AOACSPIFANMethods-2017Awards
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6 H aselberger & Jacobs : J ournal of AOAC I nternati nal Vol. 99, No. 6, 2016
H aselberger & J acobs : J ournal of AOAC I nternational V ol . 99, N o . 6, 2016 1581
Synergy1
ED_1
40.0 070715-FRUCTANQUAL ID #8
nC
35.0
2 - 2.467 3 - 2.667
30.0
25.0
9 - 6.767
7 - oligofructose - 4.917
20.0
4 -GF3 - 3.167
15.0
6 -GF4 - 4.250
10.0
5 - 3.700
8 - 6.017
1 - 1.767
11 - 8.900
5.0
13 - 11.167
10 - 7.950
18 - 17.634
21 - 22.417
23 - 23.834
19 - 19.317
20 - 20.917
25 - 25.150
27 - 27.617
28 - 28.767
26 - 26.417
17 - 15.850
12 - 9.967
16 - 13.984
14 - 12.017
29 - 29.834
15 - 13.450
30 - 30.884
0.0
31 - 31.867
48 - 42.567
32 - 32.800
33 - 33.700
47 - 42.217
34 - 34.534
36 - 36.184
42 - 40.100
43 - 40.550
45 - 41.400
35 - 35.367
37 - 36.950
44 - 40.984
46 - 41.800
38 - 37.684
41 - 39.600
39 - 38.384
22 - 23.150
40 - 39.034
24 - 24.684
min
-5.0
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
Figure 2016.06B. Beneo Orafti Synergy 1 chromatogram (Part I).
(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. (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 I. Reagents
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.
HP
ED_1
2.50 111815-fructanqual ID #9 [modifiedbyHASELPA]
nC
2.25
2.00
29 - 23.784
28 - 22.650
27 - 21.500
30 - 24.834
1.75
31 - 25.850
25 - 20.250
34 - 27.750
32 - 26.834
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
23 - 18.934
36 - 28.617
39 - 31.017
38 - 30.267
37 - 29.450
1.50
40 - 31.767
41 - 32.484
55 - 39.917
21 - 17.550
42 - 33.167
54 - 39.584
43 - 33.817
44 - 34.450
53 - 39.200
52 - 38.800
51 - 38.350
45 - 35.050
46 - 35.650
50 - 37.850
47 - 36.234
19 - 16.084
48 - 36.800
49 - 37.350
1.25
18 - 14.550
1.00
17 - 12.934
0.75
0.50
16 - 11.250
0.25
2 - 2.217 3 - 2.434 4 -GF3 - 2.650 5 - 3.117 6 -GF4 - 3.334
14 - 9.517
12 - 7.750
7 - oligofructose - 3.917 8 - 4.500 9 - 5.317 10 - 6.050
35 - 28.267
33 - 27.250
11 - 7.017
1 - 1.784
13 - 8.917
26 - 21.184
15 - 10.950
24 - 19.767
-0.00
22 - 18.217
20 - 16.817
-0.25
min
-0.50
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
Figure 2016.06C. Beneo Orafti HP chromatogram (Part I).
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