New Validated UPLC Method for the Determination of Tiemoniummethylsulphate in Pharmaceutical and Biosamples

Abstract

MaterialsHPLC-grade methanol was supplied by Sigma-Aldrich (Germany), ACN was supplied by Scharlau (Scharlab S.L, Spain) and sodium dihydrogen phosphate was supplied by Applichem GmbH (Germany). Water used throughout the study was purified by the reverse osmosis method to gain high-purity water with a Milli-Q water purification system from Millipore (Millipore, Bedford, MA, USA). Purity of reference compounds was not less than 98%. Pharmaceutical formulations commercially available in Bangladesh were analysed to check the applicability of the method: Torax(10mg) tablet by Square, Rolac(10mg) tablet by Renata, Etorac(10mg) tablet by Incepta, Zidolac(10mg) tablet by Beximco, ketonic (10mg) tablet by SK+F, Torax(30mg) injection by Square, Rolac(30mg) injection by Renata, Norvis (50mg) tablet by Square, Visceralgin (50mg) tablet by Nuvista, Timozin (50mg) tablet by Incepta , Visrul (50mg) AbstractA new method has been described to determine Tiemonium methylsulphate in biofluids and pharmaceutical samples by UPLC with a UV detector set at 240nm. Reversedphase Gemini 3U, C18, 110R (150×4.6mm, 3μm) column has been used with a mobile phase composition consisting CH 3 OH, CH 3 CN and NaH 2 PO 4 under isocratic program. When it is eluted at a short of 1.12min. A careful liquid-phase extraction was optimized to isolate the drugs from biofluids. The results were linear upto 10µg mL -1 with the correlation coefficients greater than 0.998. The sensitivity limits, LOD and LOQ were 0.12 and 0.37µg mL -1 , respectively. The method is simple, fast and reliable with good specificity and sensitivity and will be suitable for routein analysis of the drug.