Abstract

DEVELOPMENT AND VALIDATION OF HPTLC METHOD FOR ESTIMATION OF TIOTROPIUM BROMIDE MONOHYDRATE IN DRY POWDER INHALATION DOSAGE FORM

Anuja S. Nevse, Savita Yadav, Ravindra N. Purohit, Janhavi R. Rao*

ABSTRACT

A simple, precise, rapid and selective high performance thin layer chromatographic (HPTLC) method has been developed and validated for estimation of Tiotropium bromide monohydrate in bulk drug and in dry powder inhalation dosage form. TLC aluminium plates (Merck) precoated with silica gel 60F254 was used as the stationary phase. The solvent system comprising of ammonium acetate: methanol: n-propanol in the ratio of 8: 1.6: 1.6 (v/v/v) gave a dense compact spot of tiotropium bromide monohydrate with an Rf value of 0.40 ± 0.02. Densitometric analysis was carried out at 242 nm. The method was validated in compliance with ICH Guideline for linearity, limit of detection (LOD), limit of quantification (LOQ), precision, specificity, accuracy and robustness. The drug response with respect to peak area was linear over the concentration range 200-1200 ng/spot. The LOD and LOQ were 60 and 180 ng/spot respectively. Statistical evaluation proved that the established method was accurate, specific, precise, repeatable and robust for the estimation of tiotropium bromide monohydrate. Being simple and economical, the method can be employed for the routine quality control analysis of tiotropium bromide monohydrate in bulk and dry powder inhalation dosage form.

Keywords: Tiotropium bromide monohydrate, HPTLC, Method development and Validation.