(1) Annex I is amended as follows: (a) In part B, footnote (1) is replaced by the following: "(1) The sampling of such lots shall be performed in accordance with the rules set out in part L. Guidance for sampling large lots shall be provided in a guidance document available on the following website: http://ec.europa.eu/food/food/chemicalsafety/contaminants/guidance-sampling-final.pdf The application of sampling rules in accordance with EN ISO 24333:2009 or GAFTA Sampling Rules 124, applied by food business operators to ensure compliance with provisions in legislation is equivalent to the sampling rules set out in part L. For the sampling of lots for Fusarium -toxins, the application of sampling rules in accordance with EN ISO 24333:2009 or GAFTA Sampling Rules 124, applied by food business operators to ensure compliance with provisions in legislation is equivalent to the sampling rules set out in part B;"(b) In part B.2, Table 1 is replaced by the following table: "Table 1 Subdivision of lots into sublots depending on product and lot weight Depending on the lot weight — see Table 2." Commodity Lot weight (tonne) Weight or number of sublots No incremental samples Aggregate sample Weight (kg) Cereals and cereal products > 300 and < 1500 3 sublots 100 10 ≥ 50 and ≤ 300 100 tonnes 100 10 < 50 — 3-100 1-10 ----------------------Depending on the lot weight — see Table 2." (c) In part B.3, the following sentence is added at the end of the first indent: "For lots > 500 tonnes, the number of incremental samples is provided for in part L.2 of Annex I." (d) In part D.2 the following sentence is added after the first sentence: "This method of sampling is of also of application for the official control of the maximum levels established for ochratoxin A, aflatoxin B1 and total aflatoxins in spices with a relatively large particle size (particle size comparable with peanuts or larger e.g. nutmeg)."; (e) In part E, the first sentence is replaced by the following: "This method of sampling is of application for the official control of the maximum levels established for ochratoxin A, aflatoxin B1 and total aflatoxins in spices except in cases of spices with a relatively large particle size (heterogeneous distribution of mycotoxin contamination)."; (f) In part I, the heading and the first sentence are replaced by the following: "I. METHOD OF SAMPLING FOR SOLID APPLE PRODUCTS This method of sampling is of application for the official control of the maximum levels established for patulin in solid apple products, including solid apple products for infants and young children." (g) In part I.1, second paragraph, the following sentences are deleted: "In case of liquid products the lot shall be thoroughly mixed insofar as possible by either manual or mechanical means immediately prior to sampling. In this case, a homogenous distribution of patulin can be assumed within a given lot. It is therefore sufficient to take three incremental samples from a lot to form the aggregate sample." (h) New Parts L and M as set out in Annex I to this Regulation, are added.
(2) In Annex II, points 4.2 "General requirements", 4.3 "Specific requirements" and 4.4 "Estimation of measurement uncertainty, recovery calculation and reporting of results" are replaced by the text set out in Annex II to this Regulation.
Commission Regulation (EU) No 519/2014 of 16 May 2014 amending Regulation (EC) No 401/2006 as regards methods of sampling of large lots, spices and food supplements, performance criteria for T-2, HT-2 toxin and citrinin and screening methods of analysis Text with EEA relevance
| Lot size (number of retail packages) | Number of retail packages to be taken for sample | Sample size |
|---|---|---|
| 1-50 | 1 | All capsules |
| 51-250 | 2 | All capsules |
| 251- | 4 | From each retail package taken for sample, half of the capsules |
| > | 4 + 1 retail package per |
(a) Performance criteria for aflatoxins Criterion Concentration Range Recommended Value Maximum permitted Value Blanks All Negligible — Recovery — Aflatoxin M1 0,01-0,05 mg/kg 60 to 120 % > 0,05 mg/kg 70 to 110 % Recovery-Aflatoxins B 1 , B2 , G1 , G2 < 1,0 mg/kg 50 to 120 % 1-10 mg/kg 70 to 110 % > 10 mg/kg 80 to 110 % Reproducibility RSD R All As derived from Horwitz Equation (*)(**) 2 × value derived from Horwitz Equation (*)(**) Repeatability RSD r may be calculated as 0,66 times Reproducibility RSDR at the concentration of interest.Note: 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.
(b) Performance criteria for ochratoxin A Level μg/kg Ochratoxin A RSD r %RSD R %Recovery % < 1 ≤ 40 ≤ 60 50 to 120 ≥ 1 ≤ 20 ≤ 30 70 to 110 (c) Performance criteria for patulin Level μg/kg Patulin RSD r %RSD R %Recovery % < 20 ≤ 30 ≤ 40 50 to 120 20-50 ≤ 20 ≤ 30 70 to 105 > 50 ≤ 15 ≤ 25 75 to 105 (d) Performance criteria for deoxynivalenol Level μg/kg Deoxynivalenol RSD r %RSD R %Recovery % > 100-≤ 500 ≤ 20 ≤ 40 60 to 110 > 500 ≤ 20 ≤ 40 70 to 120 (e) Performance criteria for zearalenone Level μg/kg Zearalenone RSD r %RSD R %Recovery % ≤ 50 ≤ 40 ≤ 50 60 to 120 > 50 ≤ 25 ≤ 40 70 to 120 (f) Performance criteria for Fumonisin B 1 and B2 individuallyLevel μg/kg Fumonisin B 1 and B2 individuallyRSD r %RSD R %Recovery % ≤ 500 ≤ 30 ≤ 60 60 to 120 > 500 ≤ 20 ≤ 30 70 to 110 (g) Performance criteria for T-2 and HT-2 toxin individually Level μg/kg T-2 and HT-2 toxin individually RSD r %RSD R %Recovery % 15-250 ≤ 30 ≤ 50 60 to 130 > 250 ≤ 25 ≤ 40 60 to 130 (h) Performance criteria for citrinin Level μg/kg Citrinin RSD r %Recommended RSD R %Maximum allowed RSD R %Recovery % All 0,66 × RSD R As derived from Horwitz Equation (*)(**) 2 × value derived from Horwitz Equation (*)(**) 70 to 120 (i) Notes to the performance criteria for the mycotoxins: The detection limits of the methods used are not stated as the precision values given at the concentrations of interest. The precision values are calculated from the Horwitz equation, in particular the original Horwitz equation (for concentrations 1,2 × 10 –7 ≤ C ≤ 0,138) (*) and the modified Horwitz equation (for concentrations C < 1,2 × 10–7 ) (**).(*) Horwitz equation for concentrations 1,2 × 10 –7 ≤ C ≤ 0,138:RSD R = 2(1-0.5logC) (ref: W. Horwitz, L.R. Kamps, K.W. Boyer, J.Assoc.Off.Analy.Chem.,1980, 63, 1344) (**) Modified Horwitz equation (*) for concentrations C < 1,2 × 10 –7 :RSD R = 22 %(ref: M. Thompson, Analyst, 2000, 125, p. 385-386) Where: RSD R is the relative standard deviation calculated from results generated under reproducibility conditions [(sR/) × 100]C is the concentration ratio (i.e. 1 = 100g/100g, 0,001 = 1000 mg/kg)
This is a generalised precision equation which has been found to be independent of analyte and matrix but solely dependent on concentration for most routine methods of analysis.
Uf is the maximum standard measurement uncertainty (μg/kg)LOD is the limit of detection of the method (μg/kg) α is a constant, numeric factor to be used depending on the value of C. The values to be used are set out in Table hereafter. C is the concentration of interest (μg/kg)
| C (μg/kg) | α |
|---|---|
| ≤ 50 | 0,2 |
| 51-500 | 0,18 |
| 501- | 0,15 |
| 0,12 | |
| > | 0,1 |
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 obtained cut-off.
A statement on calculated false suspected rate A statement on how the false suspected rate was generated.
| Commodity groups | Commodity categories | Typical representative commodities included in the category |
|---|---|---|
| High water content | Fruit Juices | Apple juice, grape juice |
| Alcoholic beverages | Wine, beer, cider | |
| Root and tuber vegetables | Fresh ginger | |
| Cereal or fruit based purees | Purees intended for infants and small children | |
| High oil content | Tree nuts | Walnut, hazelnut, chestnut |
| Oil seeds and products thereof | Oilseed rape, sunflower, cotton-seed, soybeans, peanuts, sesame etc. | |
| Oily fruits and products thereof | 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 | Wheat, rye, barley, maize, rice, oats Wholemeal bread, white bread, crackers, breakfast cereals, pasta |
| Dietary products | 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" | ||
| High sugar low water content | Dried fruits | Figs, raisins, currants, sultanas |
| Milk and milk products | Milk | Cow, goat and buffalo milk |
| Cheese | Cow, goat cheese | |
| Dairy products (e.g. milk powder) | Yogurt, cream |
| 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, the level of recovery being indicated. 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 measurement uncertainty, using a coverage factor of 2 which gives a level of confidence of approximately 95 %.
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