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FOR EXPERT REVIEW PANEL USE ONLY
NOT FOR DISTRIBUTION
2
d)
Calculation and reporting units are given in mg/kg, while SMPR requirements are all in mcg/100 g,
could this be reviewed?
e)
Sample preparation: it does not require reconstitution and yet validation data are provided using
reconstitution, which would eventually provide better performance than expected if the method is
followed as written. Please review.
f)
MS detection is performed in MRM mode, three transitions are given for each compound, but no
details are given on which one to use for quantification and the use of the other two ions. The
reviewer would like to see this clarified, if possible with acceptance rate for ion ratios.
Method Safety Concerns:
No specific concerns on safety
Pros/Strengths:
•
Method easy to apply, which requires minimal sample preparation and lab equipment.
Cons/Weaknesses
•
As stated above, sample preparation does not require reconstitution and yet validation data are
provided using reconstitution, which would eventually provide better performance than expected if the
method is followed as written.
Supporting Data
•
General Comments:
The reviewer has a concern that validation data shown might not reflect the real performance of the
method when applied as written to all kind of samples (no sample reconstitution, while validation has been
perfomed using reconstitution), this could be solved by clearly proposing two types of sample preparation:
1. For samples known to be homogeneous 2. For samples not homogeneous
All precision data have been obtained analyzing the samples in triplicates in 2 days (n=6), while
recommended guidelines for SLV are duplicate 6 days (n=12). Although this seems to the reviewer
sufficient to establish repeatability, intermediate reproducibility data should be interpreted with caution.
Hydrolysed products showed higher variability one of the two days of analysis, there are not enough data
to evaluate if this could be a problem since only two days are available. This might not be a problem but
should be carefully reviewed if the method moves to MLT.
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Method Optimization: