Diazo Coupling for the Determination of Selexipag by Visible Spectrophotometry

Abstract

Aim and Objective: The aim and objective of this study were to develop a spectrophotometric method for the assay of selexipag (selective IP prostacyclin receptor agonist indicated for the treatment of pulmonary arterial hypertension) in pure and pharmaceutical formulations so that it will be an alternative quantitative method to chromatographic methods which require large quantities of organic solvents, where some are with hazardous and toxic properties. Materials and Methods: The method is based on the diazo coupling of selexipag with diazotized p-nitroaniline in alkaline medium to form a stable green-colored and water-soluble azo dye with a maximum absorption at 510 nm. Optimization of reaction conditions was carried out to get highly sensitive and stable colored complex. Results and Discussion: Beer's law is obeyed over the concentration range of 2-12 µg/mL with a molar absorptivity of 3.33 × 10 4 L/mol/cm. The limit of detection was 0.35 μg/mL and limit of quantification was 1.0 µg/mL. The results demonstrated that the procedure is accurate, precise, and reproducible (relative standard deviation <2%). Conclusions: This method was tested and validated for various parameters according to the current ICH guidelines.

A novel HPLC method for selexipag in human plasma and application to a prototype pharmacokinetic study

“…SLP is a relatively novel active substance for the treatment of pulmonary arterial hypertension. Existing methods for determination from plasma in the literature provide assays in rat plasma [7]. Human plasma analysis that provides quantitation in pharmacokinetic levels is a requirement for SLP.…”

“…The previously developed methods [5][6][7][8][9][10][11] provide assasys in bulk and pharmaceutical forms, they are not suitable for plasma assays and their sensitivity is not enough for bioanalytical studies. Other MS methods; LC-MS/MS [12,13,[15][16][17] and UPLC-MS/MS [14] were sensitive but they are for rat plasma samples.…”

“…In addition, there are not enough methods that provide pharmacokinetic studies to be easily applicable for the determination of SLP in human plasma. Review of literature revealed that few methods were reported for the estimation of SLP including; spectrophotometric methods [5][6][7], gas chromatograhy [8] and chromatographic methods [9][10][11][12] in dosage form, in addition to, LC-MS/MS methods in plasma [13][14][15][16][17].…”

Bioanalytical LC-MS/MS method for Determination and comparison of Selexipag Assay in various Biological materials and its Application to Pharmacokinetics Studies in Rat plasma

“…Ambrisentan was selected as internal standard, since this this drug can be used for PAH treat-ment ( Figure 2). Bioanalysis is an area of analytical chemistry (Damireddy et al, 2017) in the quantitative measurement of xenobiotics (Gorumutchu and Ratnakaram, 2018;Patil et al, 2017;Ratnakaram, 2018) and biotics in biological systems. Bioanalytical common techniques reported in the literature are, hyphenated techniques like LC-MS, GC-MS, LC-DAD, CE-MS, chromatographic methods like HPLC, GC, UPLC, Supercritical luid chromatography.…”

Visible Spectrophotometric Determination of Gemigliptin using Charge Transfer Complex

“…Out of the various reactions involved in spectrophotometric assay of pharmaceutical drugs, charge transfer reaction is proved to be highly sensitive as well as acceptable method, in addition to reactions involving to ion pair [9][10][11][12][13][14][15] and oxidation [16][17][18][19][20] . The complex formed between electron donor and acceptor compound yields a new absorption band with a precise l max pertaining to that complex.…”