A simple, accurate, isocratic stability indicating RP‐HPLC method was developed for the determination of Molnupiravir in bulk drug. This RP-HPLC was achieved on “Waters 2695 using an Agilent Zorbax Eclipse C18 (250 mm × 4.6 mm × 5 µm)” column with the mobile phase consisting of 30 mM, ammonium phosphate monobasic and Methanol in the ratio of 47:53 %v/v. The stress testing of Molnupiravir was carried out under acidic, alkaline, oxidative, thermal, and photolytic conditions and formed degradation products were well resolved from Molnupiravir API (active pharmaceutical ingredient). The suggested approach was validated according to ICH (International Council on Harmonisation) principles, and all of the validation parameters' findings were within acceptable limits. The method was proven to be appropriate for quality control of Molnupiravir in bulk and pharmaceutical dose forms, as well as stability testing.
A rapid and sensitive LC-tandem mass spectrometry (LC-MS/MS) method was developed and validated for the quantitative analysis of four potential genotoxic impurities Imp-A (2-chloro-5-nitroaniline), Imp-B (1-chloro-2-iodo-4-nitrobenzene), Imp-C (1-(2-chloro-5-nitrophenyl)ethan-1-one) and Imp-D (2-chloro-5-nitrobenzoic acid) in Vismodegib API drug sample. This trace analysis was achieved on CSH C18, 15.0 cm x 3.0 mm, 1.7 micron column maintained at 45°C. Optimal mobile phase consisted of 0.05% formic acid in water was used as mobile phase A and acetonitrile used as mobile phase B in gradient mode with the flow rate of 0.5 mL/min. The developed method had the short run time of 12 minutes. Quantification of four potential genotoxic impurities were carried out using mass detection with electrospray ionization in multiple reaction monitoring mode. The method was linear in the range of 0.03 ppm to 1.50 ppm for four potential genotoxic impurities with a correlation coefficient not less than 0.999. The recoveries were found satisfactory over the range between 96.67 and 106.90% for all selected impurities. The developed method was able to quantitate all four PGIs at a concentration level of 0.03 ppm (0.03 ppm with respect to 20 mg /mL Vismodegib).
Background: In the current study, asimple and specific stability indicating RP-HPLC method was developed and validated for the determination of Lamivudine and Raltegravir in bulk drug and it tablet dosage form using an UV-detector. Good separation was achieved by isocratic ally on a Zorbax SB-Phenyl (150 × 4.6 mm, 3.5 μ, 80 A°) column, using a mobile phase composition of buffer (0.1% v/v Phosporic acid in water): Acetonitrile (40:60 v/v) at a flow rate of 1.0 mL/min. The eluted analytes detected at 260 nm wavelength. Results: Lamivudine and Raltegravir were eluted at 3.1 and 5.4 min respectively with run time 7 min. Linearity in the method was measured in the concentration range of 30 – 70 μg/mL and 60 – 140 μg/mL for Lamivudine and Raltegravirrespectively. The percentage recoveries of Lamivudine and Raltegravirwere determined to be 100.30% and 100.53%, respectively. The validation of the developed method is carried as per USFDA and ICH guidelines, and the degradants were well resolved from Raltegravir and Lamivudine peaks. The developed RP-HPLC method was highly precise, specific, sensitive, and stability indicating. Conclusion: The results of the analysis prove that thedeveloped RP-HPLC method is simple, economical and widely acceptable, which can be used in routine quality control tests in the industry.
A liquid chromatography with single quadrupole mass detection method was developed for the determination of potential genotoxic impurities (PGIs) in the Iomeprol active pharmaceutical ingredient. Chromatographic separation was achieved on an Agilent Eclipse plus C8 column (100 mm x 2.1 mm x 1.8 μm) with 0.1% formic acid in water as mobile phase A and acetonitrile as mobile phase B in gradient elution mode at a 0.1 mL/min. Executed validation summary demonstrated that the mass detection method had highly sensitive and selective. A linear calibration curve (correlation coefficient, r> 0.999) was attained at the concentration range of 0.1-125 ppm for three PGI’s. The Limit of Detection of Imp-A, Imp-B and Imp-C in drug substance of Iomeprol is 0.05 ppm. The accuracy was confirmed by calculated recoveries (98.4-101.5%). The precision was tested at three levels: injection repeatability, analysis repeatability and intermediate precision. The calculated relative standard deviations were within the specification. The developed method was able to quantitate all three PGI’s at a concentration level of 1 µg/mL.
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