In-lab synthesized turn-off fluorescence sensor for estimation of Gemigliptin and Rosuvastatin polypill appraised by Spider diagram, AGREE and whiteness metrics.

Gemigliptin-Rosuvastatin single-pill combination is a promising therapeutic tool in the effective control of hyperglycemia and hypercholesterolemia. Organic sensors with high quantum yields have profoundly significant applications in the pharmaceutical industry, such as routine quality control of marketed formulations. Herein, the fluorescence sensor, 2-Morpholino-4,6-dimethyl nicotinonitrile 3, (λex; 226 nm, λem; 406 nm), was synthesized with a fluorescence quantum yield of 56.86% and fully characterized in our laboratory. This sensor showed high efficiency for the determination of Gemigliptin (GEM) and Rosuvastatin (RSV) traces through their stoichiometric interactions and simultaneously fractionated by selective solvation. The interaction between the stated analytes and sensor 3 was a quenching effect. Various experimental parameters and the turn-off mechanism were addressed. The adopted approach fulfilled the ICH validation criteria and showed linear satisfactory ranges, 0.2-2 and 0.1-1 µg/mL for GEM and RSV, respectively with nano-limits of detection less than 30 ng/mL for both analytes. The synthesized sensor has been successfully applied for GEM and RSV co-assessment in their synthetic polypill with excellent % recoveries of 98.83 ± 0.86 and 100.19 ± 0.64, respectively. No statistically significant difference between the results of the proposed and reported spectrophotometric methods in terms of the F- and t-tests. Ecological and whiteness appraisals of the proposed study were conducted via three novel approaches: the Greenness Index via Spider Diagram, the Analytical Greenness Metric, and the Red-Green-Blue 12 model. The aforementioned metrics proved the superiority of the adopted approach over the previously published one regarding eco-friendliness and sustainability. Our devised fluorimetric turn-off sensing method showed high sensitivity, selectivity, feasibility, and rapidity with minimal cost and environmental burden over other sophisticated techniques, making it reliable in quality control labs.

Determination of Ibuprofen and Phenylephrine in Tablets by High-Performance Thin Layer Chromatography and in Plasma by High-Performance Liquid Chromatography with Diode Array Detection.

Two chromatographic methods (high performance thin layer chromatography (HPTLC) and high performance liquid chromatography-diode array detector (HPLC-DAD)), were addressed for the analysis of a mixture consisted of phenylephrine hydrochloride and ibuprofen in two forms bulk and their combined dosage form. This binary mixture is considered to be a challenging one as the two drugs differ greatly in their chemical and physical properties. Not only this affects their simultaneous analysis, but also hinders their simultaneous extraction from biological fluids as plasma. That is the reason the literature lacks any report for the simultaneous extraction and analysis of these drugs from biological fluids. The concentration ranges of both drugs were 0.1-2.5 µg/spot and 0.1-100 µg/mL by HPTLC and HPLC, respectively. Not only was the HPLC-DAD method applied to the investigated drugs determination in pharmaceutical preparations, but also in spiked human plasma. Extensive study was conducted to optimize their simultaneous extraction from plasma as it was a crucial step for the in vivo analysis. The results obtained by proposed methods and a reference one were statistically comparable by analysis of variance test. No significant difference was recorded between the mean percent levels determined by the proposed methods and the reference one.

Application of Capillary Zone Electrophoresis Coupled with a Diode Array Detector (CZE-DAD) for Simultaneous Analysis of Ibuprofen and Phenylephrine.

Background: A validated method based on capillary zone electrophoresis coupled with a diode array detector (CZE-DAD) was investigated for analyzing binary mixture of ibuprofen (IBU) and phenylephrine (PHE) in their bulk and combined dosage form. Objective: This binary mixture is a challenging one as IBU is acidic and PHE is alkaline, which may affect their simultaneous analysis using CZE. The literature lacks any CZE report for IBU and PHE simultaneous analysis. Methods: Fused silica capillary (85 cm × 75 µm id) was used, and the electrolyte was a 50 mM borate buffer adjusted to pH 11 with 0.5 M NaOH. Results: The concentration ranges were 5-200 and 5-100 µg/mL for IBU and PHE, respectively, using CZE. High efficiency was achieved (N > 92990). Reasonable migration time (tm) was attained (tm< 8.5 min). Conclusions: Although the results obtained by the proposed CZE method and reported HPLC method were statistically comparable, the proposed method showed lower linearity ranges, higher efficiency, and a more reasonable run time. Highlights: CZE-DAD was used for the analysis of IBU and PHE in bulk and tablets, as no report was found for their determination using CZE. Binary mixture is challenging due to differences in chemical and physical properties. A detailed discussion of electrophoretic parameters optimization is included. Confirmation of peak purity was attained using DAD.