SPIFAN Nutrients ERP Book_9-29-15

BVit-02 - MEF 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

Method title:

Principle of the method:

Samples are enzymatically digested with a stable isotope labeled internal standard and analyzed by LC-MS/MS.

Weighting factor for parameter

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

Method Performance

Please report

SMPR Requirement

Parameter

in units as stated in SMPR!

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

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

same same same

Analytical Range.

200 - 10000

nearly same

10 - 2000

≤ 20 ≤ 30

9.79 8.65 95.2

Limit of quantification (LOQ)

≤ 200

12.75

≤ 10

92.4 - 102.5, mean 97.1% recovery

95.1 - 100.7, mean 97.9% recovery

Spike recovery (%)

90-110 % mean spiked recovery over the Range

100.3 - 110.7 , mean 103.8% recovery 96.8 - 100.5, mean 99.1% recovery

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

≤ 5% ≤ 5% ≤ 5% ≤ 5%

1.1 2.3 1.2 1.5 3.4 5.1 2.8 4.4

Repeatability (RSDr)

not stated not stated not stated not stated

Intermediate Reproducibility (RSDiR)

≤ 10% ≤ 10% ≤ 10% ≤ 10%

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

Reproducibility (RSDR)

ADDITIONAL EVALUATION PARAMETERS

Adequate proof of performance via system suitability

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

Bias against established method

Is there a bias Yes/No ?

Analytical equipment is commonly available in most labs.

Analytical equipment

No unique proprietary equipment/accessories are required.

Proprietary equipment

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

SPIFAN ERP Checklist v 1.6

27.06.2013