AOAC SPIFAN ERP Meeting Book-March 16, 2016

VitK-01 w/SLV FOR ERP USE ONLY DO NOT DISTRIBUTE

Silliker Chem, Res. Center Crete, IL – Validation of a LC-MS/MS Method for Vitamin K Analysis

Table 4: The analysis of vitamin K1 in NIST SRM 1849a (Infant/Adult Nutrition Folmula)

Analytes

Vitamin K1 mcg/g

NIST SRM 1849a Certified Value mcg/g for total vitamin K1 (cis +trans)

Day 1

Day 2

Day 3

Day 4

Day 5

Trans -vitamin K1 cis -vitamin K1 vitamin K1 (Total, trans +cis)

0.99 0.13

0.91 0.14

1.01 0.15

0.82 0.11

0.81 0.13

1.12

1.05

1.15

0.93

0.97

Vit K1 Total (cis + trans) mcg/g

Vitamin K1 (mcg/g) -->

Vit K1 (-trans) mcg/g

Vit K1 (-cis) mcg/g

Average

1.00

0.90

0.10

S.D.

1.06 +/- 0.17

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.

Silliker Laboratories, Chemistry Research Center, Date: 1/30/15

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