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QUANTITATIVE ANALYSIS OF ASPIRIN IN TABLETS USING ATTENUATED TOTAL REFLECTANCE FTIR WITH FULL SPECTRUM PLS ALGORITHMS

机译:用衰减总反射率与全谱PLS算法使用减毒总反射FTIR的片剂中阿司匹林的定量分析

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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), UHPLC-MS/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.
机译:乙酰水杨酸(ASA)在全球范围内广泛使用以治疗疼痛,风湿热和炎症以来。它还是作为血小板聚集抑制剂分类的原型分子,其可广泛用于降低长期治疗中动脉和静脉血栓形成的风险。各种ASA配方可在市场上提供,估计其数量和功效是最重要的,因为它主要由世界各地的许多制药公司生产。使用UV可见分光光度计,液相色谱法,与质谱仪(LC-MS),UHPLC-MS / MS,气相色谱,电化学和滴定法集成的许多分析方法支持文献。在该研究中,开发了衰减的总反射率傅里叶变换红外光谱(ATR-FTIR)方法,用于估计片剂中的ASA,并根据ICH指导验证。校准曲线在1750cm〜(-1)(ASA的强C = O拉伸振动的强C = O拉伸振动)的特定波数的峰值高度位置构造为1-100(%w / w),具有相关系数1.000。检测限(LOD)和定量极限(LOQ)分别为0.94(%w / w)和0.31(%w / w)。发现该方法在10-100%的范围内精确,分别估计为0.94和8.26的日期和日间精度值。平均恢复的百分比在103.04±2.58处估计,误差余量(±2.50%),置信区间为95%。该新方法用于量化片剂中的ASA,标记量的百分比在103.04±2.58的范围内。在光谱分析期间,片剂配方中的赋形剂未观察到显着干扰。

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