2015.14 Vitamin B (July 2018)

2015.14 (JULY 2018) BVit‐02 Total Bs ERP Evaluation Form

FOR ERP USE ONLY DO NOT DISTRIBUTE

Evaluation of Method Performance  vs. SMPR requirements.

AOAC SMPR: 2015.002, 2015.003, 2015.004, and 2015.005

BVIT‐02

Method Reference #

Simultaneous Determination of Total Vitamin B6, B2, B3 and B1 in Infant Formula Products by LC‐ MS/MS using Enzyme Digestion Samples are enzymatically digested with a stable isotope labeled internal standard and analyzed by LC‐MS/MS.

Method title:

Principle of the method:

Weighting  factor for  parameter

Suitability Ranking (1‐3‐5)  (select from drop‐down list, 5 =  best)

Method Performance                Please report  in units as stated in SMPR!

SMPR Requirement

Parameter

Applicable to all forms of infant, adult, and/or pediatric  formula (powders, ready‐to‐feed liquids, and liquid  concentrates).  Any combination of milk, soy, rice, whey, hydrolyzed  protein, starch, and amino acids, with and without intact  protein.

All SPIFAN matrices evaluated met precision and  accuracy requirements for all four vitamins.    Precision = 14 matrixes evaluated    Accuracy = 8 unique matrixes evaluated.

 SPIFAN matrices

All analytes defined in the  applicability statement are  measured.

Method determines these four vitamins simultaneously  from the same injection

Total B1, B2, B3, and B6

all units ug/100g of RTF

same same same

Total B1 Total B2 Total B3 Total B6 Total B1 Total B2 Total B3 Total B6 Total B1 Total B2 Total B3 Total B6 Total B1 Total B2 Total B3 Total B6 Total B1 Total B2 Total B3 Total B6 Total B1 Total B2 Total B3 Total B6 Total B1 Total B2 Total B3 Total B6

20 ‐ 2000 30 ‐ 4000

Analytical Range.

200 ‐ 10000

nearly same

10 ‐ 2000

9.79 8.65 95.2

≤ 20 ≤ 30

Limit of quantification (LOQ)

≤ 200

12.75

≤ 10

92.4 ‐ 102.5, mean 97.1% recovery 95.1 ‐ 100.7, mean 97.9% recovery 100.3 ‐ 110.7 , mean 103.8% recovery 96.8 ‐ 100.5, mean 99.1% recovery

Spike recovery  (%)

90‐110 % mean spiked recovery over the Range

2.2% higher than certified 11.5% higher than certified 4.7% lower than certified 1.7% higher than certified

Bias vs SRM

Use SRM 1849a

1.1 2.3 1.2 1.5 3.4 5.1 2.8 4.4

≤ 5% ≤ 5% ≤ 5% ≤ 5%

Repeatability (RSDr)

not stated not stated not stated not stated

Intermediate Reproducibility  (RSDiR)

not tested yet not tested yet not tested yet not tested yet

≤ 10% ≤ 10% ≤ 10% ≤ 10%

Reproducibility (RSDR)

ADDITIONAL EVALUATION PARAMETERS

Adequate proof of performance via system suitability

Feedback from Users of the Method since being awarded  First Action Official Methods  Status Did Method Author Consider ERP’s Method Specific  Recommendations  (See web link to specific method  comments):

Bias against established method 

Is there a bias Yes/No ?

Analytical equipment

Analytical equipment is commonly available in most labs.

Proprietary equipment

No unique proprietary equipment/accessories are required.

Laboratory safety

Method does not require any special safety precautions e.g. personal protection from highly toxic solvents.

Other Considerations

0

Overall Score

Decision by ERP

Recommendation of ERP  2 years after First Action Status

move to Final Action/repeal/remove/expand 2 year term

Notes:

a  Concentrations apply to (1) "ready to feed liquids" "as‐is"; (2) reconstituted powders (25 g into 200 g water); and (3) liquid concentrates diluted 1:1 by weight.

b    Units