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A novel, simple, sensitive and stability-indicating reverse-phase high-performance liquid chromatography (RP-HPLC) method was developed and validated for the quantitative determination of the geometric isomer (Trans) and other related substances in the active pharmaceutical ingredient (API) of Tafluprost (TFL), with their determination by an assay. A chromatographic separation of TFL and its impurities was achieved with a C18 analytical column, using gradient elution with mobile phase A consisting of a mixture of water, methanol and orthophosphoric acid (900:100:1, v/v) and mobile phase B consisting of a mixture of acetonitrile and water (900:100, v/v). The instrumental settings included a flow rate of 1.0 mL/min for related substances and 1.2 mL/min for the assay, a column temperature of 50°C and a detector wavelength of 210 nm, using a photodiode array detector. TFL was exposed to thermal, photolytic, hydrolytic and oxidative stress conditions and the stressed samples were analyzed by the proposed method. Peak homogeneity data of TFL were obtained by using a photodiode array detector in the stressed sample chromatograms, which demonstrated the specificity of the method for estimation in the presence of degradants. The developed method was validated for parameters such as precision, accuracy, linearity, limit of detection, limit of quantification, ruggedness and robustness as per ICH guidelines.

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A capillary gas chromatographic method using mass spectrometric detection was developed and validated for the trace analysis (ppm level) of methyl methane sulfonate and ethyl methane sulfonate in pharmaceutical drug substances. The method utilizes a capillary column (DB-624) with 6% cyanopropyl phenyl and 94% dimethyl polysiloxane stationary phase. A dissolve-and-injection approach was adopted for sample introduction in a split less mode. Mixture of (80:20) ratio of methanol and chloroform was used as a diluent or sample solvent. A limit of detection of about 0.17 μg/g (0.17 ppm) for methyl methane sulfonate and 0.18 μg/g (0.18 ppm) for ethyl methane sulfonate were achieved and limit of quantitation of 0.52 μg/g (0.52 ppm) for methyl methane sulfonate and 0.54 μg/g (0.54 ppm) for ethyl methane sulfonate were achieved for alkyl sulfonates in drug substance samples.