Abstract
A simple, accurate, rapid, and stability-indicating RP-HPLC method for a combination of tenofovir disoproxil fumarate, emtricitabine, and rilpivirine has been developed and subsequently validated in commercial tablets. The proposed HPLC method utilizes Phenomenex Gemini C18 column (150 mm × 4.6 mm i.d., 5 µm) and mobile phase consisting of MeCN, potassium dihydrogen phosphate buffer (20 mM, pH 3.3), and triethylamine 58.72 : 41.23 : 0.05 (v/v) at a flow rate of 1.7 mL/min. Quantitation was achieved with UV detection at 270 nm. The method was validated in terms of accuracy, precision, linearity, limits of detection, limits of quantitation, and robustness. This optimized method has been successively applied to pharmaceutical formulation and no interference from the tablet excipients was found. TDF, EMT, and RPV and their combination drug product were subjected to acid, base, neutral hydrolysis, oxidation, dry heat, and photolytic stress conditions and the stressed samples were analyzed by the proposed method. As the proposed LC method could effectively separate the drugs from its degradation products, it can be employed as stability-indicating method for the determination of instability of these drugs in bulk and commercial tablets.
Highlights
Safety and efficacy of pharmaceuticals are two basic problems with importance in drug therapy
This ICH guideline requires that stress testing on active pharmaceutical ingredients (API) and drug products should be carried out to establish their inherent stability characteristics, which should include the effect of temperature, humidity, light, and oxidizing agents as well as susceptibility across a wide range of pH
The pharmaceutical dosage form used in this study was Complera procured from the local market and labelled to contain 200 mg of emtricitabine, 300 mg of tenofovir disoproxil fumarate, and 25 mg of rilpivirine per tablet
Summary
Safety and efficacy of pharmaceuticals are two basic problems with importance in drug therapy. The development of stabilityindicating assays has increased dramatically using the approach of stress testing as enshrined in ICH guideline [1] and even this approach is being extended to drug combinations. This ICH guideline requires that stress testing on API and drug products should be carried out to establish their inherent stability characteristics, which should include the effect of temperature, humidity, light, and oxidizing agents as well as susceptibility across a wide range of pH. There are no detailed regulatory guidelines that direct how stress testing is to be done and stress testing has evolved into an “artful science” that is highly dependent on the experience of the pharmaceutical industries or the individuals directing the studies
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