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

4 5

100.9

101.1

101.7 101.7 100.0

96.2 98.6

92

Mean

94.6

n

15

15

15

SD

3.1 3.1

3.7 4.0

3.8 3.8

% RSD

Vitamin K1 recovery was tried at different spike levels. Average vitamin K1 spike recovery obtained at spike level I (1.5-2.0 mcg/100g) in five different SPIFAN samples 98.6% (n=15). Average vitamin K1 spike recovery obtained at spike level II (2.5-3.0 mcg/100g) in five different SPIFAN samples 94.6% (n=15). Average vitamin K1 spike recovery obtained at spike level III (6.0-6.5 mcg/100g) in five different SPIFAN samples 100% (n=15). Vitamin K2-7 spike recovery evaluation in SPIFAN samples was performed by spiking the first five SPIFAN samples (powder samples reconstituted as liquid, RF samples used as is) with K2-7 at different spike levels in replicates. The spiked and non-spiked samples were analyzed in replicates (usually n=3) on two separate days for vitamin K2-7 and the spike recovery calculated. The results are presented in Tables 8a-a-c. The results of the first day of the trial for vitamin K1 spike recovery evaluation are presented in Table 7a.

Table 8a Vitamin K2-7 Spike recovery in SPIFAN matrices on multiple days, Day1 data

VITAMIN K2-7

Day 1

Sample Parameters

Sample mcg/100g

spike amt mcg/100g

Obtained (mcg/100g)

Expected (mcg/100g)

% Recovery

n

Mean

3.5 0.3 9.6 5.0 0.2 4.3 1.7 0.0 1.1 3.1 0.2 5.9 1.9 0.0 2.4 2.8 0.1

3.5 0.0 0.2 4.9 0.0 0.4 1.7 0.0 0.3 3.2 0.0 0.9 1.9 0.0 0.3 3.0 0.0

100.3

3

SD

2.0

1.5

9.8 9.8

% RSD

1

Mean

101.9

SD

4.6 4.5

2.0

3.0

% RSD

Mean

100.7

3

SD

0.0

1.7

1.4 1.3

% RSD

2

Mean

97.5

SD

5.1 5.2

0.0

3.2

% RSD

Mean

98.4

3

SD

0.3

1.7

2.5 2.6

3

% RSD

Mean

92.6

0.3

3.0

SD

4.1

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

26