UPLC-MS/MS for the Simultaneous Determination of Sildenafil and N-Desmethyl Sildenafil.
J Chromatogr Sci
; 59(9): 823-829, 2021 Sep 29.
Article
in En
| MEDLINE
| ID: mdl-33517421
ABSTRACT
A sensitive high-performance liquid chromatography-tandem mass spectrometry method was established for the simultaneous determination of sildenafil and N-desmethyl sildenafil in human plasma. The protein precipitation was used for extraction and the gradient elution of the mobile phase A of water (containing 0.01% formic acid) and the mobile phase B of acetonitrile, and methanol (VV = 11, containing 0.01% formic acid) was used for chromatographic separation on a C18 column. Quantification was performed by multiple reaction monitoring mode to monitor the precursor-to-product ion transitions of m/z 475.4 â m/z 283.3 for sildenafil, m/z 461.4 â m/z 283.2 for N-desmethyl sildenafil, m/z 483.3 â m/z 108.1 for sildenafil-d8 (IS) and m/z 469.2 â m/z 283.3 for N-desmethyl sildenafil-d8 (IS) at the positive ionization mode. The intra- and inter-day relative standard deviations were less than 6.8% and 4.1% for sildenafil and N-desmethyl sildenafil, respectively. Accuracy at four levels ranged from 93.1% to 115.9% for sildenafil and 95.6% to 112.5% for N-desmethyl sildenafil. The present method was sensitive and reliable for simultaneous quantification of sildenafil and its active metabolite and was successfully applied to a pharmacokinetic study of an oral low dose of sildenafil in Chinese healthy volunteers.
Full text:
1
Collection:
01-internacional
Database:
MEDLINE
Main subject:
Plasma
/
Tandem Mass Spectrometry
Limits:
Humans
Language:
En
Journal:
J Chromatogr Sci
Year:
2021
Document type:
Article
Affiliation country: