SPSFAM ERP

Standard solutions were stored refrigerated and preserved with sodium azide as outlined in the written method. The stability data for these solutions was determined by dividing the analyte response by the determined theoretical values to establish a response factor. The response factors were then compared for percent change between the initial and new working standards. The lowest and highest working standards show acceptable stability over a 6 month time frame as the % change for each level and analytes was less than 3%. The reference standard solution stability is summarized in Table 16 .

Table 16. Reference solution stability data

Initial Theoretical (µg/mL)

New Theoretical (µg/mL)

Initial Average Area

New Average Area

Response Factor Initial

Response Factor New

% Change

Analyte

0.51250 15.375 0.50075 15.023 0.51100 15.330 0.50900 15.270 0.50245 15.074 0.50845 15.254 0.50330 15.099

0.49761 14.928 0.50525 15.158 0.51010 15.303 0.50230 15.069 0.50085 15.026 0.47473 14.242 0.47676 14.303

0.808

0.762

1.577 1.518 1.522 1.482 0.798 0.696 0.835 0.788 0.967 0.978 0.234 0.200 0.719 0.647

1.531 1.483 1.508 1.482 0.778 0.692 0.824 0.786 0.982 0.974 0.232 0.202 0.707 0.652

-2.9 -2.3 -0.9 -2.5 -0.6 -1.3 -0.3 0.0

Galactose

23.346

22.131

0.762

0.762

Glucose

22.264

22.465

0.408

0.397

Sucrose

10.672

10.588

0.425

0.414

Fructose

12.027

11.842

0.486

0.492

1.6

Lactose

14.741

14.642

-0.4 -0.9

0.119 3.053 0.362 9.771

0.110 2.872 0.337 9.323

Isomaltulose

1.0

-1.7

Maltose

0.8

Sample solutions from two separate points of the extraction process were analyzed for stability. The first of these sample stability points the injection vial stability, and it was taken from the endpoint of extraction (final injection vial). Stability data points were taken from the exact same injection vials stored at room temperature. The second sample stability solution was taken at the step where water is added to the dried filtrate. These extracts were stored refrigerated at 5±3°C. The extraction process was completed at each stability time point and injected. Three replicates of NIST 3233 were used as the test sample for this exercise, and the data collected was independent of precision and accuracy data collections. The three replicates were averaged to form one value. Stability data was collected at time points of 4, 7, and 14 days. This data is tabled below in Table 17.