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H
aselberger
&
J
acobs
:
J
ournal of
AOAC I
nternational
V
ol
.
99, N
o
. 6, 2016
1581
6
H
aselberger & Jacobs
: J
ournal of
AOAC I
nternati nal
Vol. 99, No. 6, 2016
(n)
Desiccator and indicating Drierite (or equivalent)
desiccant.
(o)
Eluent filtration apparatus with disposable membrane
filter.—
0.2 μm PES.
(p)
Micropipettor and tips.—
Assorted sizes.
(q)
Reagent bottles.—
Glass and plastic, assorted sizes.
(r)
Beakers.—
Glass, assorted sizes.
(s)
Helium sparge.—
Tubing and frit assembly.
I.
Reagents
(a)
Laboratory water.—
ASTM Type 1 water.
(b)
NaOH solution
.—50%, w/w (Fisher Part No. SS254-500
or equivalent). If an alternate vendor is selected, it is imperative
that the carbonate level be equivalent to or less than Fisher
(≤0.10%).
(c)
NaOH solution.—
1 M.
(d)
Sodium acetate trihydrate.—
Reagent grade.
(e)
Glucoheptose.—
Sigma Part No. 71188 or equivalent.
Note
: This reagent has been discontinued by Sigma. Alternate
suppliers include: Carbosynth (Part No. MG05213), MP
Biomedicals (Part No. 05207893), and Cedarlane Labs (Part
No. 157755 or 0520789380).
(f)
Fructose.—
Reference grade.
(g)
Sodium borohydride.—
>98% purity.
(h)
Maleic acid.—
>99.0% purity.
(i)
Acetic acid.—
Glacial, ACS.
(j)
Fructanase.—
Megazyme Part No. E-FRMXPD, or
equivalent.
(k)
Sucrase.—
Megazyme Part No. E-SUCR. Demonstration
of equivalent absence of activity toward fructan material is
required for any substitutions.
J. Preparation of Standards and Solutions
(a)
Fructose stock solution 100 µg/mL.—
Weigh 0.05 ±
0.0025 g fructose reference material and transfer to a 500 mL
volumetric. Bring to volume with laboratory water.
(b)
Glucoheptose IS
.—Weigh 0.1 ± 0.005 g of glucoheptose
and transfer to a 100 mL volumetric. Bring to volume with
laboratory water. It is recommended to portion out aliquots of
this solution to avoid multiple freeze thaw cycles and extend
useful life of reagent. Store frozen at –20°C for up to 6 months.
0.0
2.0
4.0
6.0
8.0
10.0
12.0
14.0
16.0
18.0
20.0
22.0
24.0
26.0
28.0
30.0
32.0
34.0
36.0
38.0
40.0
42.0
44.0
46.0
48.0
50.0
52.0
54.0
56.0
58.0
60.0
-0.50
-0.25
-0.00
0.25
0.50
0.75
1.00
1.25
1.50
1.75
2.00
2.25
2.50 111815-fructanqual ID #9 [modifiedbyHASELPA]
HP
ED_1
nC
min
1 - 1.784
2 - 2.217 3 - 2.434
4 -GF3 - 2.650
5 - 3.117 6 -GF4 - 3.334
7 - oligofructose - 3.917
8 - 4.500
9 - 5.317
10 - 6.050
11 - 7.017
12 - 7.750
13 - 8.917
14 - 9.517
15 - 10.950
16 - 11.250
17 - 12.934
18 - 14.550
19 - 16.084
20 - 16.817
21 - 17.550
22 - 18.217
23 - 18.934
24 - 19.767
25 - 20.250
26 - 21.184
27 - 21.500
28 - 22.650
29 - 23.784
30 - 24.834
31 - 25.850
32 - 26.834
33 - 27.250
34 - 27.750
35 - 28.267
36 - 28.617
37 - 29.450
38 - 30.267
39 - 31.017
40 - 31.767
41 - 32.484
42 - 33.167
43 - 33.817
44 - 34.450
45 - 35.050
46 - 35.650
47 - 36.234
48 - 36.800
49 - 37.350
50 - 37.850
51 - 38.350
52 - 38.800
53 - 39.200
54 - 39.584
55 - 39.917
56 - 40.234
57 - 40.534
58 - 40.834
59 - 41.117
60 - 41.400
61 - 41.667
62 - 41.900 63 - 42.150 64 - 42.367
Figure 2016.06C. Beneo Orafti HP chromatogram (Part I).
0.0
2.0
4.0
6.0
8.0
10.0
12.0
14.0
16.0
18.0
20.0
22.0
24.0
26.0
28.0
30.0
32.0
34.0
36.0
38.0
40.0
42.0
44.0
46.0
48.0
50.0
52.0
54.0
56.0
58.0
60.0
-5.0
0.0
5.0
10.0
15.0
20.0
25.0
30.0
35.0
40.0 070715-FRUCTANQUAL ID #8
Synergy1
ED_1
nC
min
1 - 1.767
2 - 2.467
3 - 2.667
4 -GF3 - 3.167
5 - 3.700
6 -GF4 - 4.250
7 - oligofructose - 4.917
8 - 6.017
9 - 6.767
10 - 7.950
11 - 8.900
12 - 9.967
13 - 11.167
14 - 12.017
15 - 13.450
16 - 13.984
17 - 15.850
18 - 17.634
19 - 19.317
20 - 20.917
21 - 22.417
22 - 23.150
23 - 23.834
24 - 24.684
25 - 25.150
26 - 26.417
27 - 27.617
28 - 28.767
29 - 29.834
30 - 30.884
31 - 31.867
32 - 32.800
33 - 33.700
34 - 34.534
35 - 35.367
36 - 36.184
37 - 36.950
38 - 37.684
39 - 38.384
40 - 39.034
41 - 39.600
42 - 40.100
43 - 40.550
44 - 40.984
45 - 41.400
46 - 41.800
47 - 42.217
48 - 42.567
Figure 2016.06B. Beneo Orafti Synergy 1 chromatogram (Part I).
26