ACCLAIM oa - Cromlab

Pharmaceutical Applications00–24 mAU FS12 3 4 5 6 9 100–400 mAU FSBudesonide and Related Substances0 5 10 15 20MinutesReference: Hou S, Hindle M, Byron PR;J. Pharm. Biomed. Analy. 2001 24:371-80.78Column: Acclaim 300 C18, 3 µm,4.6 x 150 mmPump: Summit P580 HPG/4Mobile Phase: (A) Acetonitrile:ethanol 15:1(B) 0.1% phosphoric acidIsocratic 66% BFlow: 1.0 mL/minTemperature: 30 °CInjection: ASI-100 autosampler, 15 µLDetector: UVD 340U; UV at 240 nmSample: Budesonide, 500 µg/mLafter three daysPeaks: 7, 8. Budesonide epimers, 99%215230.14AU0.00Hydrocortisone in Skin Ointment120 246Minutes3Column: Acclaim 120 C8, 3 µm,4.6 × 150 mmPump: Dionex GP50 microboreMobile Phase: Acetonitrile:water 49:51Flow: 1.0 mL/minTemperature: 30 °CInjection: 1 µLDetector: AD-20; UV at 245nmSample Prep.:– Disperse 100 mg of ointment in7.0 mL denatured ethanol– Mix in 3.0 mL hexane then 1.0 mL water– Centrifuge to separate emulsion– Filter ethanol layerPeaks: 1. Hydrocortisone 1.05% (label 1.0%)2. Methyl paraben 0.32%3. Propyl paraben 0.21%2152660mAU01Barbiturates on Acclaim 120 C180.0 1.5 3.0 4.5 6.0 7.5Minutes2345Column: Acclaim 120 C18 5µm, 4.6 x 50 mmPump: Summit P580 HPG/4Mobile Phase: (A) Acetonitrile:methanol 4:1 v:v(B) 0.1% phosphoric acidGradient: Time 0.0 5.0 7.5%A 20 45 45%B 80 55 55Flow: 1.0 mL/minTemperature: 30 °CInjection: ASI-100 autosampler, 3 µLDetector: UVD 340U, UV at 210 nmSample: 25 µg/mL each in methanolPeaks: 1. Barbital2. Phenobarbital3. Butabarbital4. Amobarbital5. Secobarbital215210.8AU012Active Ingredients in Cough Syrup30 5 10 15Minutes4Column: Acclaim PA2, 5 µmDimensions: 4.6 × 150 mmMobile Phase: Acetonitrile/50 mM phosphate buffer,pH 1.9 from 10/90 to40/60 (v/v) in 15 minTemperature: 30 °CFlow Rate: 1.0 mL/minInj. Volume: 20 µLDetection: UV, 210 nmPeaks: 1. Doxylamine2. Pseudo-ephedrine3. Acetaminophen4. Dextromethorphan211360.3AU001Antidepressants on Acclaim PA22Column: Acclaim PA2, 5µmDimensions: 4.6 × 150 mmMobile Phase: MeOH/10 mM triethylamine,pH 10.8, v/v 75/25Temperature: 30 °CFlow Rate: 1.0 mL/minInj. Volume: 5 µLDetection: UV, 254 nmPeaks: Concentration Asymmetry(µg/mL) (EP)1. Uracil 10 1.082. Doxepin 100 1.1433. Imipramine 80 1.1544. Amitriptyline 100 1.115 101520MinutesPhenytoin and Related Substances100Column: Acclaim 120, C18 5 µm,14.6 × 150 mmPump: Summit P680A2 Mobile Phase: 20% methanol; 30% acetonitrile;mAU 3 50% 0.05 M NH 4 H 2 PO 4 adj. to pH 2.5Flow: 1.5 mL/minB4 6Temperature: TCC100 thermostat at 60 °C7 8 Injection: ASI-100 autosampler; 25 µL0A5Detector: UVD 340U; UV at 220 nm0 5 10 15 20Samples: (A) “Low load” test mixMinutes(B) “Resolution” test mixData courtesy of: V. Bhate of Analytical SolutionsPeaks: 1. Impurity A 1 µg/mL2. Impurity B 13. Benzoic acid 94. Benzaldehyde 95. Phenytoin sodium 1000 (B) or 3 (A)6. Benzoin 97. Benzophenone 18. Benzil 92046522664APPLICATIONS- 32 -www.dionex.com