SPIFAN Nutrients ERP Book 9-29-15

Laboratory I noted that 15% KOH was used instead of 15% ROH to wash the samples as

they did not see the email about the correction in time.

Laboratory I also used a

Shimadzu UFLC which is not a UHPLC system.

Laboratory K noted that they were unable to analyze all the samples on one day so the

sample load was split between two days.

Laboratory L noted that samples were open on 02 Dec 2014 but due to instrument issues,

the samples were not analyzed until 29 Dec 2014. During this time the samples were

kept at room temperature, protected from light. The RTF samples were refrigerated at 4

degrees C.

Laboratory M noted that several samples had three phases after separation in the

separatory funnel. In all cases, only the top (clear) layer was used. Samples KDOX966,

FHTX798, ATAN351 and FRZK569 had to be reanalyzed as the initial analysis showed

poor recovery of the internal standard and samples had noticeable droplets in the solution

after the final reconstitution in 70% ACN. When the samples were reanalyzed, a second

wash step with 15% ROH solution was used to eliminate emulsions. While samples

ATAN351 and FRZK569 still had droplets in the final reconstitution in 70% ACN, all

samples demonstrated acceptable recovery of the internal standard and the qualifying

ions were in acceptable range.

Recommendations

It is the recommendation of the Study Director that the method is fit-for-purpose in

determining vitamin D

and vitamin D

in infant formula and adult/pediatric nutritional

formula and that it be adopted as an AOAC Final Action

Official Method

status.

Acknowledgement

The Study Directors are very grateful to all laboratories that participated in the studies,

especially to the following collaborators (listed alphabetically based on their institution

name):

Charles Black (Abbott Nutrition R&D, Columbus, OH)

Jing Tan (Abbott Nutrition R&D, #09-01/02 Centros Building, Singapore)

Eric Marceau (Canadian Food Inspection Agency, Quebec, Canada)

Regina Lim (Covance (Asia) Pte Ltd, #01-01 The Synergy, Singapore)

Yang Zhou (Eurofins Nutrition Analysis Center, Des Moines, IA)

Pierluigi Delmonte (FDA HFS, College Park, MD)

Sudhakar Yadlapalli (FirstSource Laboratory Solutions LLP, Hyderabad, India)

Hongwei Zhang (Food and Agricultural Testing Agency, Qingdao,

Hans Cruijsen (FrieslandCampina Laboratory & Quality Services, The Netherlands)

Jennifer Frueh (Mead Johnson Nutritionals, Evansville, IN)

2011.11 VITAMIN D MLT-Sept 2015

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