Division C.3.3.1 Performance criteriaF1

Where no specific methods for the determination of contaminants in foodstuffs are prescribed F2..., laboratories may select any validated method of analysis for the respective matrix provided that the selected method meets the specific performance criteria set out in Tables 5, 6 and 7.

It is recommended that fully validated methods (i.e. methods validated by collaborative trial for the respective matrix) are used where appropriate and available. Other suitable validated methods (e.g. in-house validated methods for the respective matrix) may also be used provided that they fulfil the performance criteria set out in Tables 5, 6 and 7.

Where possible, the validation of in-house validated methods shall include a certified reference material.

1. (a)

   F3Performance 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 2
   Reproducibility (RSD R )	HORRAT R less than 2
   Recovery	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

2. (b)

   F4Performance criteria for methods of analysis for 3-monochloropropane-1,2-diol (3-MCPD), 3-MCPD fatty acid esters and glycidyl fatty acid esters:

   • Performance criteria for methods of analysis for 3-MCPD in foods specified in point 4.1 of the Annex to Regulation (EC) No 1881/2006

     Table 6a

     Parameter	Criterion
     Applicability	Foods specified in point 4.1 of the Annex to 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 equation
     Reproducibility (RSD R )	as derived from (modified) Horwitz equation
     Recovery	75-110 %
     Limit of Detection (LOD)	≤ 5 μg/kg (on dry matter basis)
     Limit of Quantification (LOQ)	≤ 10 μg/kg (on dry matter basis)

   • Performance criteria for methods of analysis for 3-MCPD in foods specified in point 4.3 of the Annex to Regulation (EC) No 1881/2006

     Table 6b

     Parameter	Criterion
     Applicability	Foods specified in point 4.3 of the Annex to 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 equation
     Reproducibility (RSD R )	as derived from (modified) Horwitz equation
     Recovery	75-110 %
     Limit of Detection (LOD)	≤ 7 μg/kg
     Limit of Quantification (LOQ)	≤ 14 μg/kg

   • Performance criteria for methods of analysis for 3-MCPD fatty acid esters, expressed as 3-MCPD , in foods specified in point 4.3 of the Annex to Regulation (EC) No 1881/2006

     Table 6c

     Parameter	Criterion
     Applicability	Foods specified in point 4.3 of the Annex to Regulation (EC) No 1881/2006
     Specificity	Free from matrix or spectral interferences
     Repeatability (RSD r )	0,66 times RSD R as derived from (modified) Horwitz equation
     Reproducibility (RSD R )	as derived from (modified) Horwitz equation
     Recovery	70-125 %
     Limit of Detection (LOD)	Three tenths of LOQ
     Limit of Quantification (LOQ) for foods specified in 4.3.1 and 4.3.2	≤ 100 μg/kg in oils and fats
     Limit of Quantification (LOQ) for foods specified in 4.3.3 and in 4.3.4 with a fat content < 40 %	≤ two fifths of the ML
     Limit of Quantification (LOQ) for foods specified in 4.3.4 with a fat content ≥ 40 %	≤ 15 μg/kg fat

   • Performance criteria for methods of analysis for glycidyl fatty acid esters, expressed as glycidol, in foods specified in point 4.2 of the Annex to Regulation (EC) No 1881/2006

     Table 6d

     Parameter	Criterion
     Applicability	Foods specified in point 4.2 of the Annex to Regulation (EC) No 1881/2006
     Specificity	Free from matrix or spectral interferences
     Repeatability (RSD r )	0,66 times RSD R as derived from (modified) Horwitz equation
     Reproducibility (RSD R )	as derived from (modified) Horwitz equation
     Recovery	70-125 %
     Limit of Detection (LOD)	Three tenths of LOQ
     Limit of Quantification (LOQ) for foods specified in 4.2.1 and 4.2.2	≤ 100 μg/kg in oils and fats
     Limit of Quantification (LOQ) for foods specified in 4.2.3 with a fat content < 65 % and in 4.2.4 with a fat content < 8 %	≤ two fifths of the ML
     Limit of Quantification (LOQ) for foods specified in 4.2.3 with a fat content ≥ 65 % and in 4.2.4 with a fat content ≥ 8 %	≤ 31 μg/kg fat

3. (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 2
   Reproducibility (RSD R )	HORRAT R less than 2
   Recovery	50-120 %
   LOD	≤ 0,30 μg/kg for each of the four substances
   LOQ	≤ 0,90 μg/kg for each of the four substances

4. (d)

   Performance criteria for methods of analysis for acrylamide:

   Table 8

   Parameter	Criterion
   Applicability	All foods
   Specificity	Free from matrix or spectral interferences
   Field blanks	Less than Limit of Detection (LOD)
   Repeatability (RSD r )	0,66 times RSD R as derived from (modified) Horwitz equation
   Reproducibility (RSD R )	as derived from (modified) Horwitz equation
   Recovery	75-110 %
   Limit of Detection (LOD)	Three tenths of LOQ
   Limit of Quantification (LOQ)	For foods with benchmark levels < 125 μg/kg: ≤ two fifths of the benchmark level, however not required to be lower than 20 μg/kg For foods with benchmark level ≥ 125 μg/kg: ≤ 50 μg/kg

5. (e)

   F5Performance criteria for methods of analysis for perchlorate:

   Table 9

   Parameter	Criterion
   Applicability	All foods
   Specificity	Free from matrix or spectral interferences
   Repeatability (RSD r )	0,66 times RSD R as derived from (modified) Horwitz equation
   Reproducibility (RSD R )	as derived from (modified) Horwitz equation
   Recovery	70-110 %
   Limit of Detection (LOD)	Three tenths of LOQ
   Limit of Quantification (LOQ)	≤ two fifths of the ML

6. (f)

   Notes to the performance criteria:

   The Horwitz equation^f1 (for concentrations 1,2 x 10 ^-7 ≤ C ≤ 0,138) and the modified Horwitz equation^f2 (for concentrations C < 1,2 × 10 ^-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

   • C is the concentration ratio (i.e. 1 = 100g/100g, 0,001 = 1 000 mg/kg). The modified Horwitz equation applies to concentrations C < 1,2 × 10 ^-7 .

   Horwitz equation for concentrations 1,2 x 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

   • C is the concentration ratio (i.e. 1 = 100g/100g, 0,001 = 1 000 mg/kg). The Horwitz equation applies to concentrations 1,2 x 10 ^-7 ≤ C ≤ 0,138.