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Silliker
Chem, Res. Center Crete, IL – Validation of a LC-MS/MS Method for Vitamin K Analysis
Silliker Laboratories, Chemistry Research Center, Date: 1/30/15
14
Table 4: The analysis of vitamin K1 in NIST SRM 1849a (Infant/Adult Nutrition Folmula)
NIST SRM 1849a
Certified Value
mcg/g for total
vitamin K1 (cis
+trans)
Analytes
Vitamin K1 mcg/g
Day 1
Day 2
Day 3
Day 4
Day 5
Trans -vitamin K1
0.99
0.91
1.01
0.82
0.81
cis -vitamin K1
0.13
0.14
0.15
0.11
0.13
vitamin K1 (Total,
trans +cis)
1.12
1.05
1.15
0.93
0.97
1.06 +/- 0.17
Vitamin K1 (mcg/g)
-->
Vit K1 Total
(cis + trans)
mcg/g
Vit K1 (-trans)
mcg/g
Vit K1 (-cis)
mcg/g
Average
1.00
0.90
0.10
S.D.
0.10
0.10
0.00
% RSD
8.9
10.2
10.6
n
5
5
5
Number of Independent
analytical days
5
5
5
The Certified Value of Vitamin K1 (Total, cis + trans, mcg/g) in the NIST SRM 1849a (Infant Adult
Nutrition Formula) 1.06 + 0.17 matched closely to the value obtained by the method. This helps in
establishing accuracy of the method. The method precision based on the analyzed replicates of the
SRM sample on multiple days (5) was found to be satisfactory (% RSD of 8.9).
Analysis of the SPIFAN Matrices:
The Analysis of the SPIFAN samples:
Details of the Reconstitution process of the samples before the analysis:
All the powder samples received from SPIFAN were analyzed in replicates by the method for the
targeted vitamin K compounds. Every sample was analyzed in triplicates for three days with a total of 9
replicates. All of the powdered samples were reconstituted as a beverage by taking approximately 12.5
g of the powder into 100 mL of water. Details of the samples and reconstitution are provided in the
following Table 5.
VitK-01 w/SLV
FOR ERP USE ONLY
DO NOT DISTRIBUTE