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

value of all the 12 SPIFAN samples tested in replicates on multiple days is 7.9% (n=300).

% Spike Recovery Evaluation (for accuracy) of the method:

The spike recovery evaluation was performed by spiking the first five SPIFAN samples (powder samples reconstituted as liquid, RF samples used as is) with Vitamin K1, K2-4 and K2-7 at different spike levels. The samples were spiked in replicates. Spiked and non-spiked samples were analyzed in replicates (usually n=3) on two separate days for vitamin K analytes and the spike recovery was calculated. The results are presented in Tables 7a-c for Vitamin K1, 8a-c Vitamin K2-7, and 9a-c Vitamin K2-4. The results of the first day of the trial for vitamin K1 spike recovery evaluation are presented in Table 7a.

Table 7a: Vitamin K1 Spike recovery in SPIFAN matrices on multiple days, Day1 data

VITAMIN K1 Day 1

spike amt mcg/100g

Obtained (mcg/100g)

Expected (mcg/100g)

% Recovery

Sample Parameters mcg/100g

n

Mean

3.3

3.5

95.5

1.5

SD

- -

- -

- -

2.0

2

% RSD

1

Mean

4.5 0.2 4.6 3.5 0.1 2.8 4.4 0.2 4.5 5.5 0.2 2.7 6.2 0.3 5.5 5.2 0.3 5.3 6.2 0.1 1.5 3.3 0.1

4.9 0.0 0.4 3.4 0.0 0.2 4.7 0.0 0.6 5.7 0.0 0.1 6.6 0.0 0.4 5.1 0.0 0.1 6.1 0.0 0.3 3.4 0.0

92.1

SD

4.5 4.9

2.0

3.0

3

% RSD

Mean

102.6

1.7

SD

3.0 3.0

1.7

3

% RSD

2

Mean

94.0

SD

4.2 4.4

1.7

3.0

3

% RSD

Mean

97.8

2.0

SD

2.7 2.8

3.7

3

% RSD

3

Mean

94.0

SD

4.9 5.3

3.7

3.0

3

% RSD

Mean

100.9

SD

5.4 5.4

3.1

2.0

3

% RSD

4

Mean

101.1

SD

1.3 1.3

3.1

3.0

3

% RSD

Mean

96.2

5

1.9

1.5

3

SD

4.4

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

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