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

% RSD

5.3 1.5 0.0 2.3 3.0 0.3 1.8 0.1 3.6 2.7 0.1 3.6

0.8 1.5 0.0 0.1 3.0 0.0 0.6 1.8 0.0 0.1 2.8 0.0 0.6

4.5

Mean

101.3

3

SD

0.0

1.5

2.4 2.4

% RSD

4

Mean

98.8 10.6 10.7

SD

-

3.0

% RSD

10.3

Mean

103.0

3

SD

0.3

1.5

3.7 3.6

% RSD

5

Mean

96.1

SD

3.4 3.5

0.3

2.5

% RSD

The spike recovery for vitamin K2-7 obtained on the first day of the trial at all of the investigated spike levels was found to be in the range of 92.6-103% and within the range stipulated by the SMPR. The precision of the spike recovery evaluation in replicates at all spike levels as % RSD was calculated. The values obtained were quite satisfactory and in the range of 1.3-10.7%.

Vitamin K2-7 spike recovery evaluation in the SPIFAN samples was repeated on a second day at a higher spike levels and the results are presented in Table 8b.

Table 8b Vitamin K2-7 Spike recovery in SPIFAN matrices on multiple days, Day2 data

Day 2

Sample Parameters

Sample mcg/100g

spike amt mcg/100g

Obtained (mcg/100g)

Expected (mcg/100g)

% Recovery

n

Mean

1.8

6.5

8.2 0.2 3.0

8.2 0.1 0.7

100.2

3

SD

3.4 3.4

% RSD Mean SD % RSD

1

Mean

0.0

7.0

7.0 0.0 0.7

6.9 0.0 0.5

100.5

3

SD

1.1 1.1

% RSD Mean SD % RSD

2

Mean

0.2

7.0

7.0 0.1 2.1

7.1 0.0 0.1

98.0

3

SD

2.1 2.1

3

% RSD

Mean SD

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

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