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2012•Mass spectrometry lettersOpen access

Determination of the PDE-5 Inhibitors and Their Analogues by GC-MS and TMS Derivatization

Jaesung Pyo, Hee-Sang Lee, Yujin Park, Jiyeong Jo, Yonghoon Park, Sanggil Choe, Mi-Young Lee, Jaesin Lee

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Abstract

Eighteen of the PDE-5 inhibitors and their analogues were analyzed using GC-EI-MS. Fourteen of them could beidentified by simple GC-MS method without derivatization, but hydroxyhongdenafil, hydroxyvardenafil, xanthoanthrafil andmirodenafil could not be identified without derivatization for the high polarity due to the presence of hydroxyl groups. N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA) and N-methyl-N-(tert-butyldimethylsilyl)trifluoroacetamide (MTBSTFA), widely used trimethylsilyl (TMS) derivatizing reagents, were used to improve the sensitivity of the hydroxylated analogues. And the analytes could be identified by GC-MS after the derivatization.

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Eighteen of the PDE-5 inhibitors and their analogues were analyzed using GC-EI-MS. Fourteen of them could beidentified by simple GC-MS method without derivatization, but hydroxyhongdenafil, hydroxyvardenafil, xanthoanthrafil andmirodenafil could not be identified without derivatization for the high polarity due to the presence of hydroxyl groups. N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA) and N-methyl-N-(tert-butyldimethylsilyl)trifluoroacetamide (MTBSTFA), widely used trimethylsilyl (TMS) derivatizing reagents, were used to improve the sensitivity of the hydroxylated analogues. And the analytes could be identified by GC-MS after the derivatization.

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Available abstract

Eighteen of the PDE-5 inhibitors and their analogues were analyzed using GC-EI-MS. Fourteen of them could beidentified by simple GC-MS method without derivatization, but hydroxyhongdenafil, hydroxyvardenafil, xanthoanthrafil andmirodenafil could not be identified without derivatization for the high polarity due to the presence of hydroxyl groups. N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA) and N-methyl-N-(tert-butyldimethylsilyl)trifluoroacetamide (MTBSTFA), widely used trimethylsilyl (TMS) derivatizing reagents, were used to improve the sensitivity of the hydroxylated analogues. And the analytes could be identified by GC-MS after the derivatization.

Key concepts: Derivatization, BSTFA, Chemistry, Trimethylsilyl, Chromatography, Gas chromatography–mass spectrometry, Reagent, Silylation

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