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FOR EXPERT REVIEW PANEL USE ONLY
NOT FOR DISTRIBUTION
2
Cons/Weaknesses
Each oligosaccharide has an equivalent molar response in the detector.
It is necessary to know the molecular weight of each signal in the chromatogram to convert the molar
quantities analyzed to mass quantities. This can be done by coupling a mass spectrometer (but once a GOS
ingredient profile has been characterized by HILIC-FLD-MS, future samples can be analyzed without the MS).
Supporting Data
General Comment:
-
Method Optimization:
Performance Characteristics:
–
Does the method meet the SMPR for the following:
Analytical Range
:
SMPR 0.2 – 5.0 g/100 g
0.2 – 5.0
LOQ:
SMPR ≤ 0.2 g/100 g
≤ 0.15 g/100 g
Accuracy/Recovery:
SMPR 90 – 110 % of mean spiked recovery over the range of the assay
85 – 114 %
Four different blank matrices were spiked at four levels with two different GOS ingredients.
Recoveries were calculated by comparing the spiked amount vs the measured amount .
Performance is poorest at the lowest spike level (0.2 g/100g) with spike recoveries ranging from
85‐114%, at the other three levels the recoveries are in the range 86 – 94%, but in most cases the
recoveries are outside the 90 – 110% range specified in the SMPR, and in most cases the recoveries
are slightly low.
Precision (RSD
r
):
SMPR ≤ 6 %
1.0
‐3.6 %
All samples from the SPIFAN kit were analysed in duplicate on a single day, and five of the samples
were found to contain GOS.
Each of the GOS‐containing samples from the SPIFAN kit, and the two samples purchased from the