Green method by National Environmental Methods Index and Eco-Scale Assessment for evaluation of gatifloxacin-based product by HPLC.

The literature reveals gaps in the availability of green analytical methods for assessing products containing gatifloxacin (GFX), a fluoroquinolone. Presently, method development is supported by tools such as the National Environmental Methods Index (NEMI) and Eco-Scale Assessment (ESA), which offer objective insights into the environmental friendliness of analytical procedures. The objective of this work was to develop and validate a green method by the NEMI and ESA to quantify GFX in eye drops using HPLC. The method utilized a C8 column (4.6 × 150 mm, 5 µm), with a mobile phase of purified water containing 2% acetic acid and ethanol (70:30, v/v). The injection volume was 10 µL and the flow rate was 0.7 mL/min in isocratic mode at 25°C, with detection performed at 292 nm. The method demonstrated linearity in the range of 2-20 µg/mL, and precision at intra-day (relative standard deviation [RSD] 1.44%), inter-day (RSD 3.45%), and inter-analyst (RSD 2.04%) levels. It was selective regarding the adjuvants of the final product (eye drops) and under forced degradation conditions. The method was accurate (recovery 101.07%) and robust. The retention time for GFX was approximately 3.5 min. The greenness of the method, as evaluated by the NEMI, showed four green quadrants, and by ESA, it achieved a score of 88.

A Two-Step Optimization Approach: Validated RP-HPLC Method for Determination of Gatifloxacin and Dexamethasone in Ophthalmic Formulation.

The growing technology of stationary phase chemistry has a great impact on the chromatographic system performance and analysis economics. In this context, a simple rapid reversed phase high-performance liquid chromatography method development is presented for the analysis of gatifloxacin (GFN) and dexamethasone sodium phosphate (DSP) in their ophthalmic formulation. A two-step optimization approach has been conducted using optimum chromatographic conditions as well as proper selection of stationary phase. The chromatographic separation was carried out using sodium phosphate buffer pH 3.0 ± 0.1 and acetonitrile 72:28 v/v, respectively, with flow rate 1 mL min-1 and simultaneous detection at 243 nm. Three different column technologies were investigated at the optimum set of the chromatographic conditions: Xbridge® bridged ethylene hybrid silica, Kinetex™ Core-Shell and the Onyx™ Monolithic stationary phase. The monolithic column has shown better chromatographic separation, based on system suitability testing as well as shorter analysis time and sensitivity. The proposed method was validated according to International Conference on Harmonization guidelines. The linearity was achieved for GFN and DSP in the range 0.58-120 µg mL-1 and 0.50-120 µg mL-1, respectively, with acceptable accuracy, precision and selectivity.

First derivative synchronous fluorescence spectroscopy for the determination of Gatifloxacin in presence of its oxidative degradation product: Application to pharmaceutical preparation.

A highly accurate and precise spectrofluorimetric method was established for quantitation of Gatifloxacin in pure material, pharmaceutical formulations and in the existence of its oxidative degradation product. The emission was recorded at 487 nm after the excitation at 290 nm. Using micelle, sodium dodecyl sulphate (SDS), enhanced fluorescence intensity of Gatifloxacin-SDS complex. The optimization of numerous experimental conditions was carried out. The improved emission showed a suitable linear correlation between derivative synchronous fluorescence power and concentration of Gatifloxacin over the range of 10 to 100 ng/mL with a determination coefficient equals 0.9996. Studying cytotoxicity and antimicrobial susceptibility for oxidative degradation product of Gatifloxacin was carried out using Gatifloxacin as a control. In comparison, the proposed method presented a superior sensitivity and enhanced stability over the reported method.

CL sensitisation of tris-(bipyridyl) ruthenium (II) - cerium (IV) reaction system by AgNPs for determination of GFX.

The flow injection combined with tris-(bipyridyl) ruthenium (II)-cerium (IV) chemiluminescence (CL) method based on the sensitisation of silver nanoparticles (AgNPs) has been established for the quantitative analysis of gatifloxacin (GFX). AgNPs were synthesised using the reaction between ammonia gas and silver nitrate solution and was used to increase the CL intensity of the proposed system. The enhancement of CL intensity was linear with the concentration of GFX added. Effects of different experimental parameters were studied. Under the optimal conditions, the linear relationship was established between the concentration range of 1.4 × 10-10-4.5 × 10-8 M, with the correlation coefficient (r2) 02E9999. The limit of detection was found to be 4.6 × 10-11 M. The relative standard deviation obtained was 3.2% for six replicate measurements of GFX (1.2 × 10-9 M). The proposed CL method was applied to the commercial drug and the result was in agreement with the labelled amount. The technique was further adopted to the analysis of GFX in spiked urine samples. Negligible interference was found (variation in CL intensity <5%) from a few common foreign excipients applied in preparation of pharmaceutical drug. The comparative results with a few reported methods indicates that the proposed method is more sensitive than other methods..