Abstract

Ashok K. Shakya

DOI : http://dx.doi.org/10.13005/ojc/320203

The present paper involves the analytical quality by design (AQbD)-based development of a simple, rapid, accurate and precise stability-indicating method for the estimation of valsartan and hydrochlorothiazide. Optimized mobile phase (v/v/v) was water (containing 0.25 ml/L triethylamine), methanol and acetonitrile (50:38:37, pH adjusted to 3.0±0.1).  Chromatographic separation was achieved on Hypersil^®-Gold C₁₈ (150 x 4.6 mm, 5 µm, Thermo Fisher Scientific, USA), column at 25 ± 2 °C.  The method was validated as per the “International Conference on Harmonisation” (ICH) guidelines. Chromatographic run time was 10.0 minutes.  The linearity range for valsartan and hydrochlorothiazide were 1.25-64.00 µg/ml and 0.195-10.00 µg/ml respectively.  The limits of detection (LOD) for valsartan and hydrochlorothiazide were 0.253 and 0.0226 μg/ml while the limits of quantitations (LOQ) were 0.767 and 0.068 μg/ml respectively, using 10µl sample. Stability studies indicate that the degradation of valsartan was higher during oxidative stress than other stress.

Valsartan; hydrochlorothiazide; Central Composite Design; Design of experiments (DoE); Analytical Quality by Design (AQbD); Response surface methodology (RSM); HPLC

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