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 22: 5-formyl-THF analysis in BCR 485 (dried vegetable powder) over a period of about 3 months 5-CHO-THF Results 09/11/12 09/14/12 09/18/12 10/19/12 10/26/12 11/02/12 mcg/g Mean 0.063 0.070 0.073 0.065 0.059 0.071 %RSD 10.6% 51.1% 12.1% 2.9% 18.7% 12.2% N = 3 3 3 3 3 3 5-CHO-THF Results 11/07/12 11/13/12 12/27/12 Grand Grand SD mcg/g Mean 0.075 0.052 0.054 0.063 0.010 %RSD 5.2% 13.0% 3.2% 15.6% N = 3 3 6 25 25 There is no value provided for 5-formyl-THF for this sample by BCR Total folate as folic acid results obtained for the BCR 485 (dried vegetable powder) by the method over a period of about 3 months are presented in Table 29. The results obtained were quite consistent over period of analysis. Values obtained for total folate as folic acid was about 96% of the lowest range specified for this reference material. Interday as well as intraday precision of the method over a period of about 3 months was found to be satisfactory.

Table 23: Total folate as folic analysis in BCR 485 (dried vegetable powder) over a period of about 3 months

09/11/12 09/14/12 09/18/12 09/21/12 10/10/12 10/12/12 10/19/12 mcg/g

Vitamers sum as Folic

Mean %RSD

2.312 3.5%

2.465 2.3%

2.208 1.0%

2.494 3.5%

3.018 2.2%

3.333 8.0%

2.931 1.9%

N =

3

3

3

3

3

3

3

Grand SD

10/26/12 11/02/12 11/07/12 11/13/12 12/27/12 Grand

Vitamers sum as Folic

mcg/g 2.422

Mean %RSD

2.710 12.5%

2.922 0.1%

3.195 2.3%

2.654 2.4%

2.716 3.0%

0.339

0.6%

N =

3

2

3

3

6

38

38

Certified Total Folate Value* 3.15 + 0.28 *BCR Certified Total Folate value as folic acid obtained by microbiological assay (L. rhamnosus) Method Accuracy Evaluation Repeated: The method accuracy was repeated again recently (API 5500 from ABSciex). The results are presented in the following Table. The results of this investigation again help in establishing the accuracy of the method.

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