DEVELOPMENT OF A FAST LIQUID CHROMATOGRAPHY METHOD WITH A CHEMOMETRIC APPROACH BASED ON BOX-BEHNKEN DESIGN FOR THE DETERMINATION OF ANTIDEPRESSANTS IN PHARMACEUTICAL FORMULATIONS

Ankara Universitesi Eczacilik Fakultesi Dergisi Pub Date : 2024-04-01 DOI:10.33483/jfpau.1425340

Sercan Yıldırım, Tuğçe Özyiğit

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Abstract

Objective: The objective of this work was to develop a liquid chromatographic method for the quantification of antidepressants, namely duloxetine (DXN), fluoxetine (FXN), citalopram (CIT), paroxetine (PXN), and sertraline (SRN), by a chemometric approach based on Box-Behnken design. Material and Method: After initial experiments to determine significant parameters, a Box-Behnken design consisting of 17 experiment sets was carried out. All separations were conducted using an Agilent Poroshell 120 EC-C18 analytical column (75 mm × 4.6 mm × 2.7 µm). Result and Discussion: The optimum levels of pH, acetonitrile ratio, and flow rate were determined with the desirability function as 2.7, 38%, and 1.1 ml/min, respectively. The differences (<8%) between predicted optimum responses and experimentally obtained results proved the model's suitability. Limits of detection and limits of quantification values were in the ranges of 0.17-0.29 µg/ml and 0.53-0.89 µg/ml, respectively. The feasibility of the technique was proven by analyzing PXN and DXN formulations.

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基于方框-贝肯设计的化学计量学方法开发快速液相色谱法，用于测定药物制剂中的抗抑郁药

研究目的本研究的目的是通过基于方框-贝肯设计的化学计量学方法，建立一种液相色谱法，用于定量分析抗抑郁药物，即度洛西汀（DXN）、氟西汀（FXN）、西酞普兰（CIT）、帕罗西汀（PXN）和舍曲林（SRN）：经过初步实验确定重要参数后，进行了由 17 组实验组成的盒-贝肯设计。所有分离均使用 Agilent Poroshell 120 EC-C18 分析柱（75 mm × 4.6 mm × 2.7 µm）。结果与讨论用可取函数确定的最佳 pH 值、乙腈比例和流速分别为 2.7、38% 和 1.1 ml/min。预测的最佳反应与实验结果之间的差异（<8%）证明了该模型的适用性。检测限和定量限分别为 0.17-0.29 µg/ml 和 0.53-0.89 µg/ml。通过分析 PXN 和 DXN 制剂，证明了该技术的可行性。

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Ankara Universitesi Eczacilik Fakultesi Dergisi

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