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Silliker

Chem, Res. Center Crete, IL – Report of A Validation of LC-MS/MS Method for Folate Analysis

30

Table 20: 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 27. 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.

Interday as well as intraday precision of the method over a period of about 3 months was found to be

satisfactory.

5-formyl-THFresults obtained for the BCR 485 (dried vegetable powder) by the method over a period

of about 3 months are presented in Table 28. The results obtained were quite consistent over period of

analysis. The BCR has not reported any value for 5-formyl-THF in this matrix. Interday as well as

intraday precision of the method over a period of about 3 months was found to be satisfactory.

Table 21: 5-methyl-THF analysis in BCR 485 (dried vegetable powder) over a period of about 3

months

5-CH3-THF Results 09/11/12 09/14/12 09/18/12 09/21/12 10/10/12 10/12/12 10/19/12

mcg/g

Mean

2.291

2.453

2.179

2.530

2.900

2.881

2.881

%RSD

3.4%

0.9%

1.5%

3.2%

1.7%

-

2.1%

N =

3

3

3

3

3

1

3

5-CH3-THF Results 10/26/12 11/07/12 11/13/12 12/27/12 Grand

Grand

SD

mcg/g

Mean

2.949

2.613

2.465

2.708

2.615

0.249

%RSD

0.4%

2.2%

0.5%

3.2%

9.5

N =

3

3

3

6

35

35

Indicative Value*

2.14 + 0.42

*BCR Indicative Value, is not a certified value obtained by BCR analysis using a LC fluorescence

method and hog kidney conjugase based extraction and SPE clean-up.

2011.06 (Fol-22) w/SLV

FOR ERP USE ONLY

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