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

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

Grand SD

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

mcg/g

Mean %RSD

2.949 0.4%

2.613 2.2%

2.465 0.5%

2.708 3.2%

2.615

0.249

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.

30