AOAC CASP Cannabinoids ERP October Method Book

Quantitating Cannabinoids in Edible Chocolates

F.

Calculations a) Phytocannabinoid concentrations (% w/w) are calculated using the calibration parameters generated by the processing software with each sample batch analyzed. b) Sample and solvent masses are corrected as necessary. For example, the actual mass of sample or methanol used for extraction divided by the nominal amount – either 0.5 g of sample or 7.91 g for 10 mL methanol at 25 °C, respectively. c) Expected concentrations of cannabinoids and ibuprofen are outlined below (na – not applicable):

Sample type Phytocannabinoid (µg/mL) Ibuprofen (µg/mL) Unknown unknown 1 Method Blank na 1 ICS 5 5 RRS incurred + 1 2

G. Quality Control a) Calibration Check: A previous calibration function may be used provided a freshly prepared ICS meets accuracy specification of ±20% for all analytes. b) Calibration: If the calibration check does not meet specification, the detector response must be calibrated with a minimum of five calibration standards. The accuracy of each calibration point used for each analyte must be ±20% its expected value. c) Peak Detection: If a peak is identified by the data processing software, confirm its retention time by comparing samples to calibrators. d) Continuing Calibration Verification: Reinject one of the calibration standards at least once per sequence and then at a frequency of 5%. Recovery shall be between 80 - 120%. e) Method Blank: Analyze one per sample batch. Each analyte peak detected shall be below its corresponding Method Detection Limit (MDL). f) RRS: Analyze once per sample batch. A blank matrix is fortified at 1 μg/mL with all target analytes. Recovery shall be between 70 - 130%. Blank subtraction may be required depending on the incurred analytes in a given sample. g) RRS Duplicate: The RRS is always performed in duplicate. The relative percent difference (RPD; see below) of the RRS and RRS Duplicate must be < 30% for all target analytes. , % = 100 × | − |̅ , h) ICS: Analyze once per worksheet. Recovery must be between 70 and 130%. Must be prepared independently from calibration standards. i) Ibuprofen Check Standard Recovery: Recovery must be between 90 - 110% Ibuprofen (0.9 - 1.1 µg/mL in regular samples). H. Single-Laboratory Validation Study Design

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