OMB Meeting Book_9-11-14

AOAC INTERNATIONAL Stakeholder Panel for Infant Formula and Adult Nutritionals (SPIFAN)

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. 

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.