SPSFAM ERP

Figure 2. System configuration schematic

I.

System Suitability/Analytical Quality Control

(a) Each set of samples (analytical batch) must be analyzed with a validated control or spike recovery sample and a set of calibration standards covering the analytical range. Spike recoveries are evaluated using AOAC Guidelines Single-Laboratory Validation of Chemical Methods for Dietary Supplements and Botanicals, Appendix K. (b) A single calibration curve is injected at the beginning of each injection sequence. WS3 is injected as a check standard and is injected, at a minimum, between every 6 samples and at the end of the injection sequence. The measured concentration of each analyte in the check standard must be ± 5% of the analyte theoretical concentration. (c) The obtained calibration curve should have acceptable linearity with coefficient of determination r 2 ≥ 0.998. (d) Calibration curve residuals (relative error) must be ≤10% for the lowest calibration level, and ≤5% for the other calibration levels. (e) Inject at least 3 replicates of the check standard at the beginning of each sequence. The response factor %RSD of these injections must be ≤3% for all analytes. The response factor (RF) is the ratio of the analyte area to the internal standard area divided by the analyte concentration. Perform calibration using 1/x weighted linear regression where the abscissa (x-axis) is the external working analyte standard concentration (µg/mL) and the ordinate (y-axis) is a response factor defined as: ൌ A ୍ୱ୲ୢ Where: A = the analyte peak area J. Calculation (a) Integrate the analyte and internal standard (arabinose) peak areas in each standard and sample. (b)