AOAC OMB Final Action Recommendation (December 2019)-2016.14

2016.14 (October 2019) – FOS-03 MANUSCRIPT

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Table 8. Summary of analytical conditions and modifications used by laboratories 1 Lab code Option Carrez HPAE Column Post-column addition Comment

1 2 3 4

No

PA1

0.13 mL/min Little positive pressure applied on top of the SPE column.

Example of chromatograms under Figure 1 .

Yes Yes

PA20

No

PA1

0.13 mL/min

No

PA1 a

0.52 mL/min Little positive pressure applied on top of the SPE column; Flow 1.0 mL/min; Injection volume 25 µL; Calibration done by Height. Example of chromatograms Figure 2 .

5 6

Participant dropped out

Elution program described in Table 9 ; Column temperature 20 °C; Injection volume 10 µL. Example of chromatograms Figure 3 . Flow gradient described in Table 10 ; Column temperature 30 °C; Injection volume 20 µL; Detector mode flexIPAD at 35 °C; Waveform described in Table 11 . Example of chromatograms Figure 4 . The sample was loaded on the SPE column with a small pressure on top; Elution program described in Table 12 ; Column temperature 30 °C. Example of chromatograms Figure 5.

No

PA10 a

No

7

No

Metrosep Carb 2 b

No

8

No

PA1 a

No

9

No

PA1 a

0.6 mL/min Applied some vacuum during SPE. Flow 1.0 mL/ml; Injection volume 25 µL.

10 11 12

Participant dropped out

Example of chromatograms Figure 6.

Yes Yes

PA1

No No

PA1 a

SPE performed under some vacuum; Elution program described in Table 13 ; Column temperature 30 °C; Injection volume 25 µL. Example of chromatograms Figure 7.

13 14

No No

PA20

0.2 mL/min

PA1 0.13 mL/min Used pump assist for SPE (day 1 only). Injection volume 25 µL. a Analytical column dimension (4 x 250 mm, 10 µm); guard column dimension (4 x 50 mm, 10 µm). 2 b Analytical column dimension (4 x 250 mm, 5 µm); guard column dimension (5 x 4 mm, 5 µm).

3 4

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