COMMENT PARAMETERS
USER COMMENTS
AOAC OMA
2011.11
Method Name/Manuscript Title
Vitamin D in Infant Formula and Adult Nutritionals by UHPLC and
Tandem Mass Spectrometry.
Manuscript Reference
In your experience using the method, does the
method perform according to the method’s
applicability as written?
10g is insufficient for the low level Vitamin D2 & D3 in infant formula.
30g prepared sample is recommended but the low levels are difficult
to achieve. For 30g, the quantity of ethanol 40ml specified may not
be sufficient.
In your experience with the method, is there
any safety concerns identified while using or
regarding use of the method?
none
Do you have any information that supports
regarding the reproducibility of the method as
written: If so, please specify and submit
information?
Need to give proper washing with water to the hexane layer after the
extraction with alkaline extract to make it completely free from alkali.
but the method prescribes the washing with 85% water + 15% KOH.
Overnight saponification at 25°C is little time consuming. Observed
the degradation of compounds/poor recovery when increase in
temperature but below 100°C for shorter time reflux should be fine.
Please attach any documentation to support
your feedback, if available.
Based on your experience with the method,
are there any recommended changes to the
AOAC First Action Method as written?
Need to add Sufficient quantity of ethanol for uniform sample
preparation.
Washing media to be checked.
