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使用比率光谱导数分光光度法和化学计量学方法同时分光光度法测定药物制剂中甲芬那酸和对乙酰氨基酚的含量。

Simultaneous spectrophotometric determination of mefenamic acid and paracetamol in a pharmaceutical preparation using ratio spectra derivative spectrophotometry and chemometric methods.

作者信息

Dinç Erdal, Yücesoy Cem, Onur Feyyaz

机构信息

Department of Analytical Chemistry, Faculty of Pharmacy, University of Ankara, 06100 Tandoğan, Ankara, Turkey.

出版信息

J Pharm Biomed Anal. 2002 Jun 15;28(6):1091-100. doi: 10.1016/s0731-7085(02)00031-6.

Abstract

Four new methods are described for the simultaneous determination of mefenamic acid (MEF) and paracetamol (PAR) in their combination. In the first method, ratio spectra derivative method, analytical signals were measured at the wavelengths corresponding to either maximums or minimums for both drugs in the first derivative spectra of the ratio spectra obtained by dividing the standard spectrum of one of two drugs in 0.1 M NaOH:methanol (1:9). In the chemometric techniques, classical least-squares, inverse least-squares and principal component regression (PCR), the training was randomly prepared by using the different mixture compositions containing two drugs in 0.1 M NaOH:methanol (1:9). The absorbance data was obtained by the measurements at 13 points in the wavelength range 235-355 nm in the absorption spectra. Chemometric calibrations were constructed by the absorbance data and training set for the prediction of the amount of MEF and PAR in samples. In the third chemometric method, PCR, the covariance matrix corresponding to the absorbance data was calculated for the basis vectors and matrix containing the new coordinates. The obtained calibration was used to determine the title drugs in their mixture. Linearity range in all the methods was found to be 2-10 microg/ml of MEF and 4-20 microg/ml of PAR. Mean recoveries were found satisfactory (>99%). The procedures do not require any separation step. These methods were successfully applied to a pharmaceutical formulation, tablet, and the results were compared with each other.

摘要

本文描述了四种同时测定甲芬那酸(MEF)和对乙酰氨基酚(PAR)复方制剂中这两种药物含量的新方法。第一种方法为比率光谱导数法,通过将两种药物之一的标准光谱在0.1 M NaOH:甲醇(1:9)中进行除法运算得到比率光谱,然后在该比率光谱的一阶导数光谱中,于两种药物各自对应的最大或最小波长处测量分析信号。在化学计量学技术方面,采用经典最小二乘法、逆最小二乘法和主成分回归(PCR),通过使用含有0.1 M NaOH:甲醇(1:9)中两种药物的不同混合组成随机制备训练集。在235 - 355 nm波长范围内的吸收光谱中,于13个点进行测量获取吸光度数据。利用吸光度数据和训练集构建化学计量校准模型,以预测样品中甲芬那酸和对乙酰氨基酚的含量。在第三种化学计量学方法即PCR中,计算对应吸光度数据的协方差矩阵以得到基向量和包含新坐标的矩阵。所得校准模型用于测定混合物中上述两种目标药物的含量。所有方法的线性范围均为甲芬那酸2 - 10 μg/ml、对乙酰氨基酚4 - 20 μg/ml。平均回收率令人满意(>99%)。这些方法无需任何分离步骤。这些方法已成功应用于一种药物制剂片剂,并对结果进行了相互比较。

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