ANNEX
The Annex to Regulation (EC) No 333/2007 is amended as follows:
(1)
in point C.3.1, Definitions, the definitions of ‘LOD’ and ‘LOQ’ are replaced by the following:
‘“LOD” = Limit of detection, smallest measured content, from which it is possible to deduce the presence of the analyte with reasonable statistical certainty.
“LOQ” = Limit of quantification, lowest content of the analyte which can be measured with reasonable statistical certainty.’;
(2)
in point C.3.3.1, Performance criteria, point (b) is replaced by the following:
‘(b)
Performance 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)
in point C.3.3.1, Performance criteria, point (d), ‘Notes to the performance criteria’ is replaced by the following:
‘(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’
(4)
in point C.3.3.1, Performance criteria, the following points (e) and (f) are added:
‘(e)
Performance 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
(f)
Notes to the performance criteria:
The Horwitz equation ( *1 ) (for concentrations 1,2 x 10 -7 ≤ C ≤ 0,138) and the modified Horwitz equation ( *2 ) (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.
( *1 ) W. Horwitz, L.R. Kamps, K.W. Boyer, J.Assoc.Off.Analy.Chem.,63, 1980, 1344-1354."
( *2 ) M. Thompson, Analyst, 125, 2000, 385-386.’
"
(5)
in point C.3.3.2., ‘Fitness-for-purpose’ approach, the words ‘Table 8’ are replaced by the words ‘Table 10’.
( *1 ) W. Horwitz, L.R. Kamps, K.W. Boyer, J.Assoc.Off.Analy.Chem.,63, 1980, 1344-1354.
( *2 ) M. Thompson, Analyst, 125, 2000, 385-386.’
’
