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Chem, Res. Center Crete, IL – Report of A Validation of LC-MS/MS Method for Folate Analys
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Spike Recovery Evaluation in SPIFAN samples at different spike levels:
Two beverages prepared from the respective powdered samples and three RTF samples were analyzed
for all the targeted folate compounds with and without spike with respective folate compounds. The
samples were spiked with the folate compound at three spike levels . The results are presented in Table
21.
Table 21: % Spike Recovery of folate compounds in SPIFAN samples spiked with folate
compounds at three different spike levels. The results are for total folate (sum of folate
compounds after adjustment to folic acid).
Sample#
Sample
Lot#
Spike
Level
Spike of
individual
folates
compounds
as folic acid
Spike of total
folate
calculated as
folic acid
Average %
Spike
Recovery of
total folate
(n=3)
% RSD 0f the
total folate
spike recovery
replicates
(n=3)
mcg/100g
1
Child Formula
Powder
00411RF00
REC'D
12/4/15
I
70-80
500.0
97.8
0.7
II
20
120.0
99.7
0.7
III
10
60.0
103.5
1.8
2
Infant
Elemental
Powder
00402RF00
REC'D
12/4/15
I
60-70
500.0
98.1
1.2
II
20
120.0
98.8
1.4
III
10
60.0
99.1
1.5
3
Adlt
Nutritional
RTF, High
Protein
00821RF00
REC'D
12/4/15
I
60-70
500.0
93.1
0.03
II
20
120.0
95
0.6
III
10
60.0
95.1
3.9
4
Adult
Nutritional
RTF, High Fat
00820RF00
REC'D
12/4/15
I
60-70
500.0
94.3
1.0
II
20
120.0
93.5
0.9
III
10
60.0
98.8
3.5
5
Infant Formula
RTF Milk Based
(SPIFAN Blank
Milk Form)
EV4H2Q
REC'D
12/4/15
I
60-70
500.0
104.4
3.5
II
20
120.0
107.2
1.0
III
10
60.0
111.5
0.9
* Samples were spiked with each targeted folate compound at three different spike levls. Spike recovery of total
Folate calculated based on sum of the folate compounds as folic acid. Each spike recovery value is an average of
three independent analysis.
Results in the above Table 21 for % spike recovery of folic acid at varied spike levels analyzed in
SPIFAN matrices ranged from 93 to 107%. One of the samples at one of the spike levels provided a
slightly higher recovery of 111.5%. All of the other samples at every spike level provided spike
recovery within the recovery range 90-110% as required by the Folate SMPR. Folate % spike
recovery analysis was satisfactory in all of the studied SPIFAN matrices at investigated spike levels
except one of the sample at the lowest spike level of 60 mcg/100g providing about 1.5% higher
recovery than the SMPR upper range.
The repeatability of % spike recovery analysis in multiple replicate was evaluated as % RSD value. %
RSD of % spike recovery analysis of total folic acid at varied spike levels in replicates of SPIFAN
matrices ranged from 0.03 % to 3.5 %. The repeatability of folate recovery analysis was found to be
2011.06/Fol-22 (February 2016)
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