Commission Directive 98/53/EC of 16 July 1998 laying down the sampling methods and the methods of analysis for the official control of the levels for certain contaminants in foodstuffs (Text with EEA relevance)
Modified by
- Commission Directive 2002/27/ECof 13 March 2002amending Directive 98/53/EC laying down the sampling methods and the methods of analysis for the official control of the levels for certain contaminants in foodstuffs(Text with EEA relevance), 32002L0027, March 16, 2002
- Commission Directive 2003/121/ECof 15 December 2003amending Directive 98/53/EC laying down the sampling methods and the methods of analysis for the official control of the levels for certain contaminants in foodstuffs(Text with EEA relevance), 32003L0121, December 19, 2003
- Commission Directive 2004/43/ECof 13 April 2004amending Directive 98/53/EC and Directive 2002/26/EC as regards sampling methods and methods of analysis for the official control of the levels of aflatoxin and ochratoxin A in food for infants and young children(Text with EEA relevance), 32004L0043, April 20, 2004
- Commission Regulation (EC) No 401/2006of 23 February 2006laying down the methods of sampling and analysis for the official control of the levels of mycotoxins in foodstuffs(Text with EEA relevance), 32006R0401, March 9, 2006
| an identifiable quantity of a food commodity delivered at one time and determined by the official to have common characteristics, such as origin, variety, type of packing, packer, consignor or markings. | |
| designated part of a large lot in order to apply the sampling method on that designated part. Each sublot must be physically separate and identifiable. | |
| a quantity of material taken from a single place in the lot or sublot. | |
| the combined total of all the incremental samples taken from the lot or sublot. | |
| sample intended for the laboratory ( = subsample). |
Weight: in kg Sampling frequency (SF): every nth sack or bag from which an incremental sample must be taken (decimal figures should be rounded to the nearest whole number).
| No of incremental samples | |
|---|---|
| ≤ 0,1 | |
| > 0,1 - ≤ 0,2 | |
| > 0,2 - ≤ 0,5 | |
| > 0,5 - ≤ 1,0 | |
| > 1,0 - ≤ 2,0 | |
| > 2,0 - ≤ 5,0 | |
| > 5,0 - ≤ 10,0 | |
| > 10,0 - ≤ 15,0 |
| Commodity | Weight or number of sublots | Number of incremental samples | ||
|---|---|---|---|---|
| Dried figs and other dried fruit | ≥ 15 | 15-30 tonnes | 100 | 30 |
| < 15 | — | 10-100 | ≤ 30 | |
| Groundnuts, pistachios, Brazil nuts and other nuts | ≥ 500 | 100 tonnes | 100 | 30 |
| > 125 and < 500 | 5 sublots | 100 | 30 | |
| ≥ 15 and ≤ 125 | 25 tonnes | 100 | 30 | |
| < 15 | — | 10-100 | ≤ 30 | |
| Cereals | ≥ | 500 tonnes | 100 | 30 |
| > 300 and < | 3 sublots | 100 | 30 | |
| ≥ 50 and ≤ 300 | 100 tonnes | 100 | 30 | |
| < 50 | — | 10-100 | 1-10 | |
| Spices | ≥ 15 | 25 tonnes | 100 | 10 |
| < 15 | — | 10-100 | 1-10 |
On condition that the sublot can be separated physically, each lot must be subdivided into sublots following Table 2 at point 5.1. Taking into account that the weight of the lot is not always an exact multiple of the weight of the sublots, the weight of the sublot may exceed the mentioned weight by a maximum of 20 %, each sublot must be sampled separately, number of incremental samples: 100. In the case of lots under 15 tonnes, the number of incremental samples to be taken depends on the weight of the lot, with a minimum of 10 and a maximum of 100 (see point 4.3), weight of the aggregate sample = 30 kg which has to be mixed and to be divided into three equal subsamples of 10 kg before grinding (this division into three subsamples is not necessary in the case of groundnuts, nuts, dried fruit and maize intended for further sorting or other physical treatment, however, this will depend upon the availability of equipment which is able to homogenise a 30 kg sample). In cases where the aggregate sample weights are under 10 kg, the aggregate sample must not be divided into three subsamples. In the case of spices the aggregate sample weighs not more than 10 kg and therefore no division in subsamples is necessary, laboratory sample: a subsample of 10 kg (each subsample must be separately ground finely and mixed thoroughly to achieve complete homogenisation, in accordance with the provisions laid down in 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.
For groundnuts, nuts, dried fruit and maize subjected to a sorting or other physical treatment and spices: acceptance if the aggregate sample or the average of the subsamples conforms to the maximum limit, taking into account the measurement uncertainty and correction for recovery, rejection if the aggregate sample or the average of the subsamples exceeds the maximum limit beyond reasonable doubt taking into account the measurement uncertainty and correction for recovery,
for groundnuts, nuts, dried fruit and cereals intended for direct human consumption and cereals, with the exception of maize, to be subjected to a sorting or other physical treatment: acceptance if none of the subsamples exceeds the maximum limit, taking into account the measurement uncertainty and correction for recovery, rejection if one or more of the subsamples exceeds the maximum limit beyond reasonable doubt taking into account the measurement uncertainty and correction for recovery, where the aggregate sample is under 10 kg: acceptance if the aggregate sample conforms to the maximum limit, taking into account the measurement uncertainty and correction for recovery, rejection if the aggregate sample exceeds the maximum limit beyond reasonable doubt taking into account analytical uncertainty and correction for recovery.
| Number of incremental samples | |
|---|---|
| ≤ 1 | |
| > 1 - ≤3 | |
| > 3 - ≤10 | |
| > 10 - ≤20 | |
| > 20 - ≤50 |
number of incremental samples: minimum 5, weight of aggregate sample: minimum 0,5 kg or litres.
Acceptance if the aggregate sample conforms to the maximum limit, taking into account the measurement uncertainty and correction for recovery, rejection if the aggregate sample exceeds the maximum limit beyond reasonable doubt taking into account the measurement uncertainty and correction for recovery.
Acceptance if the aggregate sample conforms to the maximum limit, taking into account the measurement uncertainty and correction for recovery, rejection if the aggregate sample exceeds the maximum limit beyond reasonable doubt taking into account the measurement uncertainty and correction for recovery.
Number of incremental samples: 100. For lots of under 50 tonnes the number of incremental samples should be 10 to 100, depending on the lot weight (see Table 3 at point 5.3.1 of this Annex), the weight of the incremental sample should be about 100 grams. In the case of lots in retail packing, the weight of the incremental sample depends on the weight of the retail packing, weight of aggregate sample = 1-10 kg sufficiently mixed.
The number of aggregate samples to be taken depends on the lot weight. The division of large lots into sublots must be done as defined for cereals in Table 2 under point 5.1, each sublot must be sampled separately.
Acceptance if the aggregate sample conforms to the maximum limit, taking into account the measurement uncertainty and correction for recovery, rejection if the aggregate sample exceeds the maximum limit beyond reasonable doubt taking into account the measurement uncertainty and correction for recovery.
Acceptance if the aggregate sample conforms to the maximum limit, taking into account the measurement uncertainty and correction for recovery, Rejection if the aggregate sample exceeds the maximum limit beyond reasonable doubt, taking into account the measurement uncertainty and correction for recovery.
shelling samples of nuts "in shell" and the level of aflatoxins is directly determined in the edible part, homogenise the nuts "in shell" by taking them through the sample preparation procedure. The sampling and analytical procedure must estimate the weight of nut kernel in the aggregate sample. The weight of nut kernel in the aggregate sample is estimated after establishing a suitable factor for the proportion of nut shell to nut kernel in whole nuts. This proportion is used to ascertain the amount of kernel in the bulk sample taken through the sample preparation and analysis procedure. Approximately 100 whole nuts are taken at random separately from the lot or are to be put aside from each aggregate sample. The ratio may, for each laboratory sample, be obtained by weighing the whole nuts, shelling and re-weighing the shell and kernel portions. However, the proportion of shell to kernel may be established by the laboratory from a number of samples and so can be assumed for future analytical work. But if a particular laboratory sample is found to be in contravention of any limit, the proportion should be determined for that sample using the approximately 100 nuts that have been set aside.
| Criterion | Concentration range | Recommended value | Maximum permitted value |
|---|---|---|---|
| Blanks | All | Negligible | |
| Recovery — Aflatoxin M1 | 0,01-0,05 μg/kg | 60 to 120 % | |
| >0,05 μg/kg | 70 to 110 % | ||
| Recovery — Aflatoxins B | < 1,0 μg/kg | 50 to 120 % | |
| 1-10 μg/kg | 70 to 110 % | ||
| >10 μg/kg | 80 to 110 % | ||
| Precision RSD | All | As derived from Horwitz equation | 2 × value derived from Horwitz equation |
Values to apply to both B 1 and sum of B1 + B2 + G1 + G2 ,if sum of individual aflatoxins B 1 + B2 + G1 + G2 are to be reported, then response of each to the analytical system must be either known or equivalent,the detection limits of the methods used are not stated as the precision values are given at the concentrations of interest, the precision values are calculated from the Horwitz equation, i. e.: RSD R = 2(1-0,5 logC) where: RSD R is the relative standard deviation calculated from results generated under reproducibility conditions [(SR /x) × 100]C is the concentration ratio (i. e. 1 = 100 g/100 g, 0,001 = 1000 mg/kg).