Development of an eco-friendly UPLC method for simultaneous quantification of six selected phosphodiesterase-5 inhibitors and serotonin reuptake inhibitors in pharmaceutical formulations and adulterated food using a quality by design approach

Abstract This study introduces an innovative, environmentally sustainable ultra-performance liquid chromatography (UPLC) method with UV detection for the concurrent quantification of six clinically relevant pharmaceuticals—vardenafil, avanafil, sildenafil, dapoxetine, duloxetine, and tadalafil—frequ...

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Main Authors: Heba Abdel-Hafeez Mohamed, Mohamed Badawi NourEldin, Asmaa Ahmed El-Zaher, Sally Tarek Mahmoud
Format: Article
Language:English
Published: SpringerOpen 2025-06-01
Series:Future Journal of Pharmaceutical Sciences
Subjects:
Online Access:https://doi.org/10.1186/s43094-025-00824-4
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author Heba Abdel-Hafeez Mohamed
Mohamed Badawi NourEldin
Asmaa Ahmed El-Zaher
Sally Tarek Mahmoud
author_facet Heba Abdel-Hafeez Mohamed
Mohamed Badawi NourEldin
Asmaa Ahmed El-Zaher
Sally Tarek Mahmoud
author_sort Heba Abdel-Hafeez Mohamed
collection DOAJ
description Abstract This study introduces an innovative, environmentally sustainable ultra-performance liquid chromatography (UPLC) method with UV detection for the concurrent quantification of six clinically relevant pharmaceuticals—vardenafil, avanafil, sildenafil, dapoxetine, duloxetine, and tadalafil—frequently employed in the management of erectile dysfunction and premature ejaculation. This study employs quality by design (QbD) concepts to optimize chromatographic settings, assuring good selectivity, precision, and resilience, while conforming to green analytical chemistry standards, in contrast to previously published approaches. A face-centered composite design was utilized to systematically optimize critical parameters, resulting in effective separation using a reversed-phase C18 column, an acetate buffer (pH 3), and a mobile phase composed of buffer and methanol (72.5:27.5, v/v) at a flow rate of 0.5 mL/min. The new approach exhibited significant sensitivity and robustness in pharmaceutical dosage forms and contaminated food samples, especially in identifying illicit sildenafil and tadalafil adulteration in honey-based products. The proposed approach was thoroughly validated in accordance with ICH principles, satisfying analytical performance criteria for linearity, precision, accuracy, and robustness. The method's environmental impact was assessed using AGREE metrics, validating its adherence to green analytical chemistry standards. This approach, characterized by its swift analysis time, low solvent usage, and exceptional separation efficiency, serves as a significant analytical instrument for quality control laboratories, pharmaceutical analysis, and food safety monitoring.
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spelling doaj-art-41e8e300ac2148deada2f2c66fffda122025-08-20T02:31:03ZengSpringerOpenFuture Journal of Pharmaceutical Sciences2314-72532025-06-0111111410.1186/s43094-025-00824-4Development of an eco-friendly UPLC method for simultaneous quantification of six selected phosphodiesterase-5 inhibitors and serotonin reuptake inhibitors in pharmaceutical formulations and adulterated food using a quality by design approachHeba Abdel-Hafeez Mohamed0Mohamed Badawi NourEldin1Asmaa Ahmed El-Zaher2Sally Tarek Mahmoud3Egyptian Drug Authority (EDA)Egyptian Drug Authority (EDA)Pharmaceutical Chemistry Department, Faculty of Pharmacy, Cairo UniversityPharmaceutical Chemistry Department, Faculty of Pharmacy, Cairo UniversityAbstract This study introduces an innovative, environmentally sustainable ultra-performance liquid chromatography (UPLC) method with UV detection for the concurrent quantification of six clinically relevant pharmaceuticals—vardenafil, avanafil, sildenafil, dapoxetine, duloxetine, and tadalafil—frequently employed in the management of erectile dysfunction and premature ejaculation. This study employs quality by design (QbD) concepts to optimize chromatographic settings, assuring good selectivity, precision, and resilience, while conforming to green analytical chemistry standards, in contrast to previously published approaches. A face-centered composite design was utilized to systematically optimize critical parameters, resulting in effective separation using a reversed-phase C18 column, an acetate buffer (pH 3), and a mobile phase composed of buffer and methanol (72.5:27.5, v/v) at a flow rate of 0.5 mL/min. The new approach exhibited significant sensitivity and robustness in pharmaceutical dosage forms and contaminated food samples, especially in identifying illicit sildenafil and tadalafil adulteration in honey-based products. The proposed approach was thoroughly validated in accordance with ICH principles, satisfying analytical performance criteria for linearity, precision, accuracy, and robustness. The method's environmental impact was assessed using AGREE metrics, validating its adherence to green analytical chemistry standards. This approach, characterized by its swift analysis time, low solvent usage, and exceptional separation efficiency, serves as a significant analytical instrument for quality control laboratories, pharmaceutical analysis, and food safety monitoring.https://doi.org/10.1186/s43094-025-00824-4Green chemistryQuality by designUPLCErectile dysfunction drugPowder and dosage separation
spellingShingle Heba Abdel-Hafeez Mohamed
Mohamed Badawi NourEldin
Asmaa Ahmed El-Zaher
Sally Tarek Mahmoud
Development of an eco-friendly UPLC method for simultaneous quantification of six selected phosphodiesterase-5 inhibitors and serotonin reuptake inhibitors in pharmaceutical formulations and adulterated food using a quality by design approach
Future Journal of Pharmaceutical Sciences
Green chemistry
Quality by design
UPLC
Erectile dysfunction drug
Powder and dosage separation
title Development of an eco-friendly UPLC method for simultaneous quantification of six selected phosphodiesterase-5 inhibitors and serotonin reuptake inhibitors in pharmaceutical formulations and adulterated food using a quality by design approach
title_full Development of an eco-friendly UPLC method for simultaneous quantification of six selected phosphodiesterase-5 inhibitors and serotonin reuptake inhibitors in pharmaceutical formulations and adulterated food using a quality by design approach
title_fullStr Development of an eco-friendly UPLC method for simultaneous quantification of six selected phosphodiesterase-5 inhibitors and serotonin reuptake inhibitors in pharmaceutical formulations and adulterated food using a quality by design approach
title_full_unstemmed Development of an eco-friendly UPLC method for simultaneous quantification of six selected phosphodiesterase-5 inhibitors and serotonin reuptake inhibitors in pharmaceutical formulations and adulterated food using a quality by design approach
title_short Development of an eco-friendly UPLC method for simultaneous quantification of six selected phosphodiesterase-5 inhibitors and serotonin reuptake inhibitors in pharmaceutical formulations and adulterated food using a quality by design approach
title_sort development of an eco friendly uplc method for simultaneous quantification of six selected phosphodiesterase 5 inhibitors and serotonin reuptake inhibitors in pharmaceutical formulations and adulterated food using a quality by design approach
topic Green chemistry
Quality by design
UPLC
Erectile dysfunction drug
Powder and dosage separation
url https://doi.org/10.1186/s43094-025-00824-4
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AT mohamedbadawinoureldin developmentofanecofriendlyuplcmethodforsimultaneousquantificationofsixselectedphosphodiesterase5inhibitorsandserotoninreuptakeinhibitorsinpharmaceuticalformulationsandadulteratedfoodusingaqualitybydesignapproach
AT asmaaahmedelzaher developmentofanecofriendlyuplcmethodforsimultaneousquantificationofsixselectedphosphodiesterase5inhibitorsandserotoninreuptakeinhibitorsinpharmaceuticalformulationsandadulteratedfoodusingaqualitybydesignapproach
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