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BCS-RD-D-ROCS Method-No. 00857
D-40789 Monheim Report No. MR-099/04
5.2 Blank Values of Untreated Control Samples (contd)
Table 10 (contd): Origin of Control Material;
LOQ = 0.01 mg/kg for all individual analytes not expressed as parent compound.
(0.1 mg/kg for hop).
Control Material
Melon Peel
Melon Pulp
Onion Tuber
Hop Beer
Hop Cone dried
Hop Cone green
Broccoli Curd
Cauliflower
Inflorescence.
Lettuce Head
BYI08330
BYI08330enol
Residues [mg/kg]
BYI08330ketohydroxy
BYI08330monohydroxy
BYI08330enol-Glc
Control Material Melon Fruit
(Peel) 200203357 T03 K and T04
K
< 30% LOQ < 30% LOQ < 30% LOQ < 30% LOQ < 30% LOQ
Control Material Melon Fruit
200203422 T01K < 30% LOQ < 30% LOQ < 30% LOQ < 30% LOQ < 30% LOQ
Control Material 200305575 Mix
of T01 K and T02 K < 30% LOQ < 30% LOQ < 30% LOQ < 30% LOQ < 30% LOQ
Control Material Warsteiner
Premium Verum < 30% LOQ < 30% LOQ < 30% LOQ < 30% LOQ < 30% LOQ
Control Material Hop Cone dried
1999 00368/376/381/392 < 30% LOQ < 30% LOQ < 30% LOQ < 30% LOQ < 30% LOQ
Control Material Hop Cone green
1999 00368/376/381/392 < 30% LOQ < 30% LOQ < 30% LOQ < 30% LOQ < 30% LOQ
Control Material
R 2003 0114/6 UP0006 21 C < 30% LOQ < 30% LOQ < 30% LOQ < 30% LOQ < 30% LOQ
Control Material
R 2003 0162/6 UP0003 21 C < 30% LOQ < 30% LOQ < 30% LOQ < 30% LOQ < 30% LOQ
Control Material
R 2002 0008/0 UP0003 7 C < 30% LOQ < 30% LOQ < 30% LOQ < 30% LOQ < 30% LOQ
Remarks: If matrix effects were observed, slight deviations in the chromatographic and MS/MS conditions were used. Onion
(tuber) covers onion (onion).
5.3 Linearity of the Detector
The linearity of the detector was tested using solvent standards. The peak are ratio of
analyte/internal standard was quoted and a linear regression was performed.
The linearity was tested by triplicate injections of solvent standards at concentrations
between 5 ng/L and 50 µg/L for each analyte. The concentration of the corresponding
stable isotopically labelled internal standards was 1.0 µg/L for each analyte and in all
standard solutions.
Table 11: Standard Concentrations prepared for the Determination of Detector Linearity.
Unlabelled
[BYI], [Enol], [Ketohydroxy],
[Mono-hydroxy], [Gluco]
Stable-Labelled
[BYI- 13 C], [Enol- 13 C],
[Ketohydroxy- 13 C], [Monohydroxy-
13 C], [Gluco- 13 C]
0.005
each
1
each
0.01
each
1
each
0.05
each
1
each
Standard Concentrations [µg/L]
0.1
each
1
each
A linear correlation between the injected amount of substance and the detector
response was observed for standards in solvent (5 ng/L to 50 µg/L). The correlation
coefficients of the 1/x weighted linear regression were ranging from 0.9976 to 0.9995.
For representative linearity plots see Appendix 3.
0.5
each
1
each
1
each
1
each
2
each
1
each
5
each
1
each
10
each
1
each
50
each
1
each