Rapid Determination of Sildenafil and Its Analogues in Dietary Supplements Using Gas Chromatography-Triple Quadrupole Mass Spectrometry

Application of gas chromatography–triple quadrupole mass spectrometry for identification, confirmation and quantification of 6 phosphodiesterase-5 (PDE-5) inhibitors (sildenafil, dimethylsildenafil, homosildenafil, thiosildenafil, thiodimethylsildenafil and thiohomosildenafil) in dietary supplements...

Full description

Bibliographic Details
Main Authors:	Siti Umairah, Mokhtar, Chin, S. -T., Kee, C. L., Low, M. Y., Drummer, O. H., Marriott, P. J.
Format:	Article
Language:	English
Published:	Elsevier Ltd. 2016
Subjects:	TP Chemical technology
Online Access:	http://umpir.ump.edu.my/id/eprint/11800/ http://umpir.ump.edu.my/id/eprint/11800/ http://umpir.ump.edu.my/id/eprint/11800/ http://umpir.ump.edu.my/id/eprint/11800/1/Rapid%20Determination%20of%20Sildenafil%20and%20Its%20Analogues%20In%20Dietary%20Supplements%20Using%20Gas%20Chromatography%E2%80%93Triple%20Quadrupole%20Mass%20Spectrometry.pdf

id	ump-11800
recordtype	eprints
spelling	ump-118002017-05-29T03:28:43Z http://umpir.ump.edu.my/id/eprint/11800/ Rapid Determination of Sildenafil and Its Analogues in Dietary Supplements Using Gas Chromatography-Triple Quadrupole Mass Spectrometry Siti Umairah, Mokhtar Chin, S. -T. Kee, C. L. Low, M. Y. Drummer, O. H. Marriott, P. J. TP Chemical technology Application of gas chromatography–triple quadrupole mass spectrometry for identification, confirmation and quantification of 6 phosphodiesterase-5 (PDE-5) inhibitors (sildenafil, dimethylsildenafil, homosildenafil, thiosildenafil, thiodimethylsildenafil and thiohomosildenafil) in dietary supplements was investigated. The MS was operated in multiple reaction monitoring mode, for better sensitivity and selectivity. In this manner, the method is adequate to reduce background noise with less interference from co-eluting compounds in the samples. Two different ionisation techniques, electron ionisation (EI) and chemical ionisation (CI), were studied and compared. The chromatographic separation was performed on a short 10 m non-polar capillary column without any derivatisation step. This permitted fast analysis for all analogues with retention time less than 11 min, for both techniques. Use of backflushing can aid method retention time reduction and improves column maintenance. Evaluation of method validation included limit of detection (LOD), lower limit of quantitation (LLOQ), linearity, precision and recovery were performed for both EI and CI techniques. The LOD obtained varied from 0.03 to 1.50 μg/g and the LLOQ ranged from 0.10 to 5.00 μg/g. Good calibration linearity was obtained for all analogues for both techniques, with correlation coefficients (r2) higher than 0.99. Mean recoveries of all analogues using CI show higher values (83.4–108.8%) than that of EI (61.9–91.1%). The intra- and inter-assay precisions were evaluated for all analogues at spiked concentration of 10 μg/g and the relative standard deviation was less than 15% for both methods. These methods were then successfully applied to dietary supplement samples without prior derivatisation, confirming that the samples were adulterated with sildenafil and/or its analogues. Elsevier Ltd. 2016 Article PeerReviewed application/pdf en http://umpir.ump.edu.my/id/eprint/11800/1/Rapid%20Determination%20of%20Sildenafil%20and%20Its%20Analogues%20In%20Dietary%20Supplements%20Using%20Gas%20Chromatography%E2%80%93Triple%20Quadrupole%20Mass%20Spectrometry.pdf Siti Umairah, Mokhtar and Chin, S. -T. and Kee, C. L. and Low, M. Y. and Drummer, O. H. and Marriott, P. J. (2016) Rapid Determination of Sildenafil and Its Analogues in Dietary Supplements Using Gas Chromatography-Triple Quadrupole Mass Spectrometry. Journal of Pharmaceutical and Biomedical Analysis, 121. pp. 188-196. ISSN 0731-7085 http://dx.doi.org/10.1016/j.jpba.2016.01.034 DOI: 10.1016/j.jpba.2016.01.034
repository_type	Digital Repository
institution_category	Local University
institution	Universiti Malaysia Pahang
building	UMP Institutional Repository
collection	Online Access
language	English
topic	TP Chemical technology
spellingShingle	TP Chemical technology Siti Umairah, Mokhtar Chin, S. -T. Kee, C. L. Low, M. Y. Drummer, O. H. Marriott, P. J. Rapid Determination of Sildenafil and Its Analogues in Dietary Supplements Using Gas Chromatography-Triple Quadrupole Mass Spectrometry
description	Application of gas chromatography–triple quadrupole mass spectrometry for identification, confirmation and quantification of 6 phosphodiesterase-5 (PDE-5) inhibitors (sildenafil, dimethylsildenafil, homosildenafil, thiosildenafil, thiodimethylsildenafil and thiohomosildenafil) in dietary supplements was investigated. The MS was operated in multiple reaction monitoring mode, for better sensitivity and selectivity. In this manner, the method is adequate to reduce background noise with less interference from co-eluting compounds in the samples. Two different ionisation techniques, electron ionisation (EI) and chemical ionisation (CI), were studied and compared. The chromatographic separation was performed on a short 10 m non-polar capillary column without any derivatisation step. This permitted fast analysis for all analogues with retention time less than 11 min, for both techniques. Use of backflushing can aid method retention time reduction and improves column maintenance. Evaluation of method validation included limit of detection (LOD), lower limit of quantitation (LLOQ), linearity, precision and recovery were performed for both EI and CI techniques. The LOD obtained varied from 0.03 to 1.50 μg/g and the LLOQ ranged from 0.10 to 5.00 μg/g. Good calibration linearity was obtained for all analogues for both techniques, with correlation coefficients (r2) higher than 0.99. Mean recoveries of all analogues using CI show higher values (83.4–108.8%) than that of EI (61.9–91.1%). The intra- and inter-assay precisions were evaluated for all analogues at spiked concentration of 10 μg/g and the relative standard deviation was less than 15% for both methods. These methods were then successfully applied to dietary supplement samples without prior derivatisation, confirming that the samples were adulterated with sildenafil and/or its analogues.
format	Article
author	Siti Umairah, Mokhtar Chin, S. -T. Kee, C. L. Low, M. Y. Drummer, O. H. Marriott, P. J.
author_facet	Siti Umairah, Mokhtar Chin, S. -T. Kee, C. L. Low, M. Y. Drummer, O. H. Marriott, P. J.
author_sort	Siti Umairah, Mokhtar
title	Rapid Determination of Sildenafil and Its Analogues in Dietary Supplements Using Gas Chromatography-Triple Quadrupole Mass Spectrometry
title_short	Rapid Determination of Sildenafil and Its Analogues in Dietary Supplements Using Gas Chromatography-Triple Quadrupole Mass Spectrometry
title_full	Rapid Determination of Sildenafil and Its Analogues in Dietary Supplements Using Gas Chromatography-Triple Quadrupole Mass Spectrometry
title_fullStr	Rapid Determination of Sildenafil and Its Analogues in Dietary Supplements Using Gas Chromatography-Triple Quadrupole Mass Spectrometry
title_full_unstemmed	Rapid Determination of Sildenafil and Its Analogues in Dietary Supplements Using Gas Chromatography-Triple Quadrupole Mass Spectrometry
title_sort	rapid determination of sildenafil and its analogues in dietary supplements using gas chromatography-triple quadrupole mass spectrometry
publisher	Elsevier Ltd.
publishDate	2016
url	http://umpir.ump.edu.my/id/eprint/11800/ http://umpir.ump.edu.my/id/eprint/11800/ http://umpir.ump.edu.my/id/eprint/11800/ http://umpir.ump.edu.my/id/eprint/11800/1/Rapid%20Determination%20of%20Sildenafil%20and%20Its%20Analogues%20In%20Dietary%20Supplements%20Using%20Gas%20Chromatography%E2%80%93Triple%20Quadrupole%20Mass%20Spectrometry.pdf
first_indexed	2023-09-18T22:12:46Z
last_indexed	2023-09-18T22:12:46Z
_version_	1777415138203140096

Rapid Determination of Sildenafil and Its Analogues in Dietary Supplements Using Gas Chromatography-Triple Quadrupole Mass Spectrometry

Similar Items