Stability indicating high performance liquid chromatographic determination of sitagliptin in bulk drug and formulations

Other Title(s)

استخدام HPLC لتحديد و الاستدلال على ثبات مادة السيتاجلبتين في صيغته الخام و صيغته الدوائية

Dissertant

al-Shalabi, Rim Z.

Thesis advisor

Shakya, Ashok Kumar

University

Al-Ahliyya Amman University

Faculty

Faculty of Pharmacy and Medical Sciences

Department

Pharmaceutical Sciences

University Country

Jordan

Degree

Master

Degree Date

2013

English Abstract

The purpose of this study was to develop a new stability indicating method for the analysis of sitagiiptin in formulation and raw material.

In the present study a rapid, simple, economical reverse phase HPLC procedure has been developed for the determination of sitagiiptin.

The sitagiiptin was separated isocratically on Hypersil-Gold C18 column (Length- 250 mm.

Diameter- 4.6 mm.

Particle size-5 μm) with a mobile phase consisting of 25 % acetonitrile, 75 % water (containing 0.25 ml / L triethylamine, final pH was adjusted to 2.75 ± 0.10), operated at 25 ± 1 °C with a retention time less than 8 min.

The total run time of the stressed study was 20 mins.

The eluted drug was identified and monitored on a Photo Diode-Array detector (PDA) at λ = 215 nm.

The linearity of the method was excellent (r2 > 0.9998) over the concentrations range of 2.5-100 μg / ml ; the LOD and LOQ were 0.0627 μg / ml and 0.1896 μg / ml respectively.

The statistical evaluation of the method was examined by performing intraday and interday precision analysis.

The overall precision (% CV, RSD) was less than 2.0 %.

Mean recovery of sitagiiptin was more than 99.0 %, no interference was found from the other ingredient or component present in the preparation.

The result of stability studies indicates that the drug was stable when exposed to direct sunlight, T-TV light or chemical stress (exposure to IN HC1 or 35% H2O2).

The drug gives 2 degraded products on exposure to alkaline condition (NaOH, IN).

The percent of degraded products was 12.2 %.

In conclusion the method presented here is sensitive, rapid, accurate, precise, economic, robust, rugged and selective for the routine analysis of the drug in formulation and raw material in presence of degraded products.

Main Subjects

Pharmacology

Topics

• Drugs

• APA
• MLA
• AMA

Language

English

Data Type

Arab Theses

Record ID

BIM-357954