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 of the replicates in the range of 1.7-13.0 %. The lower relative level of the analyte in samples may be associated with the observed higher variance in the analysis of the replicates. Trans –vitamin K1 was found to be in the range of 2.1 – 10.3 µg/100g in the analyzed samples. % RSD of the trans-vitamin K1 analysis was estimated to be under 8% in replicates of many of the analyzed samples. But % RSD in the trans-vitamin K1analysis of the replicates of some of the samples gave higher % RSD values in their replicate analysis. . The sample with concentration of Vit K1 higher than 10 µg/100g provided % RSD value of 5% as stipulated in the SMPR.

A summary of the Results for the averages of repeatability/interday-precision (%RSD r

) for each of the

sample are presented Table 6.

Table 6: Analysis of different SPIFAN samples in replicates on multiple days – Results of all replicates including those analyzed on different days in replicates

Average of Analysis of replicates on All Three Days

Total (trans + cis)

Paramtrs

Trans

Cis

Sample ID

mcg/100g of RF sample as is or a powder sample reconstituted in to a liquid

Mean

10.1

1.4 0.1

11.5

0.6 6.2

0.7 6.3

Stdev

SPIFAN Sample #6

10.4

% RSD

8

8

8

n

Mean Stdev

2.2 0.3

1.1 0.1

3.3 0.4

SPIFAN Sample #7

15.3

10.8

13.0

% RSD

7

7

7

n

Mean Stdev

5.9 0.7

1.1 0.1 9.3

7.0 0.8

SPIFAN Sample #8

11.8

11.2

% RSD

8

8

8

n

Mean

7.1 0.4 5.8

1.0 0.1

8.1 0.5 6.1

Stdev

SPIFAN Sample #9

10.1

% RSD

9

9

9

n

Mean Stdev

2.4 0.3

0.3 0.0

2.6 0.3

SPIFAN Sample #10

12.8

11.1

11.0

% RSD

9

9

9

n

Mean

2.2 0.2 7.4

0.4 0.0

2.6 0.2 6.3

SPIFAN Sample #11

Stdev

10.9

% RSD

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

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