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Chem, Res. Center Crete, IL – Report of A Validation of LC-MS/MS Method for Folate Analys
17
Table 8: Folic Acid analysis in NIST SRM 1849a (Milk based Infant Formula) over a period of
about 3 months
Folic
Acid
Results
08/28/12 09/11/12 09/14/12 09/18/12 9/21/12 09/26/12 09/28/12 10/02/12 10/12/12 10/19/12
mcg/g
Mean
2.306
2.145
2.460
2.065
2.288
2.301
2.390
2.349
2.268
2.404
%RSD
7.8%
2.9%
4.2%
1.9%
4.2%
0.4%
1.4%
5.0%
4.9%
2.3%
N =
3
3
3
3
3
3
3
3
3
3
Folic
Acid
Results
10/26/12 11/02/12 11/07/12 11/13/12 11/17/12 11/26/12 11/29/12 Grand
Grand
SD
mcg/g
Mean
2.337
2.641
2.170
2.147
2.123
2.241
2.277
2.282
0.151
%RSD
1.7%
5.8%
3.5%
6.2%
2.4%
0.5%
5.5%
6.6
N =
3
2
3
3
3
3
3
50
50
NIST
Value
2.293 + 0.062
Micro
Results
2.31*
*Result for total folate in sample as folic acid (based on a single analysis)
5-methyl-THFresults obtained for the NIST SRM 1849a by the method over a period of about 3
months are presented in Table 15. The comparison of the results obtained vs NIST specified value has
already been discussed earlier. Intra-day precision (range as % RSD = 1.8% to 12.5%) as well as
interday precision (% RSD of 12.1%) of the method over a period of about 3 months was found to be
satisfactory (Table 9).
Table 9: 5-methyl-THF analysis in NIST SRM 1849a (Milk based Infant Formula) over a period
of about 3 months
5-CH3-THF
Results
08/28/12 09/11/12 09/21/12 09/26/12 09/28/12 10/02/12 10/12/12 10/19/12
mcg/g
Mean
0.146
0.125
0.153
0.173
0.177
0.185
0.159
0.183
%RSD
3.3%
0.6%
12.5%
2.7%
1.8%
8.8%
2.3%
2.6%
N =
3
3
3
3
3
2
3
3
5-CH3-THF
Results
10/26/12 11/07/12 11/13/12 11/17/12 11/26/12 11/29/12 Grand
Grand
SD
mcg/g
Mean
0.195
0.141
0.173
0.170
0.165
0.181
0.166
0.020
%RSD
2.6%
5.3%
2.3%
3.9%
1.8%
2.4%
12.1
N =
3
3
3
3
3
3
41
41
Ref Value*
0.084 + 0.031
NIST Reference Value, it's not a certified value based on NIST LC-MS in house value
5-methyl-THFresults obtained for the BCR 485 (dried vegetable powder) by the method over a period
of about 3 months are presented in Table 10. The results obtained were quite consistent over period of
analysis. 5-methyl-THF in BCR 485 was estimated by the method close to the reported upper range.
Intraday precision (% RSD range = 0.9-3.4%) as well as interday precision (% RSD = 9.5%) of the
method over a period of about 3 months was found to be satisfactory (Table 10).
5-formyl-THF results obtained for the BCR 485 (dried vegetable powder) by the method over a period
of about 3 months are presented in Table 11. The results obtained were quite consistent over the period
of analysis. The BCR has not reported any value for 5-formyl-THF in this matrix. Intraday precision
2011.06/Fol-22 (February 2016)
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