A Simple, Sensitive, and Greener HPLC-DAD Method for the Simultaneous Analysis of Two Novel Orexin Receptor Antagonists.

Iqbal, M; Haq, N; Kalam, MA; Imam, F; Shakeel, F

A Simple, Sensitive, and Greener HPLC-DAD Method for the Simultaneous Analysis of Two Novel Orexin Receptor Antagonists.

Iqbal, M Haq, N Kalam, MA Imam, F Shakeel, F

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Publisher:: American Chemical Society (ACS)
Publication Type:: Journal Article
Citation:: ACS Omega, 2024, 9, (21), pp. 23101-23110
Issue Date:: 2024-05-28

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Field	Value	Language
dc.contributor.author	Iqbal, M
dc.contributor.author	Haq, N
dc.contributor.author	Kalam, MA
dc.contributor.author	Imam, F
dc.contributor.author	Shakeel, F
dc.date.accessioned	2024-08-21T03:37:46Z
dc.date.available	2024-05-09
dc.date.available	2024-08-21T03:37:46Z
dc.date.issued	2024-05-28
dc.identifier.citation	ACS Omega, 2024, 9, (21), pp. 23101-23110
dc.identifier.issn	2470-1343
dc.identifier.issn	2470-1343
dc.identifier.uri	http://hdl.handle.net/10453/180434
dc.description.abstract	The orexin receptor antagonist (ORA) is one of the new psychopharmacological agents used in the treatment of insomnia. There are currently no documented greener high-performance liquid chromatography-diode array detector (HPLC-DAD) methods for the analysis of ORA antagonists, lemborexant (LMB) and suvorexant (SUV) simultaneously. Therefore, in this study, a simple, sensitive, and greener HPLC-DAD method has been developed for the simultaneous quantitative analysis of LMB and SUV in bulk and laboratory-prepared mixture. The developed method was validated for numerous validation parameters and evaluated for greenness. The C18 Waters Spherisorb CN (4.6 × 250 mm2; 5 μm) column was used for the chromatographic separation. The mobile phase composition was ethanol: 10 mM KH2PO4 buffer in a ratio of (60:40 v/v). The DAD detection was performed at 253 nm using a Waters DAD detector. The greenness was evaluated using the analytical Eco-Scale (AES), ChlorTox, and analytical GREEnness (AGREE) techniques. The calibration curves showed excellent linearity for LMB and SUV between the concentration range of 125-5000 ng/mL and 250-10,000 ng/mL, respectively. In addition, the proposed HPLC-DAD method was accurate, precise, robust, highly sensitive, and greener. AES, ChlorTox, and AGREE scales were predicted by the HPLC-DAD method to be 91, 1.14 g, and 0.79, respectively, showing an excellent greenness profile. The greener HPLC-DAD method was successfully used to analyze both medicines quantitatively in bulk and laboratory-prepared synthetic mixtures. The findings of this study indicated that the proposed HPLC-DAD method may be consistently applied to evaluate LMB and SUV in bulk and dosage forms.
dc.format	Electronic-eCollection
dc.language	eng
dc.publisher	American Chemical Society (ACS)
dc.relation.ispartof	ACS Omega
dc.relation.isbasedon	10.1021/acsomega.4c03976
dc.rights	info:eu-repo/semantics/closedAccess
dc.subject	0904 Chemical Engineering, 0912 Materials Engineering
dc.subject.classification	3403 Macromolecular and materials chemistry
dc.subject.classification	3406 Physical chemistry
dc.subject.classification	4004 Chemical engineering
dc.title	A Simple, Sensitive, and Greener HPLC-DAD Method for the Simultaneous Analysis of Two Novel Orexin Receptor Antagonists.
dc.type	Journal Article
utslib.citation.volume	9
utslib.location.activity	United States
utslib.for	0904 Chemical Engineering
utslib.for	0912 Materials Engineering
pubs.organisational-group	University of Technology Sydney
pubs.organisational-group	University of Technology Sydney/Faculty of Engineering and Information Technology
pubs.organisational-group	University of Technology Sydney/Faculty of Engineering and Information Technology/School of Civil and Environmental Engineering
pubs.organisational-group	University of Technology Sydney/Strength - CTWW - Centre for Technology in Water and Wastewater Treatment
utslib.copyright.status	closed_access	*
dc.date.updated	2024-08-21T03:37:40Z
pubs.issue	21
pubs.publication-status	Published online
pubs.volume	9
utslib.citation.issue	21

Abstract:

The orexin receptor antagonist (ORA) is one of the new psychopharmacological agents used in the treatment of insomnia. There are currently no documented greener high-performance liquid chromatography-diode array detector (HPLC-DAD) methods for the analysis of ORA antagonists, lemborexant (LMB) and suvorexant (SUV) simultaneously. Therefore, in this study, a simple, sensitive, and greener HPLC-DAD method has been developed for the simultaneous quantitative analysis of LMB and SUV in bulk and laboratory-prepared mixture. The developed method was validated for numerous validation parameters and evaluated for greenness. The C18 Waters Spherisorb CN (4.6 × 250 mm2; 5 μm) column was used for the chromatographic separation. The mobile phase composition was ethanol: 10 mM KH2PO4 buffer in a ratio of (60:40 v/v). The DAD detection was performed at 253 nm using a Waters DAD detector. The greenness was evaluated using the analytical Eco-Scale (AES), ChlorTox, and analytical GREEnness (AGREE) techniques. The calibration curves showed excellent linearity for LMB and SUV between the concentration range of 125-5000 ng/mL and 250-10,000 ng/mL, respectively. In addition, the proposed HPLC-DAD method was accurate, precise, robust, highly sensitive, and greener. AES, ChlorTox, and AGREE scales were predicted by the HPLC-DAD method to be 91, 1.14 g, and 0.79, respectively, showing an excellent greenness profile. The greener HPLC-DAD method was successfully used to analyze both medicines quantitatively in bulk and laboratory-prepared synthetic mixtures. The findings of this study indicated that the proposed HPLC-DAD method may be consistently applied to evaluate LMB and SUV in bulk and dosage forms.

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http://hdl.handle.net/10453/180434