Validated gradient stability indicating HPLC method for determining Diltiazem Hydrochloride and related substances in bulk drug and novel tablet formulation

Abstract

A stability-indicating liquid chromatographic method has been developed and validated for the determination of Diltiazem Hydrochloride (DTZ) together with its six related substances (Diltiazem sulphoxide, Imp-A, Imp-B, Imp-D, Imp-E, and Imp-F) in a laboratory mixture as well as in a novel tablet formulation developed in-house. Efficient chromatographic separation was achieved on a Hypersil BDS C18 (150 mm×4.6 mm, 5.0 μm) with mobile phase containing 0.2% Triethylamine (TEA) in gradient combination with acetonitrile (ACN) at a flow rate of 1.0 mL/min and the eluent was monitored at 240 nm. In the developed method, the resolution of DTZ from any pair of impurities was found to be greater than 2.0. The test solution and related substances were found to be stable in the diluent for 24 h. The developed method resolved the drug from its known impurities, stated above, and also from additional impurities generated when the formulation was subjected to forced degradation; the mass balance was found close to 99.9%.Regression analyses indicate correlation coefficient value greater than 0.997 for DTZ and its six known impurities. The LOD for DTZ and the known impurities was at a level below 0.02%. The method has shown good, consistent recoveries for DTZ (99.8–101.2%) and also for its six known impurities (97.2–101.3%). The method was found to be accurate, precise, linear, specific, sensitive, rugged, robust, and stability-indicating.

Real time calorimetric characterisation of clay – drug complex dispersions and particles

“…Results were evaluated statistically in terms of standard deviation (RSD %) (Ich, 2005). The intermediate and intra assay precision at three different concentration levels was lower than 2% RSD which complied with the acceptable criteria for quality control of pharmaceutical preparations (Ermer and Ploss, 2005, Chatpalliwar et al, 2012).…”

Magnesium Aluminium Silicate-Metformin Hydrochloride Complexes - The Use of Isothermal Calorimetry for Probing Clay and Drug Nanocomplexations

“…This was evident in the lower than 2 % RSD which complies with the acceptable criteria for quality control of pharmaceutical preparations. [31], [32] The LOQ showing the lowest drug concentration that can be recovered within acceptable limits of precision and accuracy was found to be 1.01 µg/mL indicating the high sensitivity of the proposed method and its suitability for the detection MET in solutions at low concentrations. LOD showing the lowest detectable amount of drug distinguishable from the blank was 0.33 µg/mL also showing the sensitivity of the method (Table 2).…”

Stability-indicating assay method for determination of actarit, its process related impurities and degradation products: Insight into stability profile and degradation pathways ☆

“…Solution stability of actarit in the related substance method was carried out by leaving analyte mixture solution (drug, degradation products and impurities) in a tightly capped volumetric flask at room temperature for 2 days. Content uniformity of impurities (IMP-1/DP-1, IMP-2, IMP-3, IMP-4/DP-2, IMP-5, and IMP-6) was checked in the test solutions [20] .…”