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Bayer CropScience AG Page 28 of 82 BCS-RD-D-ROCS Method-No. 00857 D-40789 Monheim Report No. MR-099/04 4.3.6 MS/MS Conditions (contd) Table 8: MS/MS Parameters for Determination of BYI08330-enol-Glc for the single deter-mination in cases of interferences (e.g. in orange). Precursor Ion Q1 Mass (amu) Product Ion Q3 Mass (amu) Dwell Time (msec) Collision Energy (eV) BYI08330-enol-Glc 1 st MRM 464 270 400 45 BYI08330-enol-Glc 2 nd MRM* 464 216 200 53 BYI08330-enol-Glc 13 C3 467 273 400 45 Different MS/MS-instruments may result in different MRM transitions. *: These transitions were used for confirmation. Table 9: MS/MS Parameters for Determination of BYI08330 for the single determination in cases of interferences (e.g. in mandarin). Precursor Ion Q1 Mass (amu) Product Ion Q3 Mass (amu) Dwell Time (msec) Collision Energy (eV) BYI08330 1 st MRM 374 216 500 47 BYI08330 2 nd MRM* 374 302 100 23 BYI08330 13 C3 377 219 400 47 Note: Different MS/MS-instruments may result in different MRM transitions. *: These transitions were used for confirmation. 4.3.7 Analytical Procedure 1. Transfer a prepared aliquot of the sample extract into a HPLC vial (sample solution). 2. Inject e.g. 10 µL (or 50 µL) of standard solution using the described HPLC, MS/MS and data acquisition conditions (bracketing standard). 3. Inject e.g. 10 µL (or 50 µL) of the sample solution of step 1. (The number of injections between the bracketing standard injections should not be higher than 10.) 4. Repeat 2. 5. Compare the peak area ratios of analyte/internal standard for the bracketing standard before and after each sample set. If there is a variation of < ± 10% between the bracketing standards the analysis should be repeated. 6. Calculate the residues as described in the following paragraphs.
Bayer CropScience AG Page 29 of 82 BCS-RD-D-ROCS Method-No. 00857 D-40789 Monheim Report No. MR-099/04 4.4 Calculation The residues and recovery rates are given as single values for each analyte. To calculate the total residue of BYI08330 parent, the individual residues of BYI08330-enol, BYI08330-ketohydroxy, BYI08330-mono-hydroxy and BYI08330-enol-Glc are recalculated with conversion factors (CF) as BYI08330 parent equivalents. The following conversion factors are used: Analyte Molecular Weight M [g/mol] Conversion Factor CF* BYI08330 373.45 1.000 BYI08330-enol 301.39 1.239 BYI08330-ketohydroxy 317.38 1.177 BYI08330-mono-hydroxy 303.40 1.231 BYI08330-enol-Glc 463.52 0.806 *: C F = M BYI08330/M Analyte The individual residues of BYI08330 and its metabolites expressed as BYI8330 parent equivalents are added to calculate the total residue of BYI08330.
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