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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, confir-mation and quantification of 6 phosphodiesterase-5 (PDE-5) inhibitors (sildenafil, dimethylsildenafil,homosildenafil, thiosildenafil, thiodimethylsildenafil and thiohomosildenafil) in dietary supplements...

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Main Authors:	Mokhtar, Siti Umairah, Chin, S. -T., Kee, C. L., Low, M. Y.
Format:	Article
Language:	English
Published:	Elsevier Ltd. 2016
Subjects:	QD Chemistry
Online Access:	http://umpir.ump.edu.my/id/eprint/31578/2/JPBA.pdf http://umpir.ump.edu.my/id/eprint/31578/ https://www.sciencedirect.com/science/article/abs/pii/S0731708516300346 https://doi.org/10.1016/j.jpba.2016.01.034
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spelling	my.ump.umpir.315782021-08-17T16:18:50Z http://umpir.ump.edu.my/id/eprint/31578/ Rapid determination of sildenafil and its analogues in dietary supplements using gas chromatography–triple quadrupole mass spectrometry Mokhtar, Siti Umairah Chin, S. -T. Kee, C. L. Low, M. Y. QD Chemistry Application of gas chromatography–triple quadrupole mass spectrometry for identification, confir-mation and quantification of 6 phosphodiesterase-5 (PDE-5) inhibitors (sildenafil, dimethylsildenafil,homosildenafil, thiosildenafil, thiodimethylsildenafil and thiohomosildenafil) in dietary supplementswas investigated. The MS was operated in multiple reaction monitoring mode, for better sensitivity andselectivity. In this manner, the method is adequate to reduce background noise with less interference fromco-eluting compounds in the samples. Two different ionisation techniques, electron ionisation (EI) andchemical ionisation (CI), were studied and compared. The chromatographic separation was performedon a short 10 m non-polar capillary column without any derivatisation step. This permitted fast analysisfor all analogues with retention time less than 11 min, for both techniques. Use of backflushing can aidmethod retention time reduction and improves column maintenance. Evaluation of method validationincluded limit of detection (LOD), lower limit of quantitation (LLOQ), linearity, precision and recoverywere performed for both EI and CI techniques. The LOD obtained varied from 0.03 to 1.50 _g/g and theLLOQ ranged from 0.10 to 5.00 _g/g. Good calibration linearity was obtained for all analogues for bothtechniques, with correlation coefficients (r2) higher than 0.99. Mean recoveries of all analogues usingCI show higher values (83.4–108.8%) than that of EI (61.9–91.1%). The intra- and inter-assay precisionswere evaluated for all analogues at spiked concentration of 10 _g/g and the relative standard deviationwas less than 15% for both methods. These methods were then successfully applied to dietary supple-ment samples without prior derivatisation, confirming that the samples were adulterated with sildenafiland/or its analogues. Elsevier Ltd. 2016-01-15 Article PeerReviewed pdf en http://umpir.ump.edu.my/id/eprint/31578/2/JPBA.pdf Mokhtar, Siti Umairah and Chin, S. -T. and Kee, C. L. and Low, M. Y. (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 https://www.sciencedirect.com/science/article/abs/pii/S0731708516300346 https://doi.org/10.1016/j.jpba.2016.01.034
institution	Universiti Malaysia Pahang
building	UMP Library
collection	Institutional Repository
continent	Asia
country	Malaysia
content_provider	Universiti Malaysia Pahang
content_source	UMP Institutional Repository
url_provider	http://umpir.ump.edu.my/
language	English
topic	QD Chemistry
spellingShingle	QD Chemistry Mokhtar, Siti Umairah Chin, S. -T. Kee, C. L. Low, M. Y. 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, confir-mation and quantification of 6 phosphodiesterase-5 (PDE-5) inhibitors (sildenafil, dimethylsildenafil,homosildenafil, thiosildenafil, thiodimethylsildenafil and thiohomosildenafil) in dietary supplementswas investigated. The MS was operated in multiple reaction monitoring mode, for better sensitivity andselectivity. In this manner, the method is adequate to reduce background noise with less interference fromco-eluting compounds in the samples. Two different ionisation techniques, electron ionisation (EI) andchemical ionisation (CI), were studied and compared. The chromatographic separation was performedon a short 10 m non-polar capillary column without any derivatisation step. This permitted fast analysisfor all analogues with retention time less than 11 min, for both techniques. Use of backflushing can aidmethod retention time reduction and improves column maintenance. Evaluation of method validationincluded limit of detection (LOD), lower limit of quantitation (LLOQ), linearity, precision and recoverywere performed for both EI and CI techniques. The LOD obtained varied from 0.03 to 1.50 _g/g and theLLOQ ranged from 0.10 to 5.00 _g/g. Good calibration linearity was obtained for all analogues for bothtechniques, with correlation coefficients (r2) higher than 0.99. Mean recoveries of all analogues usingCI show higher values (83.4–108.8%) than that of EI (61.9–91.1%). The intra- and inter-assay precisionswere evaluated for all analogues at spiked concentration of 10 _g/g and the relative standard deviationwas less than 15% for both methods. These methods were then successfully applied to dietary supple-ment samples without prior derivatisation, confirming that the samples were adulterated with sildenafiland/or its analogues.
format	Article
author	Mokhtar, Siti Umairah Chin, S. -T. Kee, C. L. Low, M. Y.
author_facet	Mokhtar, Siti Umairah Chin, S. -T. Kee, C. L. Low, M. Y.
author_sort	Mokhtar, Siti Umairah
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/31578/2/JPBA.pdf http://umpir.ump.edu.my/id/eprint/31578/ https://www.sciencedirect.com/science/article/abs/pii/S0731708516300346 https://doi.org/10.1016/j.jpba.2016.01.034
_version_	1709667682948743168
score	13.211869

Rapid determination of sildenafil and its analogues in dietary supplements using gas chromatography–triple quadrupole mass spectrometry

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