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

compounds after adjusting their values to folic acid.

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 compounds. Table 28: % Spike Recovery of folate compounds in SPIFAN samples spiked with folate compounds at three different spike levels. The results evaluated for total folate (sum of evaluated folate compounds after adjustment to folic acid).

Spike 2 T = 126; I = 19 mcg/100g*

% Spike Recovery Parameters

Spike 1 T= 492; I = 75 mcg/100g*

Spike 3 T = 63; I = 10 mcg/100g*

Sample #

Analyzed as

All Levels*

Sample

Lot #/ID

Matrix

Av % Recov

105.2

103.2

103.3

103.9

Child Formual Powder

Reconst. Beverage

1

Powder

004011RF00

SD

1.0 0.9

1.2 1.2

3.5 3.4

2.1 2.1

% RSD

Av % Recov

100.7

97.0

98.0

98.6

Infant Formula Powder

Reconst. Beverage

2

Powder

SD

2.6

1.8

1.5

2.4

00402RF00

% RSD

2.6

1.8

1.5

2.4

Av % Recov

93.5

90.5

93.2

92.4

Adult Nutritional RTF High Protein Adult Nutritional RTF High Fat Infant Formula Powder Milk Based, SPIFAN Blank Milk Form

3

Beverage

As is

SD

0.0

1.4

0.4

1.6

00415RF00

% RSD

0.0

1.6

0.4

1.7

Av % Recov

91.3

87.6

98.7

92.6

4

Beverage

As is

00407RF00

SD

1.7 1.9

1.4 1.6

7.1 7.2

6.2 6.7

% RSD

Av % Recov

101.6

101.2

100.7

101.2

SD

1.0

3.8

2.5

2.369

5

Beverage

As is

00394RF00

% RSD

0.9

3.7

2.5

2.3

* Samples were spiked with each targeted folate compound. Total Folic calcluted as sum of the folate compnds after adjusting their values to folic acid. Spike levels are for Total Folate (T) and individual folate compounds (I) Each provided value is an average of three independent replicates. Spike recovery of the different spike levels was evaluated on different days. The liquid beverage samples and the RTF liquid samples were analyzed for folate compounds and expressed as total folate after adjusting to folic acid in and % spike recovery calculated in sample at different spike levels (I, II and II). Results are presented in the above Table. All the 5 samples received from SPIFAN were analyzed in replicates at different spike levels were analyzed on different days. All replicates of the same spike level samples were analyzed on the same day. The samples were spiked with each targeted folate compound (at equal level of each of seven targeted compound) and sum of all folate compounds as folic acid provided folic acid spike level for the sample. Spike levels were calculated as mcg/100g (reconstituted beverage/RTF).

37