Oregon Health Authority
Public Health Division - Chapter 333
Division 64
ACCREDITATION OF LABORATORIES
333-064-0100
Cannabis Sampling Procedures and Testing
(1) For purposes of this rule the definitions in OAR 333-007-0310 apply unless the context indicates otherwise.
(2) Sampling.
(a) A laboratory must have and follow marijuana item and industrial hemp-derived vapor items sampling policies and procedures, accredited by ORELAP, that:
(A) Ensure sampling will result in a sample that is representative of the batch being sampled.
(B) Require sampling and laboratory personnel to document and collect any information necessary for compliance with these rules, OAR chapter 333, division 7, and any applicable TNI standards.
(C) Require chain of custody procedures consistent with TNI EL Standard V1M2 5.7 and 5.8.
(D) Are appropriate to the matrix being sampled.
(E) Are consistent with OAR 333-007-0360 and 333-007-0370 and the following ORELAP sampling protocols approved by the accrediting body, incorporated by reference:
(i) Usable Marijuana: until July 1, 2022 ORELAP-SOP-001 Rev 4.0 and on or after July 1, 2022 ORELAP-SOP-001 Rev 4.1; and
(ii) Concentrates, Extracts, Products and Industrial Hemp-derived Vapor Items: ORELAP-SOP-002 Rev 4.3.
(F) Ensure that only the finished cannabinoid concentrate, extract, product or industrial hemp-derived vapor item is sampled if testing on the finished cannabinoid concentrate, extract, product or industrial hemp-derived vapor item is required under OAR 333-007-0330 and OAR 333-007-0340.
(G) Contain training and education requirements for sampling personnel.
(b) Sampling policies and procedures must be accredited by ORELAP prior to any marijuana or industrial hemp-derived vapor item samples being taken.
(c) Laboratory personnel that perform sampling must:
(A) Comply with the laboratory’s accredited sampling policies and procedures.
(B) After taking samples:
(i) Document the samples in accordance with subsection (2)(e) of this rule; and
(ii) If sampling for a licensee or a registrant required to comply with CTS tracking under ORS 475C.871, record the sampling and transfer information in the Commission’s seed to sale system, as required by the Authority and the Commission; and
(C) Take care while sampling to avoid contamination of the non-sampled material. Sample containers must be free of analytes of interest and appropriate for the analyses requested.
(D) Take sample increments that are representative of the batch being sampled.
(d) A sufficient sample size must be taken for analysis of all requested tests and the quality control performed by the testing laboratory for these tests.
(e) A laboratory must comply with any recording requirements for samples and sample increments in the accredited policies and procedures and at a minimum:
(A) Record the location of each sample and sample increment taken.
(B) Assign a field identification number for each sample, sample increment, duplicate sample, and replicate sample that have an unequivocal link to the laboratory analysis identification.
(C) Assign a unique identification number for the test batch in accordance with OAR 333-007-0370 and TNI EL standard requirements.
(D) Have a documented system for uniquely identifying the samples to be tested to ensure there can be no confusion regarding the identity of such samples at any time. This system must include identification for all samples, sample increments, preservations, sample containers, tests, and subsequent extracts or digestates.
(E) Place the laboratory identification code as a durable mark on each sample container.
(F) Enter a unique identification number into the laboratory records. This number must be the link that associates the sample with related laboratory activities such as sample preparation. In cases where the sample collector and analyst are the same individual, or the laboratory pre-assigns numbers to sample containers, the unique identification number may be the same as the field identification code.
(f) Combining sample increments.
(A) Sample increments collected from the same batch of usable marijuana shall be combined into a single sample by a laboratory prior to testing.
(B) Prior to testing, a laboratory shall combine sample increments from a batch of a cannabinoid concentrate, extract, finished inhalable cannabinoid product, or industrial hemp-derived vapor item;
(i) Increments from a primary sample are combined into a single sample.
(ii) Increments from a duplicate sample are combined into a single sample.
(iii) Increments from each replicate sample are combined with each other but material from separate replicate samples are not combined.
(C) Prior to any testing or subsampling except as described in subparagraph (i) of this paragraph, the entire combined sample must undergo the laboratory’s homogenization process.
(i) If the homogenization process would invalidate the analysis for a required test, the laboratory must utilize a subsampling procedure to withdraw a portion of the sample prior to homogenization for the required test. Testing that would be invalidated by the homogenization process includes but is not limited to, cryogenic sterilization of the sample prior to microbiological analysis.
(ii) Potency analysis shall not be performed on material subsampled prior to homogenization steps.
(D) Sample increments and samples collected from different batches may not be combined, except as permitted by OAR 333-007-0360 and on or after July 1, 2022 using the process described in ORELAP-SOP-001 Rev. 4.1.
(E) Portions of homogenized samples that are combined for testing as permitted by OAR 333-007-0360(1)(c) shall use the laboratory’s formal subsampling method to produce a proportionally representative sample from each batch involved.
(g) Sample replicate analysis for concentrates, extracts, finished inhalable cannabinoid products, and industrial hemp-derived vapor items.
(A) When replicate samples are required per OAR 333-007-0360 Exhibit B Table 7, each sample shall be analyzed individually for residual solvents as described in OAR 333-007-0410 and adult use cannabinoids and CBD as described in OAR 333-007-0430.
(B) Two samples shall be randomly selected according to the laboratory’s policy and procedures and analyzed individually for the remaining required analyses as described in OAR 333-007-0330, 333-007-0341, and 333-007-0342.
(C) Adult use cannabinoid and CBD results for the batch or process lot are reported as the calculated average result from all sample replicates.
(3) Compliance testing validity.
(a) When testing a sample for the required microbiological compliance tests as described in OAR 333-007-0390, a laboratory must comply with additional method validation as follows:
(A) Run a negative control in accordance with TNI Standard requirements to demonstrate the procedure is free of microbiological contaminants that prevent accurate testing.
(B) Run a positive control in accordance with TNI Standard requirements to demonstrate acceptable performance of the procedure. Acceptable performance of the positive control means accurate identification and quantitation of all regulated analytes.
(b) When testing a sample for the required chemistry compliance tests as described in OAR 333-007-0400 to 333-007-0415 and 333-007-0425 to 333-007-0430, a laboratory must comply with additional method validation as follows:
(A) Run a method blank in accordance with TNI Standard requirements to demonstrate the procedure is free of contaminants at or above the limit of quantitation.
(B) Run a laboratory control standard (LCS) in accordance with TNI Standard requirements to demonstrate acceptable performance of the procedure. Acceptable performance of the LCS means percent recovery for all regulated analytes are within the limits specified in Exhibit C, Table 1.
(C) Analyze duplicate samples with a precision limit of 10 percent RPD, if duplicates are required as specified in OAR 333-007-0360 and analyze all replicate samples with a precision limit of 10 percent RSD, if replicates are required as specified in OAR 333-007-0360
(4) Calculating total delta-9 THC and total CBD.
(a) Total delta-9 THC must be calculated as follows, where M is the mass or mass fraction of delta-9 THC or delta-9 THCA:
M total delta-9 THC = M delta-9 THC + 0.877 * M delta-9 THCA.
(b) Total CBD must be calculated as follows, where M is the mass or mass fraction of CBD and CBDA:
M total CBD = M CBD + 0.877 * M CBDA.
(c) Each test report must include the results for delta-8 THC, total delta-9 THC, and total CBD.
(5) Report delta-8 THC, total delta-9 THC, and total CBD for useable marijuana as Dry Weight. A laboratory must analyze the sample as received and report delta-8 THC, total delta-9 THC and total CBD content by dry weight calculated as follows:
P delta-8 THC(dry) = P delta-8 THC(wet) / [1-(P moisture/100)]
P total delta-9 THC(dry) = P total delta-9 THC(wet) / [1-(P moisture/100)]
P total CBD(dry) = P total CBD(wet) / [1-(P moisture/100)]
(6) Calculating RPD and RSD.
(a) A laboratory must use the following calculation for determining RPD:
Relative Percent Difference
%RPD=|(sample–duplicate)|/((sample+duplicate)/2) * 100
(b) A laboratory must use the following calculation for determining RSD:
Standard Deviation
S= √(∑((xi–x)^2)/(n–1))
Relative Standard Deviation
%RSD= (S/x)* 100
(c) For purposes of this section:
(A) S = standard deviation.
(B) n = total number of values.
(C) xi = each individual value used to calculate mean.
(D) x = mean of n values.
(d) For calculating both RPD and RSD if any results are less than the Limit of Quantitation (LOQ) the absolute value of the LOQ is used in the equation.
(e) The laboratory shall not substitute the LOQ for individual components of a totaled result, such as total delta-9 THC or total Hexanes, in the calculation of the totaled result for the purpose of calculating RPD or RSD.
(7) Tentative Identification of Unknown Compounds.
(a) If a laboratory is using a gas chromatography mass spectrometry instrument for analysis when testing cannabinoid concentrates, extracts, or industrial hemp-derived vapor items for solvents the laboratory shall have an established procedure for achieving tentative identification of unknown compounds in the sample. A tentatively identified compound (TIC) means an unknown chromatographic peak that is neither included in the list of analytes the laboratory is testing for nor expected to be naturally found in cannabis concentrates, extracts, or industrial hemp-derived vapor items such as terpenes.
(b) Tentative identification is achieved by searching NIST 2014 or an equivalent database (>250,000 compounds). Match scores for background subtracted or deconvoluted spectra should exceed 90 percent compared to the database library spectrum.
(c) Upon written request from the overseeing agency of the licensee or registrant, a laboratory shall report to the licensee or registrant and the Authority or the Commission all tentatively identified compounds (TICS) that meet the identification criteria in subsection (7)(b) of this rule.
(A) TIC quantitation is estimated by comparing analyte area to the closest internal standard area and assuming a response factor (RF) =1.
(B) If a laboratory does not use internal standards, TICs shall be reported as "detected" and apparent relative concentration shall be judged based on peak area.
(8) A laboratory must provide:
(a) Any pesticide test result to the Department of Agriculture upon that agency’s request.
(b) A sample or a portion of a sample to the Department of Agriculture upon that agency’s request, document the chain of custody from the laboratory to the Department, and document that the sample or portion of the sample was provided to the Department in the Commission’s seed to sale tracking system.
(9) A laboratory performing tests for a licensee or a registrant required to use CTS under ORS 475C.871 must enter any information required by the Commission or the Authority in CTS.
(10) A laboratory performing tests for a registrant must comply with the documentation requirements in OAR 333-007-0370 and must maintain the documentation required in these rules for at least three years and provide that information to the Authority upon request.
(11) The Authority may, in its discretion, deviate from TNI Standards in order to comply with OAR 333-007-0300 to 333-007-0500 and these rules based on the state’s needs.
(12) A laboratory must be able to demonstrate that its limit of quantitation (LOQ) for all matrices in compliance testing is:
(a) Less than or equal to one-half of any action level established in OAR 333-007-0400, 333-007-0410, 333-007-0415, and 333-007-0425 Exhibit A, Tables 3, 4, 8, and 9 except for as outlined in 333-064-0110(6); and
(b) For total delta-9 THC concentration less than or equal to 0.15 percent; and
(c) For delta-8 THC concentration less than or equal to 0.15 percent.
(13) Non-compliance testing. A laboratory that conducts a quality control or research and development test for a registrant or licensee may use methods not approved by the Authority but the laboratory may not identify those test results as accredited results.
[ED. NOTE: To view attachments referenced in rule text, click here for PDF copy.]
Statutory/Other Authority: ORS 438.605, 438.610, 438.615 & 438.620, 475C.544 & 475C.560
Statutes/Other Implemented: ORS 438.605, 438.610, 438.615 & 438.620, 475C.544 & 475C.560
History:
PH 24-2022, amend filed 03/15/2022, effective 03/31/2022
PH 95-2021, amend filed 12/29/2021, effective 01/01/2022
PH 89-2020, amend filed 12/30/2020, effective 01/01/2021
PH 85-2020, amend filed 12/23/2020, effective 01/01/2021
PH 43-2020, minor correction filed 05/07/2020, effective 05/07/2020
PH 282-2018, amend filed 12/20/2018, effective 01/01/2019
PH 9-2017, f. 5-26-17, cert. ef. 5-31-17
PH 38-2016(Temp), f. 12-13-16, cert. ef. 12-15-16 thru 5-30-17
PH 35-2016(Temp), f. & cert. ef. 12-2-16 thru 5-30-17
PH 21-2016, f. 6-24-16, cert. ef. 6-28-16
PH 22-2015(Temp), f. 11-13-15, cert. ef. 1-1-16 thru 6-28-16