AOAC SPDS ERP DECEMBER 15, 2017

3. Is there information demonstrating that the

The method provides limit of quantitation (LOQ) data for the 5 required cannabinoids, with 4 of the 5 required cannabinoids achieving the SMPR specification for LOQ. CBD was determined to have an LOQ of 0.17% whereas the LOQ SMPR specification was = 0.1%. LOQs were provided for 3 of the “additional, desirable cannabinoids”; THCV, CBD, and CBC. All three of these LOQs were below the LOQ SMPR specification. The method provides recovery data for 4 of the 5 required cannabinoids, CBN was not included. Of the 4 cannabinoids tested, 2 were tested in the midrange (>1-25%) with CBDA meeting the recovery requirements and THCA falling just outside of the 97-103% range at 96.1% recovery. All 4 cannabinoids were tested in the low range (0.1- 1%) and at the lowest level 0.1% all 4 met the recovery SMPR*. The lower ranges tested are understandable due to challenges associated with procuring high concentration CRMs, but it is important to point out that the recovery of CBD, THCA, and THC technically do not meet the recovery SMPR at the highest concentrations tested (1%, 3.5%, and 1% respectively). The supporting info provides an extraction study suggesting that a single methanol extraction is exhaustive. This helps bolster the recovery data already provided in the method. Repeatability data was provided for all 5 of the required cannabinoids as well as 3 additional cannabinoids (THCV, CBG, and CBC). The Repeatability data, reported as %RSD, was generally within the SMPR specification* with the notable exception of THCA & CBDA in samples CAN008 & CAN009. It is unclear if this inhomogeneity is an artifact of an inhomogeneous sample or the method. In the supporting info, additional repeatability data is provided for samples with a higher level of cannabinoids. RSDs below the SMPR specification are achieved which adds more confidence to the overall method and may further suggest the prior repeatability outliers are due to sample inhomogeneity and not the method. Additional repeatability data is provided for CBDVA and CBGA and is on par with repeatability data previously shown for the minor cannabinoids. Reproducibility data is not provided as defined by the SMPR. Instead, intermediate precision was determined on 3 consecutive days. It is not specified, but the assumption is that this was performed by the same analyst on the same instrument. Intermediate precision showed similar % RSD when compared to Repeatability in most cases, but is likely not a sufficient replacement for Reproducibility data as defined in the SMPR. Given the nature of the analyte, “among-laboratory” data will be challenging prior to first action and intermediate precision may be considered acceptable especially if it represents multiple analysts and multiple instruments. *n.b. AOAC SMPR 2017.002 Tables 3&4 refer only to Table 2, the reviewer assumes these refer to both Tables 1&2.

method performs within the SMPR Method Performance REquirements table specifications for all analytes in the SMPR applicability statement? If not, please specify what is missing and whether or not the method's applicability should be modified.

IV. General Submission Package

IV. General Submission Package 1. Based on the supporting information, were there any additional steps in the evaluation of the method that indicated the need for any additional precautionary statements in the method?

No