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FOR EXPERT REVIEW PANEL USE ONLY
NOT FOR DISTRIBUTION
2
Cons/Weaknesses
•
Method does not show validation data for any of the SPIFAN matrices (only NIST 1849a)
•
Methionine sulfone separation has very low peak resolution
•
Internal standard is added after hydrolysis, transfer and filter steps so it is only adjusting for instrument
recovery and no prep losses.
Supporting Data
•
General Comment: Method has supporting validation data in NIST SRM 1849a only
-
Method Optimization: Concerns regarding resolution of methionine sulfone peak.
•
Performance Characteristics:
Analytical Range: 3.6 mg/100g-22,500mg/100g. (SMPR: 0.4 mg/100g-2500 mg/100g)
LOQ: 3.6 mg/100g on an as is basis (SMPR: 0.4 mg/100g on reconstituted powder basis)
Accuracy/Recovery: For NIST 1849a recoveries reported ranged from 92.4-107.6 based on result
obtained vs NIST SRM reference value. No spike recovery data reported in any SPIFAN matrices.
Precision (RSD
r
): On NIST SRM 1849a ranged from 0.6-3.2% RSD (not listed for Trp). It is not clear
how many replicates were performed to determine this value.
Reproducibility (RSD
R
): Reported in NIST SRM 1849a to range from 1.4-4.9% RSD(R) however it is
not clear what values were included and/or how this was determined.
•
System suitability:
Not specified in current documents.
Recommendation:
Request for SLV data in SPIFAN matrices.
Amino-03 Review Forms