AOAC SPIFAN ERP Meeting Book-March 16, 2016
2011.06 (Fol-22) w/SLV FOR ERP USE ONLY DO NOT DISTRIBUTE
Silliker Chem, Res. Center Crete, IL – Report of A Validation of LC-MS/MS Method for Folate Analysis
The SPIFAN samples were spiked with each targeted folate compound (at equal level of each of seven targeted compound) and total spike level as folic acid calculated as sum of concentration of all folate compounds as folic acid. Results in the above Table % spike recovery of folic acid at varied spike levels analyzed in SPIFAN matrices ranged from 88 to 106%. Only one of the samples at one of the spike level provided 88% spike recovery. All other samples at every spike level provided spike recovery within the recovery range 90-110% stipulated by the SMPR. Folate recovery analysis was satisfactory in all of the studied SPIFAN matrices at investigated spike levels. The repeatability of % spike recovery analysis in multiple replicate was evaluated as % RSD value. % RSD of % spike recovery analysis of folic acid at varied levels in replicates analyzed in SPIFAN matrices ranged from 0.009 % to 7.2 %. The spike recovery of folic acid at different spike levels analyzed in SPIFAN matrices was within range mentioned in the SMPR. The repeatability of folate recovery analysis was found to be satisfactory in all of the studied SPIFAN matrices at investigated spike levels. The results of the spike recovery evaluation are presented in simplified form in the following Table. All SPIFAN samples were spiked in triplicates with targeted folate compounds at three different levels (spike Level I, II and III) were evaluated for spike recovery of total folate (sum of spiked/analyzed folate compounds as folic acid) on different days. Averages of per cent spike recovery of total folate in replicates of all the samples calculated irrespective of their level of the spike. This provides a comprehensive and simpler evaluation of the spike recovery in the reconstituted and RTF SPIFAN samples. Table 29: % Spike recovery of total folate in samples spiked with targeted folate irrespective of the level of the spike
Average (%) Spike Recovery in All Spike samples*
% Spike Recovery Parameters
Sample #
Analyzed as
Sample
Lot #/ID
Matrix
Av % Recov
103.9
Child Formual Powder
Reconst. Beverage
1
Powder
SD
2.1
004011RF00
% RSD
2.1
Av % Recov
98.6
Infant Formula Powder
Reconst. Beverage
2
Powder
SD
2.4
00402RF00
% RSD
2.4
Av % Recov
92.4
Adult Nutritional RTF High Protein Adult Nutritional RTF High Fat Infant Formula Powder Milk
3
Beverage
As is
SD
1.6
00415RF00
% RSD
1.7
Av % Recov
92.6
4
Beverage
As is
SD
6.2
00407RF00
% RSD
6.7
Av % Recov
101.2
SD
2.4
5
Beverage
As is
00394RF00
Based, SPIFAN
% RSD
2.3
38
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