SPDS Set 1 ERP Book

PDE5-003

Question

Answer

General

AOAC Method Number:

PDE5-003

Method Title:

Adaption of the LC-MS Screen for Phosphodiesterase-5

Inhibitors to UHPLC-MS

Method Author(s):

Toomey, Subel, Flurer

Reviewer Name:

John Szpylka

Summary of Method

PDE-5 inhibitors are extracted from samples using

via votexing/sonication. The extract is

filtered, diluted, and analyzed by LC-MS (Ion Trap) using a

C18 column &

(formic) mobile phase.

Method Scope / Applicability:

The method lists the matrix scope as "samples of known

analyte concentration", "unknown sample as a dietary

supplement", "liquid sample", and "bulk powder".

Specific references to tablets, capsules (including shells),

softgels, gelcaps, or extracts as listed in SMPR Annex IV is

not present.

General Comments About the

Method:

Comparison to SMPR 2014.010 (ID for routine testing and

dispute resolution): SMPR states all target compounds in

Annex I shall be evaluated. This criterion is not

documented in the submission package. Additional data

is needed to demonstrate the method’s ability to include

the remaining analytes. I do believe this method should

be capable of characterizing all the compounds and

additional work in an SLV will likely document this.

Comparison to SMPR 2014.011 (Quantitative for routine

testing and dispute resolution): SMPR states all target

compounds in Annex I shall be evaluated; and “ideally in

all matrices in Annex II”. This criterion is not

documented in the PDE5-003 submission package.

Additional data is needed to demonstrate the method’s

ability to include the remaining analytes. I do believe this

method should be capable of characterizing all the

compounds and additional work in an SLV will likely

document this. Specific references to tablets, capsules