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Bayer CropScience AG Page 16 of 82 BCS-RD-D-ROCS Method-No. 00857 D-40789 Monheim Report No. MR-099/04 4.1 Materials 4.1.1 Apparatus • Liquid chromatograph, e.g. Agilent 1100 column compartment G1316A, Agilent 1100 binary pump G1312A, Agilent 1100 iso pump G1313A, Agilent 1100 degasser G1379A, Agilent Technologies, Böblingen, Germany • Autosampler, e.g. HTC PAL, CTC Analytics, Schwitzerland • Mass spectrometer, e.g. API 4000 with ESI interface and mass spectrometric detector, Applied Biosystems, Darmstadt, Germany • Blender, e.g. Polytron (Kinematica GmbH) • Reversed phase chromatography column, e.g. Agilent, Zorbax, Eclipse XDB-C8, 150 x 4.60 mm, 5 µ with pre-column Phenomenex C18 ODS 4x3 mm, AJO-4287 in cartridge KJO-4282 • Vacuum manifold, e.g. VacElut SPS 24, Varian, Darmstadt, Germany • Reservoir 60 mL, e.g. BondElut reservoir, Varian, Darmstadt, Germany • Volumetric flask, 10-mL, 100-mL • Variable dispenser, 10-mL, 50-mL, 100-mL • Glass beaker, 150-mL • Gilson Microman pipettes, 250 µL • Calibrated pipettes, 0.5-mL, 1-mL, 10-mL, 20-mL, e.g. Brand Co., Wertheim, Germany • Bond Elut Clean Polyethylene Frits (Frits 60-mL, 1-1/16, 20µm, Varian, Part. No. 12131024 • Small instruments, e.g. Pasteur pipettes, autosampler vials, filter frits for reservoir • 0.45 µm single use filter e.g. Sartorius Minisart RC15 (order no. 17762) 4.1.2 Reagents/Supplies • Acetonitrile for chromatography, e.g. LiChrosolv Merck KGaA, Darmstadt, Germany • Water, HPLC grade, e.g. purified with a milli-Q-water system, Millipore Co., Eschborn, Germany • Acetic acid, Suprapur, e.g. Merck KGaA, Darmstadt, Germany • Formic Acid, extra pure, e.g. Riedle-de Häen, Seelze, Germany • Filter aid, e.g. Celite 545, e.g. Merck KGaA, Darmstadt, Germany • Nitrogen 5.0, 99.9990% purity, as bath, nebulizer, collision, curtain, and turbo gas, e.g. Linde AG, Höllriegelskreuth, Germany
Bayer CropScience AG Page 17 of 82 BCS-RD-D-ROCS Method-No. 00857 D-40789 Monheim Report No. MR-099/04 4.1.3 Reference Items Generally, only sufficiently characterised and certified substances are used as reference items. Table 1: Reference Items. Names in Brackets [ ] designate the Terms used in the Raw Data. Certificate of Analysis Purity (%) Expiry Date BYI08330 (a.s.) [BYI] AZ 10811 99.2 2005-07-24 BYI08330 13 C3 [BYI- 13 C] KML 3386-1-2 95.1 --- BYI08330-enol [Enol] AZ 10531 99.4 2005-02-26 BYI08330-enol 13 C3 [Enol- 13 C] KML 3384-1-1 96.3 --- BYI08330-ketohydroxy [Ketohydroxy] AZ 10832 95.3 2005-06-14 BYI08330-ketohydroxy 13 C3 [Ketohydroxy- 13 C] KML 3387-1-8 99.4 --- BYI08330-mono-hydroxy [Mono-hydroxy] AZ 11484 99.8 2006-04-06 BYI08330-mono-hydroxy 13 C3 [Mono-hydroxy- 13 C] KML 3388-1-16 93.7 --- BYI08330-enol-Glc [Gluco] AZ 11879 99.7 2006-08-04 BYI08330-enol-Glc 13 C3 [Gluco- 13 C] KML 3405-1-8 99 ---
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