incremental samples | Aggregate sample weight (kg) |
|---|---|---|---|---|
| Dried spices | ≥ | |||
| < | — |
On condition that the sublot can be separated physically, each lot shall 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 shall be sampled separately. Number of incremental samples: 100. Weight of the aggregate sample = 10 kg. If it is not possible to carry out the method of sampling described above because of the unacceptable 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.
| Lot weight (tonnes) | Number of incremental samples | Aggregate sample weight (kg) |
|---|---|---|
| ≤ | ||
| > | ||
| > | ||
| > | ||
| > | ||
| > | ||
| > | ||
| > | ||
| > |
acceptance if the laboratory sample conforms to the maximum level, taking into account the correction for recovery and measurement uncertainty; rejection if the laboratory sample exceeds the maximum level beyond reasonable doubt taking into account the correction for recovery and measurement uncertainty. This is the case when the analytical result (corrected for recovery if applicable) minus the expanded measurement uncertainty arising from the analysis is above the maximum level.
| Form of commercialisation | Volume or weight of lot (in litre or kg) | Minimum number of incremental samples to be taken | Minimum volume or weight of aggregate sample (in litre or kg) |
|---|---|---|---|
| Bulk | — | ||
| Bottles/packages | ≤ | ||
| Bottles/packages | |||
| Bottles/packages | > |
acceptance if the laboratory sample conforms to the maximum level, taking into account the correction for recovery and measurement uncertainty; rejection if the laboratory sample exceeds the maximum level beyond reasonable doubt taking into account the correction for recovery and measurement uncertainty. This is the case when the analytical result (corrected for recovery if applicable) minus the expanded measurement uncertainty arising from the analysis is above the maximum level.
| Commodity | Lot weight (ton) | Weight or number of sublots | No incremental samples | Aggregate sample weight (kg) |
|---|---|---|---|---|
| Coffee, coffee products, cocoa, cocoa products, liquorice root and liquorice products | ≥ | |||
| < | — |
On condition that the sublot can be separated physically, each lot shall 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 vary from the mentioned weight by a maximum of 20 %. Each sublot shall be sampled separately, Number of incremental samples: 100, Weight of the aggregate sample = 10 kg, If it is not possible to carry out the method of sampling described above because of the unacceptable 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.
| Lot weight (tonnes) | No of incremental samples | Aggregate sample weight (kg) |
|---|---|---|
| ≤ | ||
| > | ||
| > | ||
| > | ||
| > | ||
| > | ||
| > | ||
| > |
acceptance if the laboratory sample conforms to the maximum level, taking into account the correction for recovery and measurement uncertainty, rejection if the laboratory sample exceeds the maximum level beyond reasonable doubt taking into account the correction for recovery and measurement uncertainty. This is the case when the analytical result (corrected for recovery if applicable) minus the expanded measurement uncertainty arising from the analysis is above the maximum level.
| Form of commercialisation | Volume of lot (in litres) | Minimum number of incremental samples to be taken | Minimum volume of the aggregate sample (in litres) |
|---|---|---|---|
| Bulk | — | ||
| Bottles/packages (beverages other than wine) | ≤ | ||
| Bottles/packages (beverages other than wine) | |||
| Bottles/packages (beverages other than wine) | > | ||
| Bottles/packages wine | ≤ | ||
| Bottles/packages wine | |||
| Bottles/packages wine | > |
acceptance if the laboratory sample conforms to the maximum level, taking into account the correction for recovery and measurement uncertainty, rejection if the laboratory sample exceeds the maximum level beyond reasonable doubt taking into account the correction for recovery and measurement uncertainty. This is the case when the analytical result (corrected for recovery if applicable) minus the expanded measurement uncertainty arising from the analysis is above the maximum level.
| Weight of lot (in kg) | Minimum number of incremental samples to be taken | Aggregate sample weight(kg) |
|---|---|---|
| < | ||
| > |
| Number of packages or units in the lot | Number of packages or units to be taken | Aggregate sample weight(kg) |
|---|---|---|
| about | ||
| > | about |
acceptance if the laboratory sample conforms to the maximum level, taking into account the measurement uncertainty and correction for recovery, rejection if the laboratory sample exceeds the maximum level beyond reasonable doubt taking into account the measurement uncertainty and correction for recovery. This is the case when the analytical result (corrected for recovery if applicable) minus the expanded measurement uncertainty arising from the analysis is above the maximum level.
The method of sampling for cereals and cereal products as set out in point A.4 in part II of this Annex shall apply to food intended for infants and young children. Accordingly, the number of incremental samples to be taken shall depend on the weight of the lot, with a minimum of 10 and a maximum of 100, in accordance with Table 2 at point A.4 in part II of this Annex. For very small lots (≤ 0,5 tonnes) a lower number of incremental samples may be taken, but the aggregate sample uniting all incremental samples shall be also in that case at least 1 kg. weight of the incremental sample shall be about 100 g. In the case of lots in retail/individual packages, the weight of the incremental sample shall depend on the weight of the retail/individual package and in case of very small lots (≤ 0,5 tonnes) the incremental samples shall have a weight as such that uniting the incremental samples results in an aggregate sample of at least 1 kg. Departure from this method shall be recorded in the record provided for under part I point A.1.8 of this Annex. weight of aggregate sample = 1-10 kg sufficiently mixed.
acceptance if the laboratory sample conforms to the maximum level, taking into account the correction for recovery and measurement uncertainty; rejection if the laboratory sample exceeds the maximum level beyond reasonable doubt taking into account the correction for recovery and measurement uncertainty. This is the case when the analytical result (corrected for recovery if applicable) minus the expanded measurement uncertainty arising from the analysis is above the maximum level.
The weight of the incremental sample shall be at least about 100 g (ml) (depending of the nature of the lot e.g. vegetable oil in bulk, at least 3 incremental samples of about 350 ml have to be taken), resulting in an aggregate sample of at least 1 kg (litre). On condition that the sublot can be separated physically, each lot shall 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 %. In case the lot is not or cannot be physically separated into sublots, a minimum of 3 incremental samples is taken from the lot. The minimum number of incremental samples to be taken from the lot shall be as given in Table 2. The lot shall be thoroughly mixed insofar possible by either manual or mechanical means immediately prior to sampling. In this case, a homogeneous distribution of mycotoxins can be assumed within a given lot, it is therefore sufficient to take three incremental samples from a lot to form the aggregate sample. Table 1 Subdivision of lots into sublots depending on lot weight Commodity Lot weight (tonne) Weight or number of sublots Minimum No incremental samples Minimum aggregate sample weight (kg) Vegetable oils ≥ 1500 500 tonnes3 1 > 300 and <1500 3 sublots3 1 ≥ 50 and ≤300 100 tonnes3 1 < 50 — 3 1 Table 2 Minimum number of incremental samples to be taken from the lot On condition that the sublot can be separated physically, large bulk lots of vegetable oils shall be subdivided into sublots as foreseen in Table 2 of this part K Form of commercialisation Weight of lot (in kg) Volume of lot (in litres) Minimum number of incremental samples to be taken Bulk — 3 packages ≤ 50 3 packages > 50 to500 5 packages > 500 10
acceptance if the laboratory sample conforms to the maximum level, taking into account the correction for recovery and measurement uncertainty, rejection if the laboratory sample exceeds the maximum level beyond reasonable doubt taking into account the correction for recovery and measurement uncertainty. This is the case when the analytical result (corrected for recovery if applicable) minus the expanded measurement uncertainty arising from the analysis is above the maximum level.
| Lot size (number of retail/individual packages) | Number of retail/individual packages to be taken for sample | Sample size (minimum amount of the aggregate sample) |
|---|---|---|
| Food supplements as capsules/pills: Total content of the retail/individual package | ||
| ||
| Food supplements as capsules/pills: total content of the two retail/individual packages | ||
| ||
| Food supplements as capsules/pills: from each retail/individual package taken for sample, half of the capsules/pills | ||
| ||
| > | ||
| ||
| Unknown (only applicable for e-commerce) | Food supplements as capsules/pills: total content of the package |
acceptance if the laboratory sample conforms to the maximum level, taking into account the correction for recovery and measurement uncertainty; rejection if the laboratory sample exceeds the maximum level beyond reasonable doubt taking into account the correction for recovery and measurement uncertainty. This is the case when the analytical result (corrected for recovery if applicable) minus the expanded measurement uncertainty arising from the analysis is above the maximum level.
| Commodity | Lot weight (tonnes) | Weight of sublots | Number of incremental samples | Aggregate sample weight (kg) |
|---|---|---|---|---|
| dried herbs, herbal infusions (dried product) teas (dried product), powdered spices | ≥ 15 | 25 tonnes | 50 | 4 |
| < 15 | — | 3 – 50 | 0,2 – 4,0 |
| Lot weight (tonnes) | Minimum number of incremental samples | Minimum aggregate sample weight (kg) |
|---|---|---|
| ≤ 0,1 | ||
| > 0,1 – ≤ 0,5 | ||
| > 0,5 – ≤ 5,0 | ||
| > 5,0 – ≤ 10,0 | ||
| > 10,0 – ≤ 15,0 |
samples of nuts and oilseeds "in shell" can be shelled and the level of mycotoxins is determined in the edible part; the nuts and oilseeds "in shell" can be taken through the sample preparation procedure. The method of sampling and analysis shall estimate the weight of kernel in the aggregate sample. The weight of kernel in the aggregate sample shall be estimated after establishing a suitable factor for the proportion of shell to kernel in whole nuts and oilseeds. This proportion is used to ascertain the amount of kernel in the aggregate sample taken through the sample preparation and method of analysis.
| Mycotoxin | Food | LOQ requirement (μg/kg) |
|---|---|---|
| Aflatoxin B1 | ≤ | |
| Aflatoxin B1, B2, G1, G2, each of the aflatoxins | All other foods | ≤ |
| Liquorice confectionary containing < 97 % liquorice extract on dry basis | ≤ | |
| Cocoa powder | ≤ | |
| Cereals and cereal-based foods | ≤ | |
| Processed cereal-based food for infants and young children | ≤ |
quality control for the batch of samples screened; providing information on robustness of the method at conditions in the laboratory that applies the method; justification of applicability of the method to different commodities; allowing to adjust cut-off values in case of gradual drifts over time.
a statement on the STC; a statement on the determined cut-off value; Note: The cut-off value shall have the same number of significant figures as the STC. Numerical values used to calculate the cut-off value need at least one more significant figure than the STC.a statement on calculated false suspected rate; a statement on how the false suspected rate was generated. Note: The statement on the calculated false suspected rate indicates if the method is fit-for-purpose as it indicates the number of blank (or low level contamination) samples that will be subject to verification.Table 2 Commodity groups for the validation of confirmatory and screening methods If a buffer is used to stabilise the pH changes in the extraction step, then this commodity group can be merged into one commodity group "High water content". "Difficult or unique commodities" needs only to be fully validated if they are frequently analysed. If they are only analysed occasionally, validation may be reduced to just checking the reporting levels using spiked blank extracts. Commodity groups Commodity categories Typical representative commodities included in the category High water content Fruit Juices Alcoholic beverages Root and tuber vegetables Cereal or fruit based purees Apple juice, grape juice Wine, beer, cider Fresh ginger, herbal infusions (liquid) Purees intended for infants and small children High oil content Tree nuts Oil seeds and products thereof Oily fruits and products thereof Walnuts, hazelnuts, chestnuts rapeseed, sunflower, cottonseeds, soybeans, peanuts, sesame seeds etc. Oils and pastes (e.g. peanut butter, tahina) High starch and/or protein content and low water and fat content Cereal grain and products thereof Dietary products Wheat, rye, barley, maize, rice, oats Wholemeal bread, white bread, crackers, breakfast cereals, pasta Dried powders for the preparation of food for infants and small children High acid content and high water content Citrus products "Difficult or unique commodities" Cocoa beans and products thereof, copra and products thereof, coffee, tea (dried product) Spices, liquorice root, herbal infusions (dried product), food supplements, pollen, and pollen products High sugar low water content Dried fruits Figs, raisins, currants, sultanas Milk and milk products Milk Cheese Dairy products (e.g. milk powder) Cow, goat and buffalo milk Cow, goat cheese Yogurt, cream Meat (tissue) Edible offals Muscle, processed meat products Kidney, liver ham Table 3 One tailed t-value for a false negative rate of 5 % Degrees of Freedom Number of replicates t-value (5 %) 10 11 1,812 11 12 1,796 12 13 1,782 13 14 1,771 14 15 1,761 15 16 1,753 16 17 1,746 17 18 1,74 18 19 1,734 19 20 1,729 20 21 1,725 21 22 1,721 22 23 1,717 23 24 1,714 24 25 1,711 25 26 1,708 26 27 1,706 27 28 1,703 28 29 1,701 29 30 1,699 30 31 1,697 40 41 1,684 60 61 1,671 120 121 1,658 ∞ ∞ 1,645
(a) Corrected for recovery, where appropriate and relevant, and when corrected it shall be stated. The recovery rate is to be quoted unless intrinsic correction for bias is part of the procedure. The correction for recovery is not necessary in case the recovery rate is between 90-110 %. (b) As x +/– U whereby x is the analytical result and U is the expanded analytical measurement uncertainty, using a coverage factor of 2 which gives a level of confidence of approximately 95 %.