SPDS Set 1 ERP Book

PDE5-003

analogs, nor does it include avanafil, lodenafil carbonate, mirodenafil, udenafil as specified in SMPR 2014.012 for PDE5 screening method. Agilent 1200 is a 400 bar/6000 psi HPLC system, typically using 0.007" ID tubing & capillary needle seat in flow path from injector to column, and column to detector. Authors refer to this as UHPLC system; is it possible their UHPLC system is an Agilent 1260 or 1200SL (600 bar/9000 psi) system? Were any modifications made to minimize extra column volume? Supporting Data the power of MS/MS technique highlighted by ability to distinguish Gendenafil (same M+H as Yohimbine) based on examination of M+H product ions for both compounds. Authors provide sources for standards - again from 2012, so this needs to be updated to current to reflect additional known PDE5 inhibitors. I also believe that MS/MS is going to be needed for a proper screening method since analogs are closely related and may not be fully resolved in HPLC/UHPLC to allow for UV detection. not clear how this method was optimized or if further optimization might be required with inclusion of additional PDE5 analogs. Method specifies Zorbax 1.8um SB-C18 50x2.1mm column and indicates other C18 columns would need to be evaluated for use in this procedure. Performance criteria (e.g. efficiency, resolution, retention) for column not indicated. Performance Characteristics working standards range of 1–5 μg/mL (1-5 ppm) ; 0.5-5 ug/mL (0.5-5 ppm) in LC/MS method.

General Comments

Method Optimization

Analytical Range:

LOQ:

Not specified

Accuracy/Recovery

Not specified

Precision (RSDr)

Not specified

Reproducibility (RSDR)

Not specified

System Suitability

Not specified

Safety Review