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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.
Method Clarity
The method is well written. Steps to set-up the
instrumentation, prepare samples for testing, and to
analyze the data is understood.
Pros/Strengths
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).
Cons/Weaknesses
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
General Comments
A single laboratory validation study was not included in
the submission.
Method Optimization
The method does include flexibility in sample preparation
to assure proper detection.
Performance Characteristics
Analytical Range:
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