SPDS Set 1 ERP Book

PDE5-003

Question

Answer

General

AOAC Method Number:

PDE5-003

Adaption of the LC-MS Screen for Phosphodiesterase-5 Inhibitors to UHPLC-MS

Method Title:

Method Author(s):

Toomey, Subel, Flurer

Reviewer Name:

John Szpylka

PDE-5 inhibitors are extracted from samples using ACN:Water via votexing/sonication. The extract is filtered, diluted, and analyzed by LC-MS (Ion Trap) using a C18 column & ACN:water (formic) mobile phase. 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. 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

Summary of Method

Method Scope / Applicability:

General Comments About the Method: