AOAC SMPR 2012.006 Table 1.

Method performance requirementsa

Analytical range 100 ppm–100%
Limit of quantitation (LOQ) ≤100 ppm
Standard Method Performance Requirements
for Vitamin K in Pre-Blends, Pre-Mixes, and Pure Repeatability (RSDr) 0.01% ≤4%
Materials 1% ≤2%
100% ≤1%
1 Applicability
Recovery 90 to 110% of mean spiked
Determination of vitamin K, defined as the sum of cis and recovery over the range of the
trans isomers of vitamin K1 (phylloquinone or phytomenadione assay
or phytonadione), dihydro-K1, and vitamin K2 (the menaquinone Reproducibility (RSDR) 0.01% ≤8%
series), in food ingredients such as pre-blends, pre-mixes, and pure 1% ≤4%
materials, including encapsulated and oil forms. 100% ≤2%
2 Analytical Technique a
Acceptance criteria are on the total analyte basis.

Chromatographic methods that utilize common instrumentation

that are readily available worldwide. 4 Method Performance Requirements
3 Definitions
See Table 1.
Pre-blends and pre-mixes.—Mixtures of one or more food 5 System Suitability Tests and/or Analytical Quality Control
additives, with food materials or water used as a carrier, and not
Suitable methods will include blank check samples, and check
intended for direct consumption by humans.
standards at the lowest point and midrange point of the analytical
Limit of quantitation (LOQ).—The minimum concentration
range.
or mass of analyte in a given matrix that can be reported as a
6 Reference Material(s)
quantitative result.
Repeatability.—Variation arising when all efforts are made Use suitable materials.
to keep conditions constant by using the same instrument and 7 Validation Guidance
operator, and repeating during a short time period. Expressed as the
repeatability standard deviation (SDr); or % repeatability relative Recommended level of validation: Official Methods of
standard deviation (%RSDr). AnalysisSM.
Reproducibility.—The standard deviation or relative standard 8 Maximum Time-to-Results
deviation calculated from among-laboratory data. Expressed as No maximum time.
the reproducibility standard deviation (SDR); or % reproducibility
relative standard deviation (%RSDR). Approved by the AOAC Stakeholder Panel on Strategic Food
Recovery.—The fraction or percentage of spiked analyte that is Analytical Methods (SPSFAM) on September 29, 2012. Final Version
Date: September 28, 2012.
recovered when the test sample is analyzed using the entire method.

© 2012 AOAC INTERNATIONAL