Abstract
The objective of the present work was to develop a stability-indicating RP-HPLC method for duloxetine hydrochloride (DUL) in the presence of its degradation products generated from forced decomposition studies. The drug substance was found to be susceptible to stress conditions of acid hydrolysis. The drug was found to be stable to dry heat, photodegradation, oxidation and basic condition attempted. Successful separation of the drug from the degradation products formed under acidic stress conditions was achieved on a Hypersil C-18 column (250 mm × 4.6 mm id, 5μm particle size) using acetonitrile: 0.01 M potassium dihydrogen phosphate buffer (pH 5.4 adjusted with orthophosphoric acid) (50:50, v/v) as the mobile phase at a flow rate of 1.0 ml/min. Quantification was achieved with photodiode array detection at 229 nm over the concentration range 1–25 μg/ml with range of recovery 99.8–101.3 % for DUL by the RP-HPLC method. Statistical analysis proved the method to be repeatable, specific, and accurate for estimation of DUL. It can be used as a stability-indicating method due to its effective separation of the drug from its degradation products,
Highlights
Duloxetine HCl (DUL) – (3S)-N-methyl-3-(naphthalen-1-yloxy)-3-(thiophen-2-yl)propan1-amine hydrochloride [1] – has an empirical formula of C18H19NOS⋅HCl and a molecular weight of 333.38 g/moL (Figure 1)
Reports were found regarding the characterization of phenolic impurities in DUL samples by MS, NMR spectrometry, and X-ray analysis [10] and of impurities formed by interaction of DUL with various enteric polymers [11]
HPLC chromatogram of Duloxetine hydrochloride (RT 5.84 min) on C18 hypersil column using 0.01 M potassium dihydrogen phosphate buffer (50:50, v/v) as the mobile phase
Summary
Duloxetine HCl (DUL) – (3S)-N-methyl-3-(naphthalen-1-yloxy)-3-(thiophen-2-yl)propan1-amine hydrochloride [1] – has an empirical formula of C18H19NOS⋅HCl and a molecular weight of 333.38 g/moL (Figure 1). It is a potent inhibitor of serotonin and norepinephrine reuptake and it is used for major depressive disorders [2,3,4]. The aim of the present work was to develop an accurate, selective, precise, robust, and stability-indicating RP-HPLC method for the determination of DUL in the presence of its degradation products and related impurities in tablets. The proposed method was validated according to ICH guidelines [18, 19] and its updated international convention ICH guideline on analytical method validation [20]
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