Table of Contents Table of Contents
Previous Page  35 / 65 Next Page
Information
Show Menu
Previous Page 35 / 65 Next Page
Page Background

FOR EXPERT REVIEW PANEL USE ONLY

NOT FOR DISTRIBUTION

3

biotin. The report does not show these chromatograms nor clarify if the “response” was attributed to

(endogenous) biotin or was an interference.

-

Method Optimization:

Performance Characteristics:

Analytical Range:

The method describes the processing of samples with biotin content over the entire concentration

range stated in the SMPR (0.1 – 150 mcg/100g as fed)

In practice, the concentration encountered in the SLV using the SPIFAN sample set was ~1.5 – 65

reconstituted.

LOQ:

The SMPR LoQ (0.1 mcg/100g reconstituted) is achieved at the lowest standard curve concentration

using the typical sample weight specified in the method for this concentration of analyte.

Accuracy/Recovery:

SMPR:

0.1

– 1 mcg/100g reconstituted: 80 - 120%

> 1 mcg/100g reconstituted: 90 – 110%

Spike and recovery: Four placebo samples (Child Formula, Infant Elemental, Adult RTF High Fat, IF Milk

RTF) were spiked at +50% and +150% of typical target, 3 days in duplicate, with recoveries meeting the

SMPR requirements ranging from 95.2% – 100%. One fortified sample (Adult RTF High Protein) was

spiked similarly and showed recovery of 96.7% - 104%, also meeting the SMPR requirement. (Table 3)

SRM 1849a: the sample was analyzed on 6 different days; the results (range 196.5 – 200.0 mcg/100g as

is) were all well within the Certified Mass Fraction range (199 ± 13 mcg/100g as is). (Table 2)

Precision (RSD

r

):

SMPR:

0.2

– 1 mcg/100g reconstituted: ≤ 8%

> 1 mcg/100g reconstituted: ≤ 6%

Reproducibility (RSD

R

):

SMPR:

0.1

– 1 mcg/100g reconstituted: ≤ 16%

> 1 mcg/100g reconstituted: ≤ 12%

RSD

IR

was characterized by duplicate analysis of the 12 fortified SPIFAN samples across 6 days (2

analysts, 2 instruments). All values were below 3.2%. Although they were not calculated

individually, none of the within day precision values appeared to be greater than this value. The

method could likely meet the SMPR requirements if extended to MLT. (Table 4)

3/2017: The MLT consisted of 12 laboratories from 10 different countries. Three laboratories only

reported results for the practice samples. One of the remaining laboratories produced results