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FOR EXPERT REVIEW PANEL USE ONLY
NOT FOR DISTRIBUTION
2
Easy to follow
Method Safety Concerns:
None
Pros/Strengths:
This procedure is a good advancement from traditional methods of analysis for vitamin B
3
. Both
compounds, nicotinic acid and its amide, are readily detected without the interferences found in LC-
UVD methods, thus permitting simplified clean-up procedures or the use of derivatization. Stable
isotopes of the analytes allow effective quantitation during LC-MSMS analysis.
Cons/Weaknesses
The isotopic internal standards are added at the end of the sample preparation and therefore don’t
compensate for manipulative variations during enzyme hydrolysis.
High cost of purchase and operation of LCMSMS equipment
Supporting Data
The report has supporting data for NIST 1849a and eleven SPIFAN matrices. Spiked recoveries have
also been performed.
Performance Characteristics
Table 1 lists performance parameters required by SMPR 2015.004
Table 1. Method performance requirements
a
Analytical range
200–10000
b
Limit of quantitation (LOQ)
≤200
b
Recovery
90–110%
Repeatability (RSD
r
)
≤5%
Reproducibility (RSD
R
)
≤10%
a
Concentrations apply to: (a) “ready-to-feed” liquids “as is”; (b)
reconstituted powders (25 g into 200 g water); and (c) liquid concentrates
diluted 1:1 by weight.
b
μg/100 g reconstituted final product.