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FOR EXPERT REVIEW PANEL USE ONLY
NOT FOR DISTRIBUTION
3
This effort was significantly hindered by shipping difficulties.
Supporting Data
General Comment:
Data provided are consistent with SMPR requirements. More data is needed to complete a full SPIFAN
SLV. This effort hindered by sample shipping issues.
Method Optimization:
Performance Characteristics:
Analytical Range:
7 working standard concentrations are indicated for both vitamin D2 and D3. Concentrations ranging
from 5-100 ng/mL
LOQ:
LOQ was evaluated using blank samples, n=10, with measured standard deviation.
VitD3 LOQ, x+10SD, is reported as 0.961 ng/100g in reconstituted/RTF product.
Vit D2 LOQ, x+10SD, is reported as 0.813 ng/100g in reconstituted/RTF product
As reported these pass SMPR requirement
Accuracy/Recovery:
Recovery of vitamin D2 was assessed by overspike experimentation using SRM 1849a at three spike
levels. Analysis was completed in duplicate on each of 6 days. It is unclear if the within day replicates
were separate preparations or duplicate injections from same sample
Recovery reported was 101%-103% with very good precision.
Three additional product samples, 3 powders and 1 liquid, were spiked at two levels with both vitamin
D3 and D2. Each sample was analyzed in triplicate.
Recoveries ranged from 89-97% (Vit D2) and 97%-102% (Vit D3)
Precision values, n=3, ranged from <1% - 8.2% for vit D2 and vit D3
vitamin D3 results are 97% relative to the NIST SRM 1849a certified value
As reported these pass SMPR requirements
Precision (RSD
r
):
Precision was evaluated using SRM 1849a (vitamin D3) and overspike results in product matrices.
Data are limited.
Vitamin D2:
3.5% at 0.12mcg/100g RTF (SMPR ≤15%)
5.2% at 1.5 mcg/100g RTF (SMPR ≤11%)
4.1% at 2.5 mcg/100g RTF(SMPR ≤11%)
Vitamin D3:
3% at 1.5 mcg/100g RTF (SMPR ≤11%)
VitD-17 Review Forms