July 2019 Sugar ERP - Review Book

Please provide justification for your answer. If specific requirements were made in the August 29, 2018 meeting, please explain how those requirements have been met or not met.

Test portion has been addressed.

Additional CRMs or SRMs have been analyzed. The accuracy and precision data have no coverage for AOAC sectors 1, 2, 3, and 8. Sector 9 only has accuracy data (no precision data) for lactose. Sector 4 only has precision data, no accuracy data. Sucrose outside of range for CRM 1869 (2 of 4 results and mean outside range). Lactose and maltose are outside SMPR %RSDr criterion (SMPR criterion is less than or equal to 7%, lactose is 14.9% RSD and maltose is 10.2% RSD). Lactose is outside the SMPR %RSDr with 8.2% RSD for MUVA 2310. The report does not explain these results outside the criteria. Additional matrices covering a broader range of AOAC sectors is needed to insure the applicability to the full range of food matrices. The calculation section describes the method as applicable only to 50% individual analyte. This maximum analyte concentration should be clearly defined in the method scope. As presented this method would be applicable to a subset of food matrices that would include cereals, grains, dairy, and dry pet food. Additional information on potential interferences is presented in the report. Not all interferants listed in table 2 of the SMPR are addressed. It appears from the validation data that there could be interference from the following groups of compounds: mannose/galactose, sucrose/epi-lactose/lactulose, cellbiose/lactose. Data on enzymatic activity is presented in the extraction robustness study. This study only addresses lactase enzymatic activity and does not present data on other enzymatic or bacterial catalytic activity that is common with other matrices, such as pet and animal feeds. Also, the extraction robustness study did not provide a control by running with aqueous extraction to show the lactase activity impacts the analysis (assumes the lactase is active and impactful). Organic acid, sugar alcohol, hydroxylated compounds, salts, and amine containing compounds (amino sugars and amino acids) would not likely interfere based on the mass selective detection. In the calibration standard chromatogram there appears to be a small signal in the galactose and glucose retention time for the maltose standard for the m/z 389. Does this same interference appear in the maltose standard for m/z 215 (which is used for galactose and glucose quantitation)? Temperature and % ethanol of extraction have not been addressed in the report. The journal article, Ellingson et al, J AOAC Int, vol 99, No 2, pp 342-352, describes the optimization of ethanol water extraction for sugar extraction as it relates to pet and animal feeds with hydrolytic activity. The journal article demonstrated that 50:50 ethanol:water was the optimal extraction solvent for these analytes and matrices. Higher temperature (above ambient, 60 C in this method) would likely increase hydrolytic activity of complex carbohydrates. Additional data demonstrating the impact of temperature and % ethanol on the analysis have not been presented. Representative chromatograms for calibration standards and potential interferences are presented. Representative chromatograms of samples are not presented. Check standards and blanks have not be included in the report. See paragraph 2 for the information on matrix applicability.