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利用归一化和因子化光谱的新型吸收性中心方法,结合内置分光光度计软件,分析不同基质中重叠光谱的混合物。

Novel absorptivity centering method utilizing normalized and factorized spectra for analysis of mixtures with overlapping spectra in different matrices using built-in spectrophotometer software.

机构信息

Pharmaceutical Chemistry Department, Faculty of Pharmaceutical Sciences & Pharmaceutical Industries, Future University in Egypt, Cairo, Egypt.

Analytical Chemistry Department, Faculty of Pharmacy, Cairo University, Kasr El-Aini Street, Cairo, Egypt.

出版信息

Spectrochim Acta A Mol Biomol Spectrosc. 2018 Jul 5;200:167-178. doi: 10.1016/j.saa.2018.04.004. Epub 2018 Apr 7.

Abstract

A novel, simple, rapid, accurate, and economical spectrophotometric method, namely absorptivity centering (a-Centering) has been developed and validated for the simultaneous determination of mixtures with partially and completely overlapping spectra in different matrices using either normalized or factorized spectrum using built-in spectrophotometer software without a need of special purchased program. Mixture I (Mix I) composed of Simvastatin (SM) and Ezetimibe (EZ) is the one with partial overlapping spectra formulated as tablets, while mixture II (Mix II) formed by Chloramphenicol (CPL) and Prednisolone acetate (PA) is that with complete overlapping spectra formulated as eye drops. These procedures do not require any separation steps. Resolution of spectrally overlapping binary mixtures has been achieved getting recovered zero-order (D) spectrum of each drug, then absorbance was recorded at their maxima 238, 233.5, 273 and 242.5 nm for SM, EZ, CPL and PA, respectively. Calibration graphs were established with good correlation coefficients. The method shows significant advantages as simplicity, minimal data manipulation besides maximum reproducibility and robustness. Moreover, it was validated according to ICH guidelines. Selectivity was tested using laboratory-prepared mixtures. Accuracy, precision and repeatability were found to be within the acceptable limits. The proposed method is good enough to be applied to an assay of drugs in their combined formulations without any interference from excipients. The obtained results were statistically compared with those of the reported and official methods by applying t-test and F-test at 95% confidence level concluding that there is no significant difference with regard to accuracy and precision. Generally, this method could be used successfully for the routine quality control testing.

摘要

一种新颖、简单、快速、准确且经济的分光光度法,即吸光度中心法(a-Centering)已经被开发和验证,用于同时测定不同基质中部分和完全重叠光谱的混合物,使用归一化或分解光谱,无需特殊购买的程序,使用内置分光光度计软件。混合物 I(Mix I)由辛伐他汀(SM)和依折麦布(EZ)组成,是片剂形式的部分重叠光谱混合物,而混合物 II(Mix II)由氯霉素(CPL)和醋酸泼尼松龙(PA)组成,是滴眼剂形式的完全重叠光谱混合物。这些程序不需要任何分离步骤。通过获得每种药物的零阶(D)光谱来实现对光谱重叠二元混合物的分辨率,然后在其最大值 238、233.5、273 和 242.5nm 处记录吸光度,分别为 SM、EZ、CPL 和 PA。校准曲线具有良好的相关系数。该方法具有简单、最小的数据处理以及最大的重现性和稳健性等显著优点。此外,它已经根据 ICH 指南进行了验证。使用实验室制备的混合物测试了选择性。发现准确性、精密度和重复性均在可接受范围内。该方法足以应用于其制剂中药物的测定,不会受到赋形剂的干扰。通过在 95%置信水平下应用 t 检验和 F 检验,将获得的结果与报道的和官方方法的结果进行了统计学比较,结论是在准确性和精密度方面没有显著差异。总的来说,该方法可以成功地用于常规质量控制测试。

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