OMB Meeting Book_9-11-14
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? In your experience with the method, is there any safety concerns identified while using or regarding use of the method? Do you have any information that supports regarding the reproducibility of the method as written: If so, please specify and submit information? 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?
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.
none
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.
Need to add Sufficient quantity of ethanol for uniform sample preparation. Washing media to be checked.
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