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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