An Ultra Performance Liquid Chromatography (UPLC) method has been developed for the simultaneous determination of ketorolac tromethamine (KTR) and tiemonium methylsulphate (TMS) in pharmaceutical and bio-samples. Calibration curves were linear with correlation coefficient 0.9997 at a studied concentration range of (0.1-10 μg mL-1) for both drugs. The method was reproducible with relative standard deviation (RSD) for intraday precision was 0.32-0.99% for KTR and 0.40-1.01% for TMS and inter day precision was 0.51-2.77% for KTR and 0.41-2.26% for TMS. The mean recovery of the intraday assay was 99.18-103.34% for KTR and 99.14-101.76% for TMS and inter-day assay at six different days was 99.39-102.04% for KTR and 98.08-103.78% for TMS. The limit of detection (LOD) and limit of quantitation (LOQ) were 0.125 and 0.41 μg mL-1 , respectively for KTR and 0.150 and 0.50 μg mL-1 , respectively for TMS. The method was successfully validated as per the ICH guidelines can be conveniently employed for routine quality control analysis of KTR and TMS in pharmaceutical formulations and biological samples without any interference.

A new UPLC method has been described to determine ketorolac tromethamine in pharmaceutical samples and biofluids. Drug was eluted using a reversed-phase Gemini 3U, C18, 110R (150 × 4.6 mm, 3 μm) column when a mobile phase composition 90:05:05 (v/v) consisting CH 3 OH, CH 3 CN and NaH 2 PO 4 under isocratic program. Ketorolac tromethamine was eluted at a short of time 2.02 min. Ketorolac tromethamine isolated from biofluids after liquid-phase extraction. The results were linear up to 10 µg mL -1 with the correlation coefficients greater than 0.999. The sensitivity limits, LOD and LOQ were 0.016 and 0.051 µg mL -1 , respectively. The method is simple, fast and reliable with good specificity and sensitivity and will be suitable for routine analysis of ketorolac tromethamine.

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.

Attempt has been made to develop a new, accurate, precise and economic spectrophotometric method for the simultaneous determination of ketorolactromethamine (KTR) and tiemoniummethylsulphate (TMS) in pharmaceutical formulation and bio-samples.It is noted that KTR shows two absorption peaks at 320 and 245 nm whereas TMS shows maximum absorption at 235 nm. In a mixture solution, peaks at 245 nm for KTR and at 235 nm for TMS are merged into a single peak at 240 nm. Hence KTR might be determined using its calibration equation constructed at 320 nm but the determination of TMS alone in their mixture measuring its absorption at 240 nm is difficult. Therefore, for the determination of TMS, a mathematical expression xT = k1.yK+T -k2.yK + k3 (y = Absorbance, x = Concentration) has been derived. This expression will give its concentration in mixture without having its absorption at 240 nm. Method has been applied to pharmaceutical and bio-samples successfully. Results have been compared to that estimated by new UPLC method developed as to validate this spectrophotometric method. The LOD and LOQ were found to be 0.25, 0.80 μg/mL for KTR and 0.31, 0.95 μg/mL for TMS, respectively.