Utility of dansyl chloride for the establishment of a sensitive spectrofluorimetric approach for estimating midodrine hydrochloride: application to content uniformity testing.

A new, straightforward spectrofluorimetric approach with high sensitivity was established for determining midodrine hydrochloride based on derivatizing this drug through its reaction with 5-(dimethylamino)naphthalene-1-sulfonyl chloride (dansyl chloride). The highly fluorescent product was extracted with methylene chloride, and then its emission was measured at 532 nm after excitation at 339 nm. The reaction was conducted in aqueous medium containing 0.1 M borate buffer (pH 8.2). The results showed that the proposed method is sensitive with high linearity in the range from 0.1 to 3 µg mL-1. The lower limits of detection and quantitation were 29 and 88 ng mL-1, respectively. Furthermore, the proposed approach was analytically assessed by applying the ICH guidelines. The suggested approach was effectively utilized for the estimation of the medicine in its marketable tablet formulations with excellent recovery and without any interfering effect from excipients. Moreover, the presented approach was utilized to test the content uniformity of commercial tablets following the USP guidelines.

Studying the kinetic of midodrine degradations using TLC stability approach: Application to dosage form and human plasma.

A simple, rapid and selective thin layer chromatographic method has been developed for estimation of the antihypotension drug, midodrine hydrochloride, in pure form, tablet, spiked plasma and artificially degraded samples. Separation was carried out using silica gel 60-F254 as a stationary and mobile phase consisting of methanol: methylene chloride: ammonia in ratio of 8:2:0.2. The detection was carried out at wavelength of 290 nm. The retardation factor was found to be 0.7 and 0.49 for midodrine and its main degradation product desglymidodrine. The method showed linearity for midodrine over a concentration range of 50-1500 ng/spot with good correlation and determination coefficient. The method was applied successfully for analysis of commercial tablets and oral drops with good recovery and without interference of excipients. The method also was applied for studying the stability of the cited drug under different stress conditions including acidic, alkaline, hydrolytic, oxidative and photo- degradations. Furthermore, the kinetic of acidic and alkaline degradations was investigated and the rate constants were found to be 0.620 and 0.074 K h-1 while half life time (t1/2) values were 1.12 and 9.32 h, respectively.