连续小波变换与多元校正法用于同时分光光度测定药物制剂和生物样本中坦索罗辛和索利那新
Comparative Study of Continuous Wavelet Transform and Multivariate Calibration for the Simultaneous Spectrophotometric Determination of Tamsulosin and Solifenacin in Pharmaceutical Formulation and Biological Sample.
作者信息
Ashrafi Nazanin, Sohrabi Mahmoud Reza, Saber Tehrani Mandana
机构信息
Islamic Azad University, Department of Chemistry, North Tehran Branch, Vafadar Blvd., Shahid Sadoughi St., Hakimiyeh Exit, Shahid Babaee Highway, Tehran 1651153311, Iran.
出版信息
J AOAC Int. 2023 Nov 2;106(6):1620-1628. doi: 10.1093/jaoacint/qsad065.
BACKGROUND
Spectrophotometry alone is not applicable for the simultaneous determination of drugs in a multicomponent pharmaceutical formulation owing to their overlap.
OBJECTIVE
In this study, the combination of UV-Vis spectrophotometry and chemometric methods, including continuous wavelet transform (CWT) and partial least-squares (PLS) was presented for the simultaneous estimation of tamsulosin (TAM) and solifenacin (SOL) in synthetic mixtures, commercial formulations, and a biological sample.
METHODS
The simultaneous spectrophotometric determination of TAM and SOL in binary mixtures, a real sample, and a biological sample was performed by applying CWT and PLS approaches.
RESULTS
In the CWT method, two various wavelet families named Daubechies (db2) at wavelength 223 nm and Biorthogonal (bior1.3) at wavelength 227 nm based on the appropriate zero-crossing point were selected for TAM and SOL, respectively. The linear ranges of TAM and SOL were 0.25-4 μg/mL and 10-30 μg/mL, respectively. The LODs were 0.0459 μg/mL and 0.2085 μg/mL, while the LOQs were 0.3208 μg/mL and 0.6495 μg/mL for TAM and SOL, respectively. The average recovery values of 18 mixtures were 98.28% and 97.79% for TAM and SOL, respectively. Also, the root mean square error (RMSE) of both components was lower than 2.3. Based on the k-fold cross-validation in the PLS approach, the optimum number of components related to TAM and SOL were 9 and 5 with a mean square error prediction (MSEP) of 0.0153 and 0.0370, respectively. The mean recovery values of the test set were found to be 100.09% for TAM and 99.95% for SOL where RMSE values were 0.0064 and 0.0169 for TAM and SOL, respectively.
CONCLUSION
Analysis of variance (ANOVA) was applied to the results of the real sample and there was no significant difference between the proposed methods and HPLC as a reference technique. The result obtained revealed that the proposed methods were found to be fast, facile, economical, and precise, and provide a suitable alternative to the HPLC technique for the concurrent determination of TAM and SOL in QC laboratories.
HIGHLIGHTS
UV-Vis spectrophotometry combined with CWT and PLS was developed. Simultaneous analysis of TAM and SOL was performed using the proposed approaches. These methods were implemented on synthetic mixtures, commercial formulations, and a biological sample. ANOVA test was used to compare the suggested methods and the HPLC technique.
背景
由于多组分药物制剂中药物的重叠，分光光度法不适用于同时测定药物。
目的
本研究将紫外-可见分光光度法与化学计量学方法（包括连续小波变换（CWT）和偏最小二乘（PLS））相结合，用于同时估算合成混合物、商业制剂和生物样品中的坦索罗辛（TAM）和索利那新（SOL）。
方法
通过应用 CWT 和 PLS 方法，对 TAM 和 SOL 在二元混合物、实际样品和生物样品中的同时分光光度测定。
结果
在 CWT 方法中，分别选择基于适当的过零点的两种不同的小波家族，即 Daubechies（db2）在波长 223nm 和 Biorthogonal（bior1.3）在波长 227nm，用于 TAM 和 SOL。TAM 和 SOL 的线性范围分别为 0.25-4μg/mL 和 10-30μg/mL。TAM 和 SOL 的检测限分别为 0.0459μg/mL 和 0.2085μg/mL，定量限分别为 0.3208μg/mL 和 0.6495μg/mL。对于 TAM 和 SOL，18 个混合物的平均回收率值分别为 98.28%和 97.79%。此外，两种成分的均方根误差（RMSE）均低于 2.3。基于 PLS 方法中的 k 折交叉验证，与 TAM 和 SOL 相关的最佳组件数分别为 9 和 5，均方误差预测（MSEP）分别为 0.0153 和 0.0370。测试集的平均回收率值分别为 TAM 的 100.09%和 SOL 的 99.95%，其中 TAM 和 SOL 的 RMSE 值分别为 0.0064 和 0.0169。
结论
对实际样品的结果进行方差分析（ANOVA），结果表明所提出的方法与 HPLC 作为参考技术之间无显著性差异。结果表明，所提出的方法快速、简便、经济、准确，为 QC 实验室中 TAM 和 SOL 的同时测定提供了一种合适的 HPLC 替代方法。
重点
建立了紫外-可见分光光度法与 CWT 和 PLS 的结合。采用所提出的方法同时分析 TAM 和 SOL。这些方法已应用于合成混合物、商业制剂和生物样品。采用 ANOVA 检验比较建议的方法和 HPLC 技术。
Zotero 插件