2018 Sugar ERP - Method Review Book

3. Are the definitions specified in the SMPR used and applied appropriately in the method? If no, please indicate how the terms are used. 4. Does the method, as written, contain all appropriate precautions and warnings related to the method's reagents, components, instrumentation, or method steps that may be hazardous? If no, please suggest wording or option(s). III. Review of Supporting Information 1. Are the definitions specified in the SMPR used and applied appropriately in the supporting documentation (manuscripts, method studies, etc...)? If not, please explain the differences and if the method is impacted by the difference. 2. Is there information demonstrating that the method meets the SMPR Method Performance Requirements using the Reference Materials stated in the SMPR? If not, then specify what is missing and how this impacts demonstration of performance of the method.

Method validation guidelines and the SMPR definitions are followed and well documented. It is a large method with various multi lab validation results data included. Special appreciation to the method author following the SMPR and method validation guidelines and documenting the outliers wherever applicable.

This method uses solid - Sodium Azide as the stabilizer agent. Sodium azide is rapidly acting, potentially deadly chemical and it can easily can absorbed through skin when exposed. Sodium azide containing internal standard is added to all the samples. With acidic samples – such as juice – sodium azide is converted to hydrazoic acid, which is a low boiling, volatile and highly toxic gas. Other than referencing AOAC appendix B, in section of F of the submitted method, this method does not adequately address the safety aspect related to sodium azide handling. It is highly recommended the safety committee to review this method for the suitability before accepting it for first action. Documentation meets the SMPR requirements. Method Author has done a very good job of writing and compiling the supporting data. Many places author explains the discrepancies from SMPR and comes up with explanations. Outliers were indicated in Bold.

Method is tested using 3 different CRM/SRM substances. For BCR-644 CRM, the sucrose and Lactose monohydrate are not within the RM Range (%). May be because of the gradient interference at the Lactose peak. A shoulder peak close to lactose is visible in Figure 5. This shoulder peak is also visible for NIST 1849 a Infant formula SRM (FIGURE AII-1-3) – May be the integration including the shoulder peak lead to higher recovery and acceptable RM range for this CRM.

For BCR-644 Artificial Foodstuff CRM (FIGURE AII-1-4) – this shoulder peak is not visible and a baseline shift due to hydroxide gradient is noticed.

Specificity and the gradient baseline drift can lead to variation in accuracy - mainly at LOD level.