TLC densitometric approach for concurrent determination of quinary mixture for treatment of migraine with appraisal to method greenness and whiteness.

Abstract

A new accurate, precise thin layer chromatographic (TLC densitometric) approach was developed for the simultaneous analysis of ergotamine tartrate (ERG), phenobarbital sodium (PHEN), caffeine anhydrous (CAF), dipyrone sodium (DIP) and meprobamate (MEP) in their pure form and in their combined formulation; (MIGRANIL tablets). TLC separation depended on using a stationary phase of TLC plates F₂₅₄ (20 × 10 cm) and using a developing system of ethyl acetate: methanol: n- hexane (8:2:3, by volume) with UV scanning at 254 nm for ERG, PHEN, CAF and DIP. For MEP, detection was done at 560 nm after spraying with 0.3% ethanolic solution of para -dimethylaminobenzaldehyde (PDAB) and heating at 110 ºC for 30 min. Analysis was performed in the concentration intervals of 0.06-2, 0.15-5 µg/band for ERG and PHEN, respectively; while for CAF, DIP and MEP it was done in the ranges of 0.3-9, 0.5-10, 1-100 µg/band, respectively. Moreover, the method was used for the quantitation of the five studied drugs in their unique formulation and the recovery% was calculated and found to be 102.04, 100.73, 100.65, 99.91, 1nd 101.77% for ERG, PHEN, CAF, DIP, and MEP, in order and all these outcomes proved excellent selectivity of the method. Other validation parameters were tested following ICH guidelines. Accuracy ranged from 98.02 to 100.53% while the obtained %RSD of interday day precision ranged from 1.215 to 1.940%. The environmental impact and performance of the method was tested with several tools; Analytical eco-scale, green analytical procedure index (GAPI), Analytical GREEnness Metric Approach (AGREE), Blue applicability grade index (BAGI), and RGB additive color model. Results ensured minimum hazardous effect on health and environment. This is the first analytical approach developed for simultaneous analysis of the quinary mixture which can be easily applied in any analytical laboratory.