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Quantitative analysis of aspirin in tablets using attenuated total refletance FTIS with full spectrum PLS algorithms

By: Yau, Xin Y.
Contributor(s): Lokesh, V. V. S.
Publisher: Mumbai Indian Drug Manufacture's Association - IDMA 2019Edition: Vol.56(10), Oct.Description: 50-56p.Subject(s): PHARMACEUTICSOnline resources: Click here In: Indian drugsSummary: Acetyl salicylic acid (ASA) is widely used globally to treat pain, rheumatic fever and inflammation since more than a century. It is also a prototypical molecule categorized as a platelet aggregation inhibitor, that could be widely used to reduce the risk of arterial and venous thrombosis in long term therapy. Various ASA formulations are available in the market and estimation of their quantity and efficacy is of utmost importance since it is largely being produced by many pharmaceutical companies all over the world. Literature is supported with many analytical methods using UV-visible spectrophotometer, liquid chromatography, liquid chromatography integrated with mass spectrometer (LC-MS), UHPLCMS/MS, Gas chromatography, electrochemical and titrimetric methods. In this study, an Attenuated total Reflectance Fourier transform Infrared Spectroscopy (ATR-FTIR) method was developed for the estimation of ASA in tablets and validated as per ICH guidelines. The calibration curve was constructed on peak height location at a specific wavenumber of 1750 cm-1 (Strong c=O stretching vibration of ASA) in the concentration range from 1-100 (%w/w) with a correlation coefficient of 1.000. the limit of detection (LOD) and limit of quantification (LOQ) were 0.94 (%w/w) and 0.31 (%w/w), respectively. the method was found to be precise over a range of 10- 100%, with intra-day and inter-day precision values were estimated as 0.94 and 8.26 respectively. The percentage of mean recovery was estimated at 103.04 ±2.58 with margin of error (± 2.50%) at 95% confidence interval. This new method was used for the quantification of ASA in tablets and percentage of labeled amount was found within the range of 103.04 ±2.58. No significant interference was observed by excipients in the tablet formulation during the spectral analysis.
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Acetyl salicylic acid (ASA) is widely used globally to treat pain, rheumatic fever and inflammation since more than a century. It is also a prototypical molecule categorized as a platelet aggregation inhibitor, that could be widely used to reduce the risk of arterial and venous thrombosis in long term therapy. Various ASA formulations are available in the market and estimation of their quantity and efficacy is of utmost importance since it is largely being produced by many pharmaceutical companies all over the world. Literature is supported with many analytical methods using UV-visible spectrophotometer, liquid chromatography, liquid chromatography integrated with mass spectrometer (LC-MS), UHPLCMS/MS, Gas chromatography, electrochemical and titrimetric methods. In this study, an Attenuated total Reflectance Fourier transform Infrared Spectroscopy (ATR-FTIR) method was developed for the estimation of ASA in tablets and validated as per ICH guidelines. The calibration curve was constructed on peak height location at a specific wavenumber of 1750 cm-1 (Strong c=O stretching vibration of ASA) in the concentration range from 1-100 (%w/w) with a correlation coefficient of 1.000. the limit of detection (LOD) and limit of quantification (LOQ) were 0.94 (%w/w) and 0.31 (%w/w), respectively. the method was found to be precise over a range of 10- 100%, with intra-day and inter-day precision values were estimated as 0.94 and 8.26 respectively. The percentage of mean recovery was estimated at 103.04 ±2.58 with margin of error (± 2.50%) at 95% confidence interval. This new method was used for the quantification of ASA in tablets and percentage of labeled amount was found within the range of 103.04 ±2.58. No significant interference was observed by excipients in the tablet formulation during the spectral analysis.

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