<strong>Bayer</strong> <strong>CropScience</strong> <strong>AG</strong> <strong>Page</strong> 42 <strong>of</strong> <strong>82</strong> <strong>BCS</strong>-<strong>RD</strong>-D-ROCS Method-No. 00857 D-40789 Monheim Report No. MR-099/04 5.6 Stability in Standard and Stock Solution The stability <strong>of</strong> BYI08330 and its metabolites BYI08330-enol, BYI08330-ketohydroxy, BYI08330-mono-hydroxy and BYI08330-enol-Glc in stock and standard solutions was tested. For this purpose aged standard and stock solutions were quantified against freshly prepared standard solutions. The aged solutions were stored in volumetric flasks. Fresh solutions were mostly prepared at the date <strong>of</strong> analysis. The results indicate that all analytes are stable in standard solutions for at least four weeks <strong>of</strong> storage in a refrigerator at 4°C ± 3°C under dark conditions. Remark: All standard solutions should be prepared in solvent mixtures (acetonitrile/water; 2/8, v/v containing 0.22 mL/L formic acid and acetonitrile/water; 15/85, v/v containing 0.22 mL/L formic acid, respectively). To reduce the oxygen content which is supposed to degrade the BYI08330-enol solutions can be degassed with helium. 6 References [1] Methodensammlung der Arbeitsgruppe Analytik, Deutsche Forschungsgemeinschaft Rückstandsanalytik von Pflanzenschutzmitteln, Mitteilung VI der Senatskommission für Pflanzenschutz-, Pflanzenbe-handlungs- und Vorratsschutzmittel, VCH Verlagsgesellschaft, Weinheim; Deerfield Beach, Florida; Basel, 1. bis 11. Auflage 1991. Translation: Method compilation from the working group Analytics, German Research Association Residue Analysis <strong>of</strong> Crop Protection Products, Note VI <strong>of</strong> the Senate Commission for pesticides, crop treatment products and products for stored commodities , VCH publishers, Weinheim; Deerfield Beach, Florida; Basel, 1. bis 11. edition 1991. [2] Besondere Schutzmaßnahmen in Laboratorien, Merkblatt M 006 6/89, [3] Berufsgenossenschaft der chemischen Industrie, Jedermann-Verlag Dr. Otto Pfeffer oHG, Heidelberg, 1989. Translation: Special Protective Measures in Laboratories, Note M 006 6/89, Employees' Liability Insurance Association, Jedermann publishers Dr. Otto Pfeffer oHG, Heidelberg, 1989. Verordnung zum Schutz vor gefährlichen St<strong>of</strong>fen (Gefahrst<strong>of</strong>fverordnung, GefSt<strong>of</strong>fV) vom 26. Oktober 1993 (BGB I.I S. 17<strong>82</strong>), zuletzt geändert durch die Erste Verordnung zur Änderung chemikalienrechtlicher Verordnungen vom 12. Juni 1996 sowie durch das Gesetz zur Beschleunigung und Vereinfachung immissionsrechtlicher Genehmigungsverfahren vom 9. Oktober 1996, Carl Heymanns Verlag, Köln, 13. Auflage 1999. Translation: Regulation on protection against dangerous materials (Dangerous Material Act) from October 26, 1993 (BGB I.I S. 17<strong>82</strong>), last updated by the First regulation amending chemical law regulations from June 12, 1996 and the law for the acceleration and simplification <strong>of</strong> emmission law approval procedures from October 9, 1996, Carl Heymanns publishers, Cologne, 13th edition 1999. [4] Guidance for generating and reporting methods <strong>of</strong> analysis in support <strong>of</strong> pre-registration data requirements for Annex II (part A, Section 4) and Annex III (part A, Section 5) <strong>of</strong> Directive 91/414 (working document), European Commission, Directorate General Health and Consumer Protection, SANCO/3029/99 rev. 4, 2000-07-11. I
<strong>Bayer</strong> <strong>CropScience</strong> <strong>AG</strong> <strong>Page</strong> 43 <strong>of</strong> <strong>82</strong> <strong>BCS</strong>-<strong>RD</strong>-D-ROCS Method-No. 00857 D-40789 Monheim Report No. MR-099/04 Appendix 1: Representative Chromatograms BYI08330 (0.1 µg/L; top), BYI08330 (0.1 µg/L, 2 nd MRM) and BYI08330- 13 C3 (1 µg/L; bottom)