nm802nm259nm283128141( erusserP fooitaR*nm322nm791339223 Poymer-basedReversedPhase Chromatography Coumns (12341234312050505)% 01i.i.i.i.4i.501230123 ll )ODP2HPColumn Eluent Flow rate Detector Column temp. : 40 ˚C: Shodex ODP2 HP-4D : H2O/CH3CN = 55/45: 0.6 mL/min: UV (254 nm)ODP2 HP columns are packed with gels with increased surface polarity and smaller pore size which prevent the adsorption of proteins.BSA was injected multiple times to both ODS and ODP2 HP columns. A signi■cant column pressure increase was observed for the ODS column, while no considerable change was observed for the ODP2 HP column even after 140 injections.ODS column(2.0 mm I.D. × 50 mm)ODP2 HP-2B (2.0 mm I.D. × 50 mm)Column Eluent Flow rate Detector Column temp. : 30 ˚C: Shodex ODP2 HP-2B ODS column from other manufacturer: 1 mM CH3COONH4 aq./CH3CN = 90/10: 0.2 mL/min: UV (220 nm)ODP2 HP-2B(2.0 mm I.D. x 50 mm)Sample : 5 µL1. Phenol 300 mg/L2. Methyl benzoate 350 mg/L3. Toluene 1000 mg/L150 mg/L4. Naphthalene 160Sample : 5 µLBSA 7.0 mg/mL150140130120110100902040BarbitalPeak area : 100 %Barbital 500 ng/mL in BSA 7.0 mg/mLBarbitalPeak area : 99 %TP : 11,40010 min6080100120Number of Injection*Considering original pressure as 100 %Barbital 500 ng/mL4 minTP : 5,70010 min140Barbital 500 ng/mLBarbitalPeak area : 100 %Barbital 500 ng/mL in BSA 7.0 mg/mLBarbitalPeak area : 71 %4 minColumn Eluent Flow rate Detector Column temp. : 40 ˚C: Shodex ODP2 HP-4E : 10 mM Na2HPO4 aq./CH3CN = 90/10: 0.8 mL/min: UV (220 nm)Sample pretreatment:Mix the same volumes of serum and acetonitrile. Centrifuge the mixture at 6000 x g for 5 minutes. Use the supernatant as sample. : Shodex ODP2 HP-4E: 25 mM Sodium phosphate buffer (pH5.2)/CH3CN = 680/320: 0.35 mL/min: UV (210 nm)LC/MS analysis of drugs in biological samples is often interfered by ion suppression caused by presence of protein when using general ODS columns. However, ODP2 HP does not retain proteins and elutes them at the void volume. Thus, elution of barbital is not affected when using the ODP2 HP and provides better recovery rate than that of an ODS column. : Shodex ODP2 HP-2B ODS column from other manufacturer: 10 mM CH3COONH4 aq. /CH3CN = 70/30: 0.2 mL/min: ESI-MS (SIM Negative: m/z 183)Column Eluent Flow rate Detector Column temp. : 30 ˚CInjection vol. : 10 µLSample : 0.1 % each, 10 µL1. Imidazole2. 2-Methylimidazole3. 4-Methylimidazole Sample : 20 µL 1. 2-Acetaminophenol (I.S.) 10 µg/mL 13.0 µg/mL2. Zonisamide 19.0 µg/mL3. Phenobarbital 4.5 µg/mL4. Carbamazepine 5. Phenytoin 9.0 µg/mLData provided by Katsuko Hara.MT Yutaka Komiyama .Ph.D., Department of Clinical Sciences and Laboratory Medicine, Kansai Medical University.10 minComparison between ODP2 HP and ODP-50Influence of repeated protein injection on column pressureComparison of barbital recovery rate using ODP2 HP-2B and ODS in the presence of BSAImidazolesAnticonvulsant in serumODP2 HP-4DColumn Eluent Flow rate Detector Column temp. : 40 ˚C: Shodex Asahipak ODP-50 4D : H2O/CH3CN = 35/65: 0.6 mL/min: UV (254 nm)ODS column(2.0 mm I.D. x 50 mm)ODP-50 4DColumn Eluent Flow rate Detector Column temp. : 40 ˚C13
元のページ ../index.html#15