Background: Molnupiravir was granted approval by the UKS medicines and health product regulatory agency on 04 November 2021 and on 23 December 2021, granted emergency use of authorization by FDA. Objective: Provide a technique for measuring Molnupiravir in active pharmaceutical ingredients and formulations. Method: The wavelength maximum was found to be 236 nm. ICH guidelines were followed. The forced degradation study in the form of acidic, alkali, thermal, photolytic, hydrolytic, and oxidative stress conditions was carried out for Molnupiravir. Results: The method was linear, as measured by a coeffi cient of correlation (R2) of 0.9991 in the 10 to 50 μg/mL range. The %RSD for precision, accuracy, limit of detection (LoD), limit of quantitation (LoQ), ruggedness, and robustness was within acceptable limits per ICH Q2 (R1). Conclusion: HPLC equipped with a UV detector is used to create and verify the proposed method. An acetonitrile mobile phase component of 20% was used, demonstrating the more cost-eff ective technique. The extensive data of mobile phase optimization gives a complete idea of fi nal chromatographic conditions, which can be further implemented for future analysis. Molnupiravir shows less than 4% degradation under diff erent stress conditions. The forced degradation data helps show stability, indicating the behavior of Molnupiravir.
New medication combinations are introduced every day. As a result, various diseases and disorders are treated using a combination of several therapeutic medicines that each have a somewhat distinct mechanism of action. Therefore, it is crucial to develop methods of analyzing medicines employing a range of methods that may be utilized. A UV 730d (dad) absorbance detector, a 20 L injection loop, a sp 930d pump, a 4.6 by 100 mL C18 column (Agilent), and Chemstation software are all included in the setup: approximately 60 water and 40% methanol (pH 3.0 adjust with OPA). Maximum effi ciency was achieved when the system was operated at a wavelength of 233 nm. The procedure’s effi cacy was confi rmed by testing it against ICH guidelines. These techniques were found to be linear, precise, broad, and stable. The procedure was found to be easy, accurate, exact, aff ordable, and easy to use again and again. This means that olmesartan and hydrochlorothiazide, in both bulk form and fi nished products, can be tested for quality using the proposed methodologies.
Background: Achieving a predictable degree of quality with intended and planned specifications is known as "quality by design." QbD (Quality-by-Design) is an alternative to conventional method development that places more attention on identifying and mitigating potential risks. Component of the Quality-by-Design methodology involves conducting a series of experiments to learn how various factors, including the dependant variables, affect the answers of interest. Here, we use a QbD (Quality-by-Design) loom to detail the creation and verification of a stability-indicating high-performance liquid chromatography (HPLC) method for Fostemsavir in both bulk and finished-goods forms. Results: In this work, we present a workable experimental design for optimising the RP-HPLC separation technique by identifying the optimum mobile phase concentration and flow rate. Below are the ideal chromatographic conditions as calculated by Design Expert version 13.0: Mobile phase: 80 parts acetonitrile to 20 parts formic acid (v/v), flow rate: 0.8 millilitres per minute, retention time: 3.24 minutes, column dimensions: GIST C18 (250 mm × 4.6 mm × 5.0 μm). Here we propose a practical experimental layout for determining the optimal mobile phase concentration and flow rate for the RP-HPLC separation technique. Using Design Expert version 13.0, the optimum chromatographic conditions were determined to be as follows: Shim-pack GIST C18 (250 mm 4.6 mm, 5.0 μ), mobile phase acetonitrile to 1% formic acid (80:20, v/v), flow rate 0.8 ml/min, and retention period 3.24 min. At a detection wavelength of 266 nm, it was discovered that the devised technique was linear over a concentration range of 50-90 μg/ml (r2 = 0.997). Test parameters for the system's appropriateness were determined to be 1.124 for the tailing factor and 9480 for the theoretical plates. Intraday RSD was found to range from 0.70 to 0.94, whereas interday RSD was found to range from 0.55 to 0.95 percent. Values for robustness were under 2%. The solution stability % RSD was calculated to be 0.83. The result of the assay was 100.05 percent. The created methodologies were used to studies of forced degradation, and the stressed materials were analysed. The parameters used to validate the procedure fell within the acceptable range recommended by ICH. Conclusion: Using Design Expert 13.0, we created a central composite design experiment that illustrates the relationships between mobile phase and flow rate across three levels, with retention duration, tailing factor, as well as theoretical plates as the responses of interest. By this work, we gain insight into the variables that affect chromatographic separation and strengthen our conviction that the HPLC method we've devised will serve our needs. Quantitative method development was applied to improve comprehension of multi-tiered method variables.
For the determination of the assay of voriconazole in bulk and in pharmaceutical dosage forms, a novel stability indicating RP-HPLC method was designed and validated, exhibiting a very low run time. The stability-indicating nature of the approach is supported by the fact that it is unique, quick, precise, accurate, and capable of isolating the voriconazole peak from any contaminating or degrading components. Isocratic elution on a 100 mm x 4.6 mm, 3μm agilent C18 column at 45°C and a UV detection wavelength of 256 nm constitutes the analytical procedure at at a flow rate of 1.0 mL/min. After injecting 20µL of voriconazole sample, the elution peak occurred at 3.5 minutes, and the entire run time was 15 minutes. Between 98% and 102% was a reasonable range for the percentage of recovery. It was determined that the method's RSD for precision and accuracy was less than 2%. The method has been verified for routine analysis of voriconazole in bulk materials and its formulations according to the standards established by the International Conference on Harmonization (ICH).
High performance thin layer chromatography (HPTLC) and Ultra-High-Performance Liquid Chromatography (UHPLC) techniques were developed and validated to quantify Withanolide in extract and formulation. On Al-backed silica gel 60 F254 TLC plates (10 cm × 10 cm, layer thickness 0.2 mm), which had been prewashed with methanol, HPTLC separation was carried out. Dichloromethane: Methanol: Toluene: Acetone in various ratios produced good separation in mobile phase (5:1:1:0.5 v/v). Camag TLC scanner densitometric scanning at 365 nm determined and quantified. This approach produced compact Withanolide spots at Rf 0.48. ICH guidelines verified HPTLC's precision, reproducibility, and accuracy. Withanolide linearity was 500-3000 ng/spot with R2= 0.9994. LOD & LOQ were found to be 9.48 & 28.73 ng respectively. For UHPLC, Cosmosil C18 was used with acetonitrile: water (0.2 % OPA) (70:30, v/v) mobile phase. Flow rate was 1.5 mL/min. Under optimal chromatographic conditions, Withanolide was retained for 5.9 min and detected at 254 nm. ICH guidelines verified UHPLC's precision, repeatability, and accuracy. Withanolide linearity was 10-60 μg/mL with R2= 0.9994. LOD along with LOQ were 0.411 and 1.245 μg. HPTLC and UHPLC procedures utilized for regular quality control and quick screening of active components from plant extracts.
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