zhpsЖурнал прикладной спектроскопииZhurnal Prikladnoii Spektroskopii0514-7506B. I. Stepanov Institute of Physics of the National Academy of Scienceszhps-715Research ArticleСтатьиОДНОФАКТОРНЫЕ И ХЕМОМЕТРИЧЕСКИЕ ВСПОМОГАТЕЛЬНЫЕ СПЕКТРОФОТОМЕТРИЧЕСКИЕ МЕТОДЫ ОПРЕДЕЛЕНИЯ ФЛИБАНСЕРИНА В ЛЕКАРСТВЕННОЙ ФОРМЕUNIVARIATE AND CHEMOMETRICS-ASSISTED SPECTROPHOTOMETRIC METHODS FOR DETERMINATION OF FLIBANSERIN IN A RECENTLY RELEASED DOSAGE FORMAhmedR. M.AhmedRasha M.

Каир

Cairo

AbdallahI. A.AbdallahInas A.

Садат-Сити

Sadat City

inas.abdallah@fop.usc.edu.egМеждународный университет МисрDepartment of Pharmaceutical Chemistry, Faculty of Pharmacy, Misr International UniversityУниверситет Садат-СитиDepartment of Analytical Chemistry, Faculty of Pharmacy, University of Sadat City202002112020875855(1)-855(10)Copyright © Ahmed R.M., Abdallah I.A., 20202020Ahmed R.M., Abdallah I.A.Ahmed R.M., Abdallah I.A.Данная работа распространяется под лицензией Creative Commons Attribution 4.0.This work is licensed under a Creative Commons Attribution 4.0 License.https://zhps.ejournal.by/jour/article/view/715

Разработаны пять простых, селективных и быстрых спектрофотометрических методов для определения флибансерина (FL) в присутствии продуктов его окислительного разложения (ODP). Стресс-исследования проведены в соответствии с руководящими принципами Международной конференции по гармонизации (ICH) для оценки поведения FL в отношении окислительных, термических и кислотных условий. FL оказался устойчив к термическим и кислотным условиям, в то время как ранее он был подвержен окислительной деструкции. Три спектрофотометрических метода одномерные: третья производная (D3), разность отношений спектров отношения (RD) и отношение первой производной спектров (D1R). Два других метода многомерные: частичный метод наименьших квадратов (PLS) и регрессия главных компонент (PCR), в них не требовалось предварительных этапов разделения. Химическая структура ODP подтверждена с помощью масс-спектрометрии и спектроскопии ЯМР 1Н. Определены линейность, точность и прецизионность. Селективность оценена путем анализа синтетических лабораторных смесей, содержащих различные соотношения FL и его ODP. Статистическое сравнение пяти спектрофотометрических методов не обнаружило никаких существенных различий.

Five simple, selective, and rapid spectrophotometric methods are developed for the determination of flibanserin (FL) in the presence of its oxidative degradation products (ODPs). Stress studies are performed according to the International Conference on Harmonization (ICH) guidelines to assess the behavior of FL against oxidative, thermal, and acidic conditions. FL was stable against thermal and acidic conditions, while it was susceptible to oxidative degradation. Three of the spectrophotometric methods were univariate methods, namely, third derivative (D3), ratio difference of ratio spectra (RD), and first derivative ratio of spectra (D1R), while the other two methods were multivariate methods, namely, partial least square (PLS) and principal components regression (PCR). No preliminary separation steps were required in these methods. The chemical structures of the ODPs were confirmed using mass spectrometry and 1H NMR spectroscopy. The proposed methods were developed and validated according to the ICH guidelines. The linearity, accuracy, and precision were determined, and the selectivity was assessed by analyzing synthetic laboratory mixtures containing different ratios of FL and its ODPs. Statistical comparisons were applied to the five spectrophotometric methods, and no significant differences were found. The validated methods could be applied for routine testing and quality control.

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The authors declare that there are no conflicts of interest present.