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

Mean

7.3 0.3 3.7

0.9 0.1 9.5

8.3 0.6 7.2

Stdev

SPIFAN Sample #9

% RSD

3

2

9

n

Mean

2.1 0.3

0.3 0.0

2.4 0.3

Stdev

SPIFAN Sample #10

12.7

13.0

10.8

% RSD

3

2

3

n

Mean

2.1 0.2

0.4 0.0 8.1 0.9 0.1 8.7 1.1 0.1 7.7 1.2 0.1 9.7 1.4 0.1 8.4 2.5 0.2 6.0 3.0 0.1 4.7 2 3 3 3 3 3

2.5 0.2 7.2 8.1 0.0 0.6 2

Stdev

SPIFAN Sample #11

10.5

% RSD

2

n

Mean

7.3 0.1 0.8

Stdev

SPIFAN Sample #12

% RSD

3

3

n

Mean Stdev

5.1 0.6

6.2 0.7

SPIFAN Sample #13

12.5

11.6

% RSD

3

3

n

Mean

5.2 0.2 4.8

6.4 0.3 4.9

Stdev

SPIFAN Sample #14

% RSD

3

3

n

Mean Stdev

8.2 1.1

9.6 1.2

SPIFAN Sample #15

13.7

12.7

% RSD

3

3

n

Mean

5.9 0.5 8.4 7.7 0.4 5.2 3

8.4 0.5 5.8

Stdev

SPIFAN Sample #16

% RSD

3

n

Mean

10.7

0.5 5.0

Stdev

SPIFAN Sample #17

% RSD

n 2 All powder samples reconstituted before the analysis (About 25 in 200 mL water). RF samples analyzed as such. Concentration of Vitamin K1 (Total, trans + cis) was found to be in the range of 2.1 – 10.3 µg/100g in the analyzed samples when analyzed third time in replicates. The precision of the vitamin K1 analysis in terms of the % RSD was estimated to be equal or under 8% in most of the analyzed samples with concentration of total (trans + cis) vitamin K1 within the range of 1 -10 mcg/100g as stipulated in the Vitamin K SMPR 2014.001. Some samples however gave % RSD values some what higher values (10.8%, 11.6% and 12.7%) in their replicate analysis. The sample with concentration of Vit K1 higher than 10 µg/100g, provided % RSD values closer to 5%. Cis –vitamin K1 was always found at relatively lower levels (0.4-3.0 µg/100g) in the samples with a % 2 2

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

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