AOAC SPIFAN Review Team Meeting Book-December 2015
VitK-01 MEF FOR ERP USE ONLY DO NOT DISTRIBUTE
Evaluation of Method Performance vs. SMPR requirements.
AOAC SMPR: ………….. AOAC SMPR 2014.001
VITK‐01
Method title: Principle of the method: Method Reference #
A LC‐MS/MS Method for Vitamin K Analysis in Infant Formula and Adult Nutrition Samples
Fat in sample is hydrolyzed by lipase after adding internal std. Vitamin K is extracted by a solvent extraction. The reconstituted extract is analyzed by LC‐MS/MS for vitamin K.
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.
1
SPIFAN matrices
The method is applicable to all the matrices listed in the SMPR.
All analytes defined in the applicability statement are measured.
1
Analytical Range.
1
Analyte 1 Analyte 2 Analyte 3 Analyte 4 Analyte 5 Analyte 1 Analyte 2 Analyte 3 Analyte 4 Analyte 5
trans‐vitamin K1 = 0.5‐100 mcg/100g cis‐vitamin K1 = 0.1‐100 mcg/100g Total‐vitamin K1 = 0.6‐100 mcg/100g
trans‐vitamin K1 = 1‐100 mcg/100g recostituted sample cis‐vitamin K1 = 1‐100 mcg/100g recostituted sample Total‐vitamin K1 = 1‐100 mcg/100g recostituted sample
Limit of detection (LOD)
1
trans‐vitamin K1 = <1 mcg/100g recostituted sample cis‐vitamin K1 = <1mcg/100g recostituted sample Total‐vitamin K1 = <1mcg/100g recostituted sample
trans‐vitamin K1 = 0.5 mcg/100g
cis‐vitamin K1 = 0.1/100g
Limit of quantification (LOQ)
2
Total‐vitamin K1 = 0.6mcg/100g
2
Spike recovery (%) Vitamin K1 (cis + trans) = 90‐100%
Vitamin K1 (cis + trans) = 97.8 + 5.2% (n=44)
Accuracy/Recovery
NIST SRM 1849a Vitamin K1 = 1.00 + 0.10 mg/Kg (n=5)
3
Bias vs SRM NIST SRM 1849a Vitamin K1 = 1.06 + 0.17 mg/Kg
<8% RSD <5% RSD
Repeatability (RSDr)
3
7.90% 6.30%
1‐10 mcg/100g >10 mcg/100g
<8% RSD <5% RSD
Intermediate Reproducibility (RSDiR)
1
Reproducibility (RSDR)
1
ADDITIONAL EVALUATION PARAMETERS
Blank check and lowest and midrange calibration
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.
Method does not require any special safety precautions e.g. personal protection from highly toxic solvents.
Laboratory safety
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
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