Validated green micellar electrokinetic capillary chromatography for simultaneous determination of simvastatin and sitagliptin phosphate binary mixture in pharmaceutical formulation

Abstract

Diabetics are liable to fatal atherosclerotic cardiovascular diseases. It is clinically attributed to their imbalanced plasma lipoproteins. Fixed‐dose combination “polypill” of simvastatin (10 mg) and sitagliptin phosphate (100 mg) is mainly indicated for the treatment of diabetic dyslipidemia. Novel green micellar electrokinetic capillary chromatographic method has been developed for simultaneous determination of simvastatin and sitagliptin phosphate in binary synthetic mixtures and their pharmaceutical formulation. Separation was achieved using a deactivated fused silica capillary (50 cm effective length × 50 μm id) through a background running electrolyte of 100 mM borate buffer (pH 9.1) and 100 mM sodium dodecyl sulfate. Diode array detection was set at 238 and 210 nm for simvastatin and sitagliptin phosphate, respectively. All experimental parameters were closely varied and optimized. Both drugs declared good linearities over the range of 10–100 μg/mL. Proposed study was validated according to International Council for Harmonization guidelines. It was applied to the assay of laboratory‐made binary mixtures and marketed tablets. Electrophoretic assay was compared with a reported spectrophotometric one. Satisfactory t‐test and F‐ratio indicated insignificant differences between both methods. Moreover, it is the first capillary electrophoretic simultaneous assay for simvastatin and sitagliptin phosphate, and fits a linear correlation with the green analytical attributes.

Bioanalytical Method Development and Validation of Tofacitinib in Rat Plasma Using Green Solvent and Application to Pharmacokinetic Study by LC‐MS

“…In terms of sample preparation, ideally, extraction‐free methods are preferred, but complex sample matrices often make this impractical. Some techniques like liquid–liquid microextraction and solid‐phase microextraction reduce solvent use, they are often too slow and labor‐intensive for high‐throughput laboratories like those in drug discovery these methods also face limitations in solvent choice, sensitivity, precision, and stability, making them less suitable for routine use [2–9]. As per literature review it was found that tofacitinib a small molecule used to treat ulcerative colitis and approved in the EU in 2018 [10], is typically analyzed using LC‐MS methods that rely heavily on acetonitrile for both extraction and mobile phases and no method is available with methanol as in chromatographic condition as well as in extraction procedure use methanol.…”

Bioanalytical Method Development and Validation of Tofacitinib in Rat Plasma Using Green Solvent and Application to Pharmacokinetic Study by LC‐MS

“…In terms of sample preparation, ideally, extraction‐free methods are preferred, but complex sample matrices often make this impractical. Some techniques like liquid–liquid microextraction and solid‐phase microextraction reduce solvent use, they are often too slow and labor‐intensive for high‐throughput laboratories like those in drug discovery these methods also face limitations in solvent choice, sensitivity, precision, and stability, making them less suitable for routine use [2–9]. As per literature review it was found that tofacitinib a small molecule used to treat ulcerative colitis and approved in the EU in 2018 [10], is typically analyzed using LC‐MS methods that rely heavily on acetonitrile for both extraction and mobile phases and no method is available with methanol as in chromatographic condition as well as in extraction procedure use methanol.…”

Bioanalytical Method Development and Validation of Tofacitinib in Rat Plasma Using Green Solvent and Application to Pharmacokinetic Study by LC‐MS

“…In terms of sample preparation, ideally, extraction‐free methods are preferred, but complex sample matrices often make this impractical. Some techniques like liquid–liquid microextraction and solid‐phase microextraction reduce solvent use, they are often too slow and labor‐intensive for high‐throughput laboratories like those in drug discovery these methods also face limitations in solvent choice, sensitivity, precision, and stability, making them less suitable for routine use [2–9]. As per literature review it was found that tofacitinib a small molecule used to treat ulcerative colitis and approved in the EU in 2018 [10], is typically analyzed using LC‐MS methods that rely heavily on acetonitrile for both extraction and mobile phases and no method is available with methanol as in chromatographic condition as well as in extraction procedure use methanol.…”

Bioanalytical Method Development and Validation of Tofacitinib in Rat Plasma Using Green Solvent and Application to Pharmacokinetic Study by LC‐MS

“…In terms of sample preparation, ideally, extraction‐free methods are preferred, but complex sample matrices often make this impractical. Some techniques like liquid–liquid microextraction and solid‐phase microextraction reduce solvent use, they are often too slow and labor‐intensive for high‐throughput laboratories like those in drug discovery these methods also face limitations in solvent choice, sensitivity, precision, and stability, making them less suitable for routine use [2–9]. As per literature review it was found that tofacitinib a small molecule used to treat ulcerative colitis and approved in the EU in 2018 [10], is typically analyzed using LC‐MS methods that rely heavily on acetonitrile for both extraction and mobile phases and no method is available with methanol as in chromatographic condition as well as in extraction procedure use methanol.…”