تحديد الشوائب المرافقة و منتجات التخرب في آرغاتروبان Argatroban باستعمال الاستشراب السائل مع مكشاف طيف الكتلة LC-MS

الملخص EN

Argatroban is a direct thrombin inhibitor used as intravenous anticoagulant drug.

the purpose of this work was to develop suitable stability-indicating LC-MS method for the determination of Argatroban, its related impurities and its degradation products in active pharmaceutical ingredient (API).

the analysis were carried out by using UV detector at 257 nm and by using MS detector with electro-spray ionization ESI, the column oven temperature was at 35°C, the Argatroban impurities were determinated on a Shimadzu XR-ODS II column, with a mobile phase containing water and acetonitrile in gradient program, at a flow rate of 0.3ml/min.

forced degradation study was carried out under different acidic, alkaline, oxidative, photolytic and thermal conditions to demonstrate the stability-indicating nature of the developed method.

with the aid of MS, photo-diode-array and UV techniques, 13 impurities and 38 degradation products have been determinate, and their molecular weights information have been obtained.

the method was validated, according to USP 35 guideline recommendations and to the ICH guidelines for validation.

the method is suitable for practical routine analysis of active pharmaceutical ingredient (API).