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Commodities for Specificity Evaluation:
1.
Maltrin M-40 maltodextrin (Grain Processing Corporation, vendor lot# unknown)
2.
Maltrin M-200 maltodextrin (Grain Processing Corporation, vendor lot# M1213233)
3.
Fibersol 2, resistant maltodextrin(Matsutani, vendor lot# 20090307)
4.
Polydextrose (Danisco, vendor lot# 1922293217)
Apparatus
1.
LC system
- Dionex ICS-3000 or 5000 consisting of a SP, DP, WPS-3000 (TB; P or S type), and an electrochemical cell
with a conventional gold working electrode (p/n 079850) and combination pH Ag/AgCl reference electrode (p/n
061879). Utilizing Chromeleon 6.80 or equivalent.
2.
Analytical Column Set
–
Analytical column, Thermo CarboPac PA1, 250x4mm (p/n 035391);
PA1 guard column
(Thermo p/n 043096).
3.
Analytical Balance
–
readability to 0.01 mg recommended.
4.
Syringe filter
–
0.45 μm nylon (Whatman p/n 6752-2504 or equivalent).
Reagents
1.
Lab water
- ASTM Type 1 water.
2.
50% w/w NaOH
(Fisher p/n SS254-500). If an alternate vendor is selected, it is imperative that the carbonate level be
equivalent to or less than Fisher
(≤0.10%)
.
3.
Sodium Acetate trihydrate
(Sigma p/n 71188).
4.
Helium Gas (Ultra high purity)
5.
Fructan commodities to act as RT standards as noted under fructan materials above.
Preparation of Standards and Spikes
1.
Fructan RT marker standards
–
Weigh 0.4 ± 0.004 g of each fructan reference material (one each of scFOS, Synergy 1,
and HP) and transfer to a 1000 mL volumetric. Bring to volume with lab water. Transfer to autosampler vials. Store at
-20 °C for up to 6 months.
Sample Preparation
1.
Powder sample reconstitution (if needed)
–
Accurately weight 5.0 g ± 10% into a 100 mL beaker (record
powder
weight)
. Tare and deliver 40 g of lab water to beaker (record
water weight
). Allow to stir for 30 minutes, or until
dissolved.
2.
Sample dilution
–
Samples require differing dilutions according to their individual fructan content as follows: Record
all weights to four decimal places.
This aliquot can be shared with the quantitative fructan methodology in Part 2,
do not discard!
Table 1-1
Sample Size Guidelines
Sample type
Fructan Level
(as-is)
SW
1
(g)
Volumetric Flask Size
(mL)
Powder Product
0.27-1.0%
10 g± 10%
50
Powder Product
1.1-10%
7 g± 10%
200
Powder Product
11-45%
4 g± 10%
500
RTF Product
*
0.03-0.20%
10 g± 10%
50
RTF Product
*
0.21-1.0%
7 g± 10%
200
RTF Product
*
1.1-5.0%
4 g± 10%
500
Commodity
45-100%
0.4 g± 10%
1000
*
For concentrated liquid (CL) products dilute 10 mL of product with 10 mL of laboratory water and then treat the resultant
material per RTF guidelines.
3.
Filtration and analysis
–
After bringing the samples to volume, filter through a 0.45 μm nylon syringe filter into an
autosampler vial (prepared samples can be stored in vials at 2-10 °C for 5 days).
Fos-04 (February 2016)
FOR ERP USE ONLY
DO NOT DISTRIBUTE