Analytical lifecycle management oriented development and validation of a new stability-indicating ultra-fast liquid chromatographic method: case study of Glycopyrrolate

A new stability-indicating liquid chromatographic method was developed and validated for the estimation of glycopyrrolate in pharmaceutical formulations. A contemporary approach to analytical life-cycle management was followed to develop a robust and reliable chromatographic method. Scouted method variables such as % methanol, the strength of tetra butyl ammonium hydrogen sulfate and mobile phase flow rate were optimized using the design of experiment approach and their effect on critical quality attributes was studied. The critical quality attributes viz. retention time, theoretical plate count and symmetry factor were highly influenced by the three critical method variables. Optimum chromatography was attained on a C-18 column with a mobile phase methanol: 10 mM tetra butyl ammonium hydrogen sulfate (80:20, v/v) flowing at 1.0 mL.min-1. Chromatographic method specificity was ensured by degrading the drug forcefully. Validation studies postulated method acceptability and suitability for estimating glycopyrrolate in both bulk as well as injection formulation. Results for parameters viz. linearity (5-250 µg.mL-1), accuracy (>99%) and precision (<2%) advocated method reliability. Overall the method was reliable and of optimum quality and, possess the potential of application in routine and bio-analytical purposes

A RP-HPLC Method Development and Validation for the Estimation of Gliclazide in bulk and Pharmaceutical Dosage Forms.

A simple, selective, linear, precise and accurate RP-HPLC method was developed and validated for rapid assay of Gliclazide in pharmaceutical dosage form. Isocratic elution at a flow rate of 1.2 ml min -1 was employed on a symmetry C18 column at ambient temperature. The mobile phase consisted of methanol: phosphate buffer 50:50 (V/V). The UV detection wavelength was at 210 nm. Linearity was observed in concentration range of 1-100 μg/mL. The retention time for Gliclazide was 3.25 min. The method was validated as per the ICH guidelines. The proposed method can be successfully applied for the estimation of Gliclazide in pharmaceutical dosage forms.

Synthesis and biological evaluation of new 4-bromo-3, 5-diaryl-1-phenyl-2-pyrazoline derivatives as antioxidant and anti-inflammatory agents.

A number of substituted 1, 3-diphenylprop-2-en-1-one were prepared by Claisen-Schmidt condensation of p-substituted acetophenone with o,m,psubstituted aryl aldehydes which undergoes bromination and subsequent cyclization with phenyl hydrazine to yield 4-bromo-3(substituted phenyl)-5(substituted phenyl)-1-phenyl-2-pyrazoline (3a-l). The structures of compounds were confirmed by elemental analysis, IR, 1HNMR and mass spectral data. The synthesized compounds (3a-l) were screened for anti-oxidant and anti-inflammatory activity. The free radical scavenging properties were screened by using ascorbic acid as standard antioxidant. Free radical scavenging activity was evaluated using 1,1-diphenyl-2-picryl hydrazyl (DPPH) free radical. The antioxidant activity of compound 3b was found to be the strongest. The IC50 values of the synthesized compounds ranged between 8.87 and 81.07 (μg mL-1). The anti-inflammatory activities were evaluated by using diclofenac sodium as a standard dug. All the compounds (20mg/kg po) possess significant anti-inflammatory activity, as reflected by their ability to provide protection (66-99%) against carragenan induced edema in rat paw. The anti-inflammatory activity of compound 3g was found to be the highest. The safety of substituted bromo-pyrazolines is reflected by toxicity studies.