SPDS ERP - TEA-01

Std

L-Theanine concentration

L-Norleucine concentration

Relative back-calculated errors, %

Day 1 0.37 0.02 0.09 0.14 -0.78 -0.67 -1.35 1.35 1.05 -0.02 3.74 4.19 1.70

Day 2 0.51 1.21 0.26 -0.41 -1.01 -0.73 -2.13 -1.99 -1.91 -3.33 3.49 -0.79 6.82

Day 3 -0.31 0.28 0.22 0.88 -0.14 -0.49 -0.63 0.68 -1.03 -1.65 -3.55 1.09 14.9

Day 4 0.17 -0.11 0.82 0.01 -0.73 -0.49 0.16 -0.69 -1.36 -0.30 -1.75 -0.17 4.43

Day 5 0.69 -0.05 -0.06 -0.55 0.02 0.14 -0.71 0.02 0.01 -0.48 0.82 -0.33 0.88

Day 6 0.29 -0.88 0.36 1.08 0.24 -0.49 -1.45 -0.25 -2.03 1.69 2.13 4.24 -4.95

1 2 3 4 5 6 7 8 9

100 ug/mL 80 ug/mL 60 ug/mL 50 ug/mL 40 ug/mL 25 ug/mL 20 ug/mL 10 ug/mL 7.48 ug/mL

10 ug/mL 10 ug/mL 10 ug/mL 10 ug/mL 10 ug/mL 10 ug/mL 10 ug/mL 10 ug/mL 10 ug/mL 10 ug/mL 10 ug/mL 10 ug/mL 10 ug/mL

10 11 12 13

5 ug/mL 2 ug/mL 1 ug/mL

0.5 ug/mL

Table 8. Ruggedness Trial Experimental Design

Factor

Value 1

Value 2

Formulation of Ninhydrin Reagent

T100, 1-part Ninhydrin Reagent (A)

T200, 2-part Ninhydrin Reagent (a)

HPLC Flow Rate Extraction Volume

0.35 mL/min (B)

0.38 mL/min (b)

25 mL (C)

10 mL (c)

Analyst

Analyst 1 (D)

Analyst 2 (d)

Extraction time

2h (E)

1.5 h (e) Lot 2 (f) 125 o C (g)

Extraction Solution Li220 Reactor Temperature

Lot 1 (F) 130 o C (G)

Experiment Number

Combination of Factors

1 2 3 4 5 6 7 8

ABCDEFG ABcDefg AbCdEfg AbcdeFG aBCdeFG aBcdEfG abCDefG abcDEFg

Table 9. Results of the Ruggedness Trial

The Effect of Changing Factors Calculated as Described (20) √ *SD = 0.0639 A-a 0.0467 < √2 *SD B-b 0.0002 < √2 *SD

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