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case with SRM 1974 available, it could have been handled differently. The selection of the 19 target PAHs to determine
could be questioned. The authors comment on criteria for separation of chrysene and triphenylene and also BaP and BeP,
which is good, but perhaps triphenylene and BeP should have been included. There were no performance criteria for the
separation of the alkyl-PAHs from potential isomers, e.g., with 3-MeChr targeted, how do you know if you are separating it
from other methylchrysene or methyl-BaA isomers? The inclusion of several alkyl-PAHs is good, but will this really provide a
method to look at the alkyl-PAHs, which in petroleum contaminated samples may be more abundant than the parent PAHs.
Should there be a provision for looking at the alkyl-PAHs as a group by MS? Perhaps this is beyond the intended scope of
this method.
ER 7
Fish, one of the most common seafood, was not covered in this method. Oyster needs to be stored at -70 C, which is not
very easy for many labs to maintain.
ER 8
no comment
Supporting Data Comments
ER 1
Great summary of results and provided complete statistical information. Would like to see more on linearity results.
ER 2
The supporting data indicates that the method is rugged and accurate.
ER 3
Nicely organized.
ER 4
na
ER 5
More specificity needed in quantitative parameters.
ER 6
In general, this is a good method, but needs further validation.
ER 7
Tested real samples. Additional experiments with shrimp matrix performed.
ER 8
good
Method Optimization
ER 1
N/A
ER 2
Was well described and performed appropriately.
ER 3
Good.
ER 4
na
ER 5
The Safety Section must be in the front of the method since safety is more important than any other part of the protocol.
Method must be more specific when outlining quantitative parameters. Under Degradation Issues on page 18, the
discussion emphasizes the need for a Stability Study. 18.2 megaohm water should be used for any GC/MS method (page 9,
Section C). Need a statement that documented calibrations/reference checks were performed on all analytical equipment
and instrumentation used in the collaborative study.
ER 6
The method optimization is well done in particular the SPE cleanup. Could the use of an aminopropyl SPE be less sensitive
than silica regarding deactivation by moisture content?
ER 7
Elution solvent volume for silica gel SPE cleanup is optimized. Increased water amount (10 mL) is used in shrimp samples to
help shake and extract PAHs from more viscous shrimp samples.
ER 8
good
Candidates for 2016 Method of the Year
269