6. AOACSPIFANMethods-2018Awards

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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).