Commission Regulation (EC) No 333/2007 of 28 March 2007 laying down the methods of sampling and analysis for the official control of the levels of lead, cadmium, mercury, inorganic tin, 3-MCPD and benzo(a)pyrene in foodstuffs (Text with EEA relevance )
Modified by
- Commission Regulation (EU) No 836/2011of 19 August 2011amending Regulation (EC) No 333/2007 laying down the methods of sampling and analysis for the official control of the levels of lead, cadmium, mercury, inorganic tin, 3-MCPD and benzo(a)pyrene in foodstuffs(Text with EEA relevance), 32011R0836, August 20, 2011
- Commission Regulation (EU) 2016/582of 15 April 2016amending Regulation (EC) No 333/2007 as regards the analysis of inorganic arsenic, lead and polycyclic aromatic hydrocarbons and certain performance criteria for analysis(Text with EEA relevance), 32016R0582, April 16, 2016
Lot weight (ton) | Weight or number of sublots |
---|---|
≥ | 500 tonnes |
> 300 and < | 3 sublots |
≥ 100 and ≤ 300 | 100 tonnes |
< 100 | — |
Lot weight (ton) | Weight or number of sublots |
---|---|
≥ 15 | 15-30 tonnes |
< 15 | — |
Weight or volume of lot/sublot (in kg or litre) | Minimum number of incremental samples to be taken |
---|---|
< 50 | |
≥ 50 and ≤ 500 | |
> 500 |
Number of packages or units in the lot/sublot | Number of packages or units to be taken |
---|---|
≤ 25 | at least 1 package or unit |
26-100 | about 5 %, at least 2 packages or units |
> 100 | about 5 %, at maximum 10 packages or units |
(a) Performance criteria for methods of analysis for lead, cadmium, mercury, inorganic tin and inorganic arsenic Table 5 Parameter Criterion Applicability Foods specified in Regulation (EC) No 1881/2006 Specificity Free from matrix or spectral interferences Repeatability (RSD r )HORRAT r less than 2Reproducibility (RSD R )HORRAT R less than 2Recovery The provisions of point D.1.2 apply LOD = three tenths of LOQ LOQ Inorganic tin ≤ 10 mg/kg Lead ML ≤ 0,01 mg/kg 0,01 < ML ≤ 0,02 mg/kg 0,02 < ML < 0,1 mg/kg ML ≥ 0,1 mg/kg ≤ ML ≤ two thirds of the ML ≤ two fifths of the ML ≤ one fifth of the ML Cadmium, mercury, inorganic arsenic ML is < 0,100 mg/kg ML is ≥ 0,100 mg/kg ≤ two fifths of the ML ≤ one fifth of the ML (b) Performance criteria for methods of analysis for 3-MCPD: Table 6 Parameter Criterion Applicability Foods specified in Regulation (EC) No 1881/2006 Specificity Free from matrix or spectral interferences Field blanks Less than LOD Repeatability (RSD r )0,66 times RSD R as derived from (modified) Horwitz equationReproducibility (RSD R )as derived from (modified) Horwitz equation Recovery 75-110 % LOD ≤ 5 μg/kg (on dry matter basis) LOQ ≤ 10 μg/kg (on dry matter basis) (c) Performance criteria for methods of analysis for polycyclic aromatic hydrocarbons: The four polycyclic aromatic hydrocarbons to which these criteria apply are benzo(a)pyrene, benz(a)anthracene, benzo(b)fluoranthene and chrysene. Table 7 Parameter Criterion Applicability Foods specified in Regulation (EC) No 1881/2006 Specificity Free from matrix or spectral interferences, verification of positive detection Repeatability (RSD r )HORRAT r less than 2Reproducibility (RSD R )HORRAT R less than 2Recovery 50-120 % LOD ≤ 0,30 μg/kg for each of the four substances LOQ ≤ 0,90 μg/kg for each of the four substances (d) Notes to the performance criteria: The Horwitz equation (for concentrations 1,2 × 10W. Horwitz, L.R. Kamps, K.W. Boyer, J.Assoc.Off.Analy.Chem.,1980, 63, 1344. –7 ≤ C ≤ 0,138) and the modified Horwitz equation (for concentrations C < 1,2 × 10M. Thompson, Analyst, 2000, p. 125 and 385-386. –7 ) are generalised precision equations which are independent of analyte and matrix but solely dependent on concentration for most routine methods of analysis.Modified Horwitz equation for concentrations C < 1,2 × 10 –7 :RSD R = 22 %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 = 100 g/100 g, 0,001 = 1000 mg/kg). The modified Horwitz equation applies to concentrations C < 1,2 × 10–7 .
Horwitz equation for concentrations 1,2 × 10 –7 ≤ C ≤ 0,138:RSD R = 2C(–0,15) 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 = 100 g/100 g, 0,001 = 1000 mg/kg). The Horwitz equation applies to concentrations 1,2 × 10–7 ≤ C ≤ 0,138.
Uf is the maximum standard measurement uncertainty (μg/kg). LOD is the limit of detection of the method (μg/kg). The LOD must meet the performance criteria set in point C.3.3.1 for the concentration of interest. C is the concentration of interest (μg/kg); α is a numeric factor to be used depending on the value of C. The values to be used are given in Table 8.
C (μg/kg) | α |
---|---|
≤ 50 | |
51-500 | |
501- | |
> |