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Validation of a LC-MS/MS method of Analysis of Nicotinic acid and Nicotinamide in infant formula and adult
nutritional samples
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Copyright © 2012 Silliker, Inc.
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The inter-day precision of the total niacin estimation in replicates (n=6 except NIST SRM with
n=4) on two days by the method in the SPIFAN samples in terms of % RSD varied in the range of
3.5% to 6.0%. The inter-day precision was slightly higher than 5% specified in the SMPR in some
of the samples though the value presented in the study are for the inter-day precision (Tables 3
and 4).
Spike Recovery Evaluation in SPIFAN Sample:
Spike Recovery of nicotinic acid as well as nicotinamide was evaluated in a SPIFAN
sample (Child Formula powder) at three different concentrations. . The summary of the
spike recovery results is presented in the following Table.
Table 5: Spike recovery evaluation of nicotinic acid and nicotinamide in a SPIFAN
Sample at different concentrations.
Average % Spike Recovery (n = 3)
Spike amount mcg/100g of the
reconstituted sample
Spike Level -->
250 (n=3)
500 (n=3)
1000 (n=3)
Nicotinic acid
99.5
99.5
99.5
Nicotinamide
99.4
99.4
99.4
Total Niacin
99.5
99.5
99.5
Child Formula powder sample was analyzed in replicates
wth and without spikes of different concentrations of
nicotinic acid as well as nicotinamide and their spike
recovery was estimated.
The % spike recovery of the nicotic acid and nicotinamide at all the concentrations
studied was found to be within 99.4 - 99.5%.
LOD / LOQ
Determination of the Method
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The LOD and LOQ of the method were determined by replicate analysis of one of the
SPIFAN sample (
Adult Nutritional Powder Milk Protein based)
.
The sample was
analyzed in replicates (n=3) on multiple days (2 days) (total n=6). LOD & LOQ are calc
by 3*Stdev and 10*Stdev for total vitamin B3 (niacin) and the result are summarized in
the following Table 6.
VALIDATION REPORT
FOR ERP USE ONLY
DO NOT DISTRIBUTE