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Gradient RP-HPLC method for the determination of potential impurities in atazanavir sulfate.

Journal of pharmaceutical and biomedical analysis (2011-02-15)
Sreenivasa Rao Chitturi, Yallappa Somappa Somannavar, Badarinadh Gupta Peruri, Sreenivas Nallapati, Hemant Kumar Sharma, Shankar Reddy Budidet, Vijay Kumar Handa, Hima Bindu Vurimindi
ABSTRACT

This paper proposes a simple and selective RP-HPLC method for the determination of process impurities and degradation products (degradants) of atazanavir sulfate (ATV) drug substance. Chromatographic separation was achieved on Ascentis(®) Express C8, (150mm×4.6mm, 2.7μm) column thermostated at 30°C under gradient elution by a binary mixture of potassium dihydrogen phosphate (pH 3.5, 0.02M) and ACN at a flow rate of 1.0ml/min. A photodiode array (PDA) detector set at 250nm was used for detection. Stress testing (forced degradation) of ATV was carried out under acidic, alkaline, oxidative, photolytic, thermal and humidity conditions. In presence of alkali, ATV transformed into cyclized products and the order of degradation reaction is determined by the method of initial rates. The unknown process impurities and alkaline degradants are isolated by preparative LC and characterized by ESI-MS/MS, (1)H NMR, and FT-IR spectral data. The developed method is validated with respect to sensitivity (lod and loq), linearity, precision, accuracy and robustness and can be implemented for routine quality control analysis and stability testing of ATV.

MATERIALS
Product Number
Brand
Product Description

Supelco
Ascentis® Express C8 Capillary, 2.7 μm HPLC Column, 2.7 μm particle size, L × I.D. 15 cm × 75 μm
Supelco
Ascentis® Express C8 Capillary, 2.7 μm HPLC Column, 2.7 μm particle size, L × I.D. 5 cm × 500 μm
Supelco
Ascentis® Express C8 Capillary, 2.7 μm HPLC Column, 2.7 μm particle size, L × I.D. 5 cm × 75 μm
Supelco
Ascentis® Express C8 Capillary, 2.7 μm HPLC Column, 2.7 μm particle size, L × I.D. 5 cm × 200 μm
Supelco
Ascentis® Express C8 Capillary, 2.7 μm HPLC Column, 2.7 μm particle size, L × I.D. 5 cm × 300 μm
Supelco
Ascentis® Express C8 Capillary, 2.7 μm HPLC Column, 2.7 μm particle size, L × I.D. 5 cm × 100 μm
Supelco
Ascentis® C8 HPLC Column, 5 μm particle size, L × I.D. 25 cm × 4.6 mm
Supelco
Ascentis® C8 HPLC Column, 5 μm particle size, L × I.D. 15 cm × 4.6 mm
Supelco
Ascentis® C8 HPLC Column, 3 μm particle size, L × I.D. 10 cm × 4.6 mm
Supelco
Ascentis® C8 HPLC Column, 3 μm particle size, L × I.D. 15 cm × 2.1 mm
Supelco
Ascentis® C8 HPLC Column, 3 μm particle size, L × I.D. 15 cm × 4.6 mm
Supelco
Ascentis® C8 HPLC Column, 3 μm particle size, L × I.D. 10 cm × 2.1 mm
Supelco
Ascentis® C8 HPLC Column, 3 μm particle size, L × I.D. 3 cm × 2.1 mm
Supelco
Ascentis® C8 HPLC Column, 5 μm particle size, L × I.D. 25 cm × 21.2 mm
Supelco
Ascentis® Express C8 Capillary, 2.7 μm HPLC Column, 2.7 μm particle size, L × I.D. 15 cm × 500 μm
Supelco
Ascentis® C8 HPLC Column, 3 μm particle size, L × I.D. 5 cm × 2.1 mm
Supelco
Ascentis® Express C8 Capillary, 2.7 μm HPLC Column, 2.7 μm particle size, L × I.D. 15 cm × 200 μm
Supelco
Ascentis® Express C8 Capillary, 2.7 μm HPLC Column, 2.7 μm particle size, L × I.D. 15 cm × 100 μm
Supelco
Ascentis® Express C8, 2.7 μm HPLC Column, 2.7 μm particle size, L × I.D. 7.5 cm × 4.6 mm
Supelco
Ascentis® Express C8, 2 μm UHPLC Column, 2 μm particle size, L × I.D. 7.5 cm × 2.1 mm
Supelco
Ascentis® Express C8, 2 μm UHPLC Column, 2 μm particle size, L × I.D. 10 cm × 2.1 mm
Supelco
Ascentis® Express C8, 2 μm UHPLC Column, 2 μm particle size, L × I.D. 15 cm × 2.1 mm
Supelco
Ascentis® Express C8, 2 μm UHPLC Column, 2 μm particle size, L × I.D. 3 cm × 3 mm
Supelco
Ascentis® Express C8, 2 μm UHPLC Column, 2 μm particle size, L × I.D. 3 cm × 2.1 mm
Supelco
Ascentis® Express C8, 2 μm UHPLC Column, 2 μm particle size, L × I.D. 5 cm × 3 mm
Supelco
Ascentis® Express C8, 2 μm UHPLC Column, 2 μm particle size, L × I.D. 5 cm × 2.1 mm
Supelco
Ascentis® Express C8, 2 μm UHPLC Column, 2 μm particle size, L × I.D. 7.5 cm × 3 mm
Supelco
Ascentis® Express C8, 2 μm UHPLC Column, 2 μm particle size, L × I.D. 10 cm × 3 mm
Supelco
Ascentis® Express C8, 2 μm UHPLC Column, 2 μm particle size, L × I.D. 15 cm × 3 mm
Supelco
Ascentis® Express C8, 2 μm UHPLC Column, 2 μm particle size, L × I.D. 2 cm × 2.1 mm