Department of Analytical Chemistry, Faculty of Pharmacy, Ankara University, Ankara, Turkey.
Department of Analytical Chemistry, Faculty of Pharmacy, Ankara University, Ankara, Turkey.
Spectrochim Acta A Mol Biomol Spectrosc. 2020 Apr 5;230:118049. doi: 10.1016/j.saa.2020.118049. Epub 2020 Jan 8.
A three-way analysis method, parallel factor analysis (PARAFAC) model was applied to the pH-absorbance dataset for the simultaneous determination of paracetamol and its acid-base dissociation constant in presence of excipient interference in a syrup formulation without using chemical pretreatment or chromatographic separation step. The UV spectroscopic data matrices of calibration set, validation and unknown samples were obtained from the absorbance measurements at the five different pH media, considering conjugate acid/base properties of the related drug. Their pH-absorbance data matrices were arranged as a cubic data array (wavelength x sample x pH) (425x52x5). Three-way array of pH-absorbance dataset was decomposed into a trilinear set of spectral, pH and relative concentration profiles of paracetamol and excipients in the commercial syrup using PARAFAC model. In the PARAFAC implementation, paracetamol in the commercial syrup formulation and its pKa value were simultaneously predicted from the relative concentration and pH profiles, respectively. In the method validation step of this study, the performance of PARAFAC model was checked by analyzing the validation samples in terms of selectivity, sensitivity, accuracy and precision of the method. The determination results of paracetamol and its pKa value provided from PARAFAC application were compared to those obtained by a newly developed ultra-performance liquid chromatography (UPLC) method, in terms of simplicity, applicability, interpretability with low cost and short analysis time.
采用三向分析方法——平行因子分析（PARAFAC）模型，应用于 pH-吸光度数据集，在糖浆制剂中存在赋形剂干扰的情况下，无需使用化学预处理或色谱分离步骤，同时测定对乙酰氨基酚及其酸碱离解常数。校准集、验证集和未知样品的 UV 光谱数据矩阵是通过在五个不同 pH 介质下测量吸光度获得的，考虑了相关药物的共轭酸碱性质。它们的 pH-吸光度数据矩阵排列为立方数据数组（波长 x 样品 x pH）（425x52x5）。使用 PARAFAC 模型，将 pH-吸光度数据集的三向数组分解为商业糖浆中对乙酰氨基酚和赋形剂的光谱、pH 和相对浓度分布的三线性集。在 PARAFAC 的实现中，分别根据相对浓度和 pH 分布，从商业糖浆制剂中的对乙酰氨基酚及其 pKa 值预测对乙酰氨基酚。在本研究的方法验证步骤中，通过分析验证样品，检查 PARAFAC 模型的选择性、灵敏度、准确性和精密度，以验证该方法的性能。通过与新开发的超高效液相色谱（UPLC）方法相比，从 PARAFAC 应用中获得的对乙酰氨基酚及其 pKa 值的测定结果在简单性、适用性、可解释性、低成本和短分析时间方面进行了比较。
