SPDS Set 1 ERP Book

PDE5-003

(including shells), softgels, gelcaps, or extracts as listed in SMPR Annex II is not present. SMPR states a desired analytical range of 50 – 500,000ppm. PDE5-003 does not specifically note the analytical range nor an LOD/LOQ. Using the listed sample prep conditions, the upper limit of the analytical range is within the scope of this method by following the dilution instructions. Using the same information, I was able to estimate the LOD/LOQ which is above the 50ppm lower level; however data may be available by the authors to demonstrate the method determined lower level of detection. Comparison to SMPR 2014.012 (Routine surveillance): SMPR states all listed matrices will be evaluated; validated for at least 1 raw ingredient and for at least 1 finished product. The method implies these evaluations and validations were performed; however, documentation for these studies is not included. The method is well written. Steps to set-up the instrumentation, prepare samples for testing, and to analyze the data is understood. PDE5-003 is a well-developed method utilizing a simple clean-up protocol, requiring a relatively short analysis time, and confirming analytes using MS. The analyte and matrix range is listed as appropriate (see comments below). Supporting data on the performance of the method for all the required analytes in the listed matrices ststed in the 3 SMPRs is not present. A detailed SLV was also not supplied with the submission. The method does appear to be able to meet the requirements but proper documentation for transparency is needed. Supporting Data A single laboratory validation study was not included in the submission. The method does include flexibility in sample preparation to assure proper detection. Performance Characteristics An analytical range of 1-5 mcg/mL is listed for samples "one-tenth to one-fifth of a dosage unit" and for 10-20 mg of bulk material followed by dilution ("typically 1:10

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Method Optimization

Analytical Range: