C2H589 Poymer-basedReversedPhase Chromatography Coumns (1234532112313200001342582154305050556423171234567890l liAsahpak)MWRecovery(%)9711881060925749716739955610013489314508157503496959114300961479961750083Column Eluent Flow rate Detector Column temp. : 30 ˚C: Shodex Asahipak ODP-50 4D : 10 mM NaOH aq. (pH12.0)/CH3CN = 35/65 : 0.6 mL/min : UV (254 nm)Column Eluent Flow rate Detector Column temp. : 40 ˚C: Shodex Asahipak ODP-50 4D: 0.1 % H3PO4 in (H2O/CH3CN = 30/70): 1.0 mL/min: UV (215 nm)Column Eluent Flow rate Detector Column temp. : 40 ˚C: Shodex Asahipak ODP-50 4E: 6.7 g/L Dibasic potassium phosphate aq. (pH11.0 adjusted with 10 M KOH) /CH3CN = 40/60: 1.0 mL/min: UV (210 nm)10Sample : 0.002 % each (in Ethanol), 5 µL1. EPA (Eicosapentaenoic acid)2. α-Linolenic acid 3. DHA (Docosahexaenoic acid) 4. Arachidonic acid 5. Linoleic acidSample : 10 LStandard solutionSystem suitability solutionAzaerythromycin ASample : 1. Acetophenone2. Butyrophenone3. Hexanophenone4. Heptanophenone5. Octanophenone330 hr230 hr90 hr0 hr20 min1015minAzithromycin(0.53 mg/mL)Azithromycin(0.5 mg/mL)(0.5 mg/mL)Rs > 6.01015minDissociation of tertiary amino groups in basic drugs can be suppressed by making pH of the eluent higher than pKa of the amino groups. This increases the relative hydrophobicity of the basic drugs, thereby allowing the column to retain the drugs stronger and provide baseline separation of them.Column Eluent Flow rate Detector Column temp. : 30 ˚C : Shodex Asahipak ODP-50 4D: 25 mM Phosphate buffer/CH3CN = 60/40: 0.6 mL/min : UV (254 nm) Column Eluent Flow rate Detector Column temp. : 30 ˚C: Shodex Asahipak ODP-50 4E : CH3CN/CH3OH = 50/50: 0.6 mL/min: UV (280 nm)20 min1020 % CH3CNColumn Eluent Flow rate Detector Column temp. : 30 ˚C: Shodex Asahipak ODP-50 6D : (A); 0.05 % TFA aq./CH3CN = 80/20 (B); 0.05 % TFA aq./CH3CN = 50/50 Linear gradient; (A) to (B), 20 min: 1.0 mL/min: UV (220 nm)20 min20 minSample : 20 µL1. Vitamin K3 2. Vitamin A 3. Vitamin A acetate 4. Vitamin D2 5. Vitamin D3 6. Vitamin E acetate 7. Vitamin E 8. Vitamin K1 671520Sample : 40 µL1011121020 min50 % CH3CNNo.SampleLys-BradykininBradykininMet-EnkephalinNeurotensinSubstance PLeu-EnkephalinBacitracinInsulinInsulin B chain10Lysozyme11Mastoparan12MyoglobinSample :1. BenzocaineCOOC2H52. LidocaineCH3NHCOCH2NCH33. TetracaineCOOCH2CH2NCH3CH3NH(CH2)3CH31.5 µg/mL0.3 µg/mL1.9 µg/mL0.3 µg/mL0.3 µg/mL2.4 µg/mL2.5 µg/mL2.4 µg/mL 25 minH2NC2H5Alkaline tolerance of ODP-50Unsaturated fatty acidsAnalysis of azithromycin according to USP-NF methodGradient analysis of proteins and peptidesLocal anestheticsFat-soluble vitaminspH3pH7pH1115
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