107 / 116
PDE5-005
Question
Response
General
AOAC Method Number:
PDE5-005
Method Title:
SLV Study of a method for Screening
Method Author(s):
Vaclavik, Schmitz, Halbardier, Mastovska
Reviewer Name:
Tom Phillips
Summary of Method
PDE5 inhibitors are extracted from the dietary ingr
edient or supplement samples using a 50:50 (v/v
) mixture of acetonitrile and water and centrifuged
. Supernatant is diluted, filtered and analyzed by LC-
HRMS. Data are collected in MS acquisition mode that
combines full-scan MS experiment with ion
fragmentation and data-dependent MS/MS product ion
scan experiment. This approach enables collection of MS
and MS/MS data for both targeted and non-targeted
PDE5 inhibitors in a single chromatographic run.
Software-facilitated identification of targeted analytes is
performed based on retention time, accurate mass and
isotopic pattern of pseudomolecular ion, and accura
te masses of fragment ions using in-house developed
compound database. Detection and identification of
other PDE5 inhibitors and novel analogues are performed
by retrospective evaluation of MS and MS/MS
experimental data.
Method Scope / Applicability:
Applicable to screening and identification of acet
aminotadalafil, acetildenafil, avanafil, homo sildenafil,
hydroxyacetildenafil, hydroxyhomos ildenafil,
hydroxythiohomosildenafil, lodenafil carbonate,
mirodenafil, propoxyphenyl homohydroxysildenafil,
sildenafil, tadalafil, thiohomosildenafil, udenafil,
vardenafil and other known and novel analogues of the
above PDE5 inhibitors.
General Comments About the
Method:
The method is miniaturized which allows high throughput
for samples. Sample preparation is easy and simple. The
linearity for the three compounds studied is excellent,