Section 216-RICR-60-05-6.21 - Sample AnalysisA. General Requirements1. All cannabis product samples described in these regulations must be analyzed by analytical laboratories licensed by the RIDOH.2. Use only chemical standards manufactured by a provider acceptable to the Director to prepare calibration and quality control standards. Analytical laboratories must maintain standard preparation records and the certificates of analysis for all chemical standards, reference materials and reagents for at least five (5) years.3. Licensed analytical laboratories must demonstrate the ability to perform the quantitative analytical methods approved by RIDOH, and to provide defensible documentation and quality assurance.B. Approved Methods 1. Methods approved by RIDOH for the analysis of cannabinoids and contaminants in cannabis products are listed in Table 1. Equivalent test procedures may be followed if the laboratory has demonstrated the analysis is an acceptable alternative to normally used reference methods to the satisfaction of RIDOH.2. Table 1: List of Approved Methods for the Analysis of Cannabinoids and Contaminants. Analytical Component (where applicable, notes are listed in parenthesis, and described below in § 6.21(B)(3) of this Part) | Methodology (where applicable, notes are listed in parenthesis and described below in § 6.21(B)(3) of this Part) | Agency or Organization (see Definitions § 6.4 of this Part) Procedures (listed in parenthesis and described below in § 6.21(B)(3) of this Part) |
FDA | AOAC | AHP | USP | USDA | WHO |
Cannabinoids |
[DELTA]9-THC, [DELTA]8-THC THCa, CBD, CBDa (a) | LC-DAD (b) | (b) |
LC - MS, LC-MS/MS (b) | (b) |
Metals |
Arsenic--Total mg/L | Digestion followed by ICP/MS (c) | (f) | (g), (h) | (j) |
Digestion followed by ICP/AES or OES |
Cadmium--Total mg/L | Digestion followed by ICP/MS (c) | (f) | (g), (h) | (j) |
Digestion followed by ICP/AES or OES | (i) |
Lead--Total, mg/L | Digestion followed by ICP/MS (c) | (f) | (g), (h) | (j) |
Digestion followed by ICP/AES or OES | (i) |
Mercury - Total, mg/L | Digestion followed by ICP/MS (c) | (f) | (g), (h) | (j) |
Cold Vapor AA (c) | (e) |
Pesticides and Plant Growth Regulators |
Pesticides and Plant Growth Regulators - mg/L | QuEChERS, GC-MS/MS | (k) | (l), (m) | (o) |
QuEChERSLC-MS/MS | (k) | (l), (m) | (o) |
Water Activity |
Water Activity | Humidity Meter, Hygrodynamic Hygrometer | (q) |
Microbiological |
Total Viable Aerobic Bacteria | Culture and enumeration | (r) | (w), (x), (y) | (z) |
Total Yeast and Mold | Culture and enumeration | (s) | (w), (x), (y) | (z) |
Total Coliforms | Culture and enumeration | (t) |
Bile-tolerant Gram-negative Bacteria | Culture and enumeration | (w), (x) | (z) |
E. coli (pathogenic) | Culture | (u) | (z) |
Salmonella | Culture | (v) | (z) |
Residual Solvents |
Residual Solvents | Headspace GC/MS | (aa) |
a. Table 1 Key:(1) GC = Gas chromatography(2) MS = Mass spectrometry(3) LC = Liquid chromatography.3. Procedures and Notes for Table 1:a. Quantitative analysis including the percentage of [DELTA]9-tetrahydrocannnabinol ([DELTA]9-THC), [DELTA]8- tetrahydrocannnabinol ([DELTA]8-THC), cannabidiol (CBD), tetrahydrocannabinolic acid (THCa) and cannabidiolic acid (CBDa) of the total amount of THC. b. AHP. 2014. Cannabinoids by LC-Diode Array Detector, or modified to use LC-Mass Spectrometer instead of LC-DAD.c. A digestion procedure is required to solubilize analytes in suspended material and to break down organic-metal complexes for determination of total metals (which are equivalent to total recoverable metals).d. FDA Elemental Analysis Manual for Food and Related Products Section 4.5"Cold Vapor Atomic Absorption Spectrometric Determination of Total Mercury in Seafood Using Microwave Assisted Digestion."e. FDA Elemental Analysis Manual for Food and Related Products Section 4.7"Inductively Coupled Plasma-Mass Spectrometric Determination of Arsenic, Cadmium, Chromium, Lead, Mercury, and other Elements in Food Using Microwave Assisted Digestion."f. AOAC Official Method 2013.06 3- Arsenic, Cadmium, Mercury, and Lead in Foods - Pressure Digestion and Inductively Coupled Plasma-Mass Spectrometry (First Action 2013).g. AOAC Official Method 2015.01 4 - Heavy Metals in Food - Inductively Coupled Plasma-Mass Spectrometry (First Action 2015) h. Second Supplement to USP 35-NF 30 (Chapter 233) Elemental Impurities Proceduresi. FDA KAN-LAB-PES.053. Analysis of Pesticides and Industrial Chemicals by the QuEChERS Procedurej. AOAC Official Method 2007.01. Pesticide residues in foods by acetonitrile extraction and partitioning with Magnesium Sulfate.k. AOAC Official Method 2014.09. Determination and Confirmation of Residues of 653 Multiclass Pesticides and Chemical Pollutants in Teal. AOAC Official Method 998.01-2003 Synthetic pyrethroids in agricultural products.m. USDA NOP 2611. Instructions for Laboratory Selection Criteria for Pesticide Residue Testing n. EPA Index of Residue Analytical Methods (RAM)o. Official Methods of Analysis of the AOAC. 978.18. Water Activity: 16th Edition,1995p. FDA. 2001. Biological Analytical Manual. Chapter 3 Total Viable Aerobic Bacteria.q. FDA. 2015. Biological Analytical Manual. Chapter 18 Total Yeast and Mold.r. FDA. 2013. Biological Analytical Manual, Chapter 4 Enumeration of E. coli and Coliform.s. FDA. 2016. Biological Analytical Manual, Chapter 4A Diarrheagenic Escherichia coli.t. FDA. 2016. Biological Analytical Manual, Chapter 5 Salmonella.u. USP. 2008. "Microbiological Examination of Nonsterile Products: Microbial Enumeration Tests." USP 31, Chapter 61.v. USP. 2008. "Microbiological Examination of Nonsterile Products: Tests for specified Microorganisms." USP 31, Chapter 62.w. USP. Undated-b. "Articles of Botanical Origin." USP 36, Chapter 561.x. WHO 2007 guidelines for assessing quality of herbal medicines regarding contaminants and residues. Annex 5 y. USP. Chemical Tests. Chapter 467 Residual SolventsC. Cannabinoid Profile Analysis- Additional Information/Requirements 1. All finished cannabis plant components, extracts and concentrates must be quantitatively analyzed following methods described in § 6.21(B)(1) of this Part, to determine the total THC and its cannabinoid profile in the product. Although many cannabinoids and related compounds are present in the cannabis plant, characterization of the cannabinoid profile of the total THC in the cannabis product must include, at a minimum, the percentage of [DELTA]9-tetrahydrocannnabinol ([DELTA]9-THC), [DELTA]8-tetrahydrocannnabinol ([DELTA]8-THC), cannabidiol (CBD), tetrahydrocannabinolic acid (THCa) and cannabidiolic acid (CBDa). Percentage amounts of other cannabinoids may be reported, but are not required.D. Metals Analysis- Additional Information/Requirements1. Finished cannabis plant products must be tested for metals including arsenic, cadmium, lead, and mercury following methods described in § 6.21(B)(1) of this Part. Quantitative analyses of arsenic, cadmium, and lead, must be performed using, inductively coupled plasma - mass spectrometry (ICP-MS), optical emission spectrometry (ICP-OES or ICP-AES). The analysis of mercury must be performed using cold vapor atomic absorption analysis (CVAA) or by ICP-MS.2. The analytical limit for finished cannabis products including finished plant materials, resins, and concentrates is specified in § 6.21(D)(2)(a) of this Part (Table 2). a. Table 2: Analysis Requirements for Metals in Finished Cannabis Products for All Uses. Analytical results which exceed these upper limits must be reported with a qualifier indicating the contaminant measured in the cannabis product is above the concentration allowable for the intended use. Metal | All uses * Upper Limit (µg/kg) |
Arsenic (inorganic) | 200 |
Cadmium | 200 |
Lead | 500 |
Mercury | 100 |
* These limits apply to finished plant material, cannabis resin, cannabis concentrates intended for ingestion, inhalation or dermal application. These limits are based on inhalation limits described in USP<232> Elemental Impurities - Limits. |
E. Pesticides Residues Analysis- Additional Information/Requirements1. Analytical laboratories must quantitatively analyze production batches of finished plant material and extracts, resins, and concentrates for residues of prohibited pesticides following methods described in § 6.21(B)(1) of this Part. At a minimum, samples of finished plant material must be tested for the pesticides, including plant growth regulators listed in § 6.21(E)(1)(a) of this Part (Table 3), which includes the appropriate analytical methods for each of the listed pesticides. These pesticides were identified by AHP (2014) as commonly used in cannabis cultivation.a. Table 3: Maximum Allowable Limits for Residues of Pesticides and Plant Growth Regulators in Cannabis. Pesticide | CAS # | Action Limits (µg/g) |
Abamectin | 71751-41-2 | 0.05 |
Acephate | 30560-19-1 | 0.1 |
Acequinocy | 57960-19-7 | 0.1 |
Acetamiprid | 135410-20-7 | 0.1 |
Aldicarb | 116-06-3 | 0.1 |
Azoxystrobin | 131860-33-8 | 0.1 |
Acephate | 30560-19-1 | 0.1 |
Acequinocyl | 57960-19-7 | 0.1 |
Acetamiprid | 135410-20-7 | 0.1 |
Aldicarb | 116-06-3 | 0.1 |
Azoxystrobin | 131860-33-8 | 0.1 |
Bifenazate | 149877-41-8 | 0.1 |
Bifenthrin | 82657-04-3 | 0.2 |
Boscalid | 188425-85-6 | 0.1 |
Carbaryl | 63-25-2 | 0.2 |
Carbofuran | 1563-66-2 | 0.1 |
Chlorantraniliprole | 500008-45-7 | 0.2 |
Chlormequat chloride | 999-81-5 | 0.1 |
Chlorfenpyr | 122453-73-0 | 0.1 |
Chlorpyrifos | 2921-88-2 | 0.1 |
Clofentezine | 74115-24-5 | 0.1 |
Cyfluthrin | 6859-37-5 | 1 |
Cypermethrin | 52315-07-8 | 1 |
Daminozide | 1596-84-5 | 0.05 |
Dimethomorph | 110488-70-5 | 2 |
DDVP (Dichlorvos) | 62-73-7 | 0.05 |
Diazinon | 333-41-5 | 0.1 |
Dimethoate | 60-51-5 | 0.1 |
Ethoprophos | 13194-48-4 | 0.05 |
Etofenprox | 80844-07-1 | 0.1 |
Etoxazole | 153233-91-1 | 0.1 |
Fenoxycarb | 72490-01-8 | 0.05 |
Fenpyroximate | 134098-61-6 | 0.1 |
Fenhexamid | 126833-17-8 | 0.1 |
Fipronil | 120068-37-3 | 0.05 |
Flonicamid | 158062-67-0 | 0.1 |
Fludioxonil | 131341-86-1 | 0.1 |
Hexythiazox | 78587-05-0 | 0.1 |
Imazalil | 35554-44-0 | 0.05 |
Imidacloprid | 138261-41-3 | 0.1 |
Kresoxim"methyl | 143390-89-0 | 0.1 |
Malathion | 121-75-5 | 0.2 |
Metalaxyl | 57837-19-1 | 0.2 |
Methiocarb | 2032-65-7 | 0.1 |
Methomyl | 16752-77-5 | 0.4 |
Methyl parathion | 298-00-0 | 0.1 |
MGK-264 | 113-48-4 | 0.2 |
Myclobutanil | 88671-89-0 | 0.1 |
Naled | 300-76-5 | 0.1 |
Oxamyl | 23135-22-0 | 0.5 |
Paclobutrazol | 76738-62-0 | 0.1 |
PCNB | 82-68-8 | 0.1 |
Permethrin | 52645-53-1 | 0.1 |
Pendimethalin | 40487-42-1 | 0.1 |
Phosmet | 732-11-6 | 0.1 |
Piperonyl Butoxide | 51-03-6 | 0.5 |
Prallethrin | 23031-36-9 | 0.2 |
Propiconazole | 60207-90-1 | 0.4 |
Propoxur | 114-26-1 | 0.2 |
Pyrethrins | 8003-34-7 | 0.5 |
Pyridaben | 96489-71-3 | 0.1 |
Spinetoram | 187166-40-1 | 0.1 |
Spinosad | 168316-95-8 | 0.1 |
Spiromesifen | 283594-90-1 | 0.1 |
Spirotetramat | 20313-25-1 | 0.1 |
Spiroxamine | 118134-30-8 | 0.1 |
Tebuconazole | 107534-96-3 | 0.1 |
Trifloxystrobin | 141517-21-7 | 0.1 |
F. Water Activity Analysis- Additional Information/Requirements Finished cannabis plant material must be tested for water activity following methods described in § 6.21(B)(1) of this Part. See the definition of water activity in § 6.4 of this Part. The water activity upper limit for unbound water is equal to or less than 0.6 aW.
G. Microbiological Contaminants Analysis- Additional Information/Requirements 1. Finished cannabis plant products must be tested for microbiological contaminants following methods described in § 6.21(B)(1) of this Part. Methods used must be consistent with the following United States Pharmacopeia (USP) chapters:a. USP Chapter <61>: Microbiological Examination of Nonsterile Products: Microbial Enumeration Tests. USP 36, Chapter 6, and b. USP Chapter <62>: Microbiological Examination of Nonsterile Products: Tests for specified Microorganisms. USP 36, Chapter 622. Limits for microbiological contaminants are listed in § 6.21(G)(2)(a) of this Part (Table 4). a. Table 4: Upper Limits for Microbiological Contaminants. Cannabis Material | Total Viable Aerobic Bacteria (CFU)/g) | Total Yeast and Mold (CFU/g) | Total Coliforms (CFU/g) | Bile-tolerant Gram Negative Bacteria (CFU/g) | E. Coli (pathogenic strains) and Salmonella spp. |
Finished Plant Material | 100,000 | 10,000 | 1,000 | 1,000 | Not detected in 1 g of sample |
3. Notes for Table 4: a. Analytical limits are based on American Herbal Pharmacopoeia (AHP) (2014).b. CFU means colony forming unit.H. Residual Solvents Analysis- Additional Information/Requirements 1. Finished cannabis extracts, resins and concentrates must be tested for residual solvents when solvent has been used in the production process following methods described in § 6.21(B) of this Part.2. Analytical laboratories are required to test for the residual solvents listed in §6. 21(H)(3) of this Part (Table 5) unless it can document that no solvents were used in the cannabis oil production process.3. Table 5: A nalysis Re quirements for Residual Solvents Solvent | CAS # | Upper Limit (mg/kg)* | Solvent | CAS # | Upper Limit (mg/kg)* |
Acetone | 67-64-1 | 5,000 | Heptane | 142-82-5 | 5,000 |
Acetonitrile | 75-05-8 | 410 | Hexane | 110-54-3 | 290 |
Benzene** | 71-43-2 | 2 | Isobutane | 75-28-5 | 5,000 |
Butane | 106-97-8 | 5,000 | Isopropyl acetate | 108-21-4 | 5,000 |
1-Butanol | 71-36-3 | 5,000 | Methanol | 67-56-1 | 3,000 |
2-Butanol | 78-92-2 | 5,000 | Methylbutylketone | 591-78-6 | 50 |
2-Butanone | 78-93-3 | 5,000 | Methylcyclohexane | 108-87-2 | 1,180 |
Carbon tetrachloride ** | 56-23-5 | 4 | Methylethylketone | 78-93-3 | 5,000 |
Cumene | 98-82-8 | 70 | Methylisobutylketone | 108-10-1 | 5,000 |
Cyclohexane | 110-82-7 | 3,880 | Methylpropane | 75-28-5 | 5,000 |
1,2-Dichlorethane** | 107-06-2 | 5 | 2-Methyl-1-propanol | 78-83-1 | 5,000 |
1,1- Dichloroethene** | 75-35-4 | 8 | 2-Methylbutane | 78-78-4 | 5,000 |
1,2-Dichloroethene | 540-59-0 | 1,870 | 2-Methylpentane | 107-83-5 | 290 |
Dichloromethane | 75-09-2 | 600 | 3-Methylpentane | 96-14-0 | 290 |
1,2-Dimethoxyethane | 110-71-4 | 100 | N-Methylpyrrolidone | 872-50-4 | 530 |
1,2-Dimethylbenzene | 95-47-6 | 2,170 | Nitromethane | 75-52-5 | 50 |
1,3-Dimethylbenzene | 108-38-3 | 2,170 | Pentane | 109-66-0 | 5,000 |
1,4-Dimethylbenzene | 106-42-3 | 2,170 | 1-Pentanol | 71-41-0 | 5,000 |
2,2-Dimethylbutane | 75-83-2 | 290 | 1-Propanol | 71-23-8 | 5,000 |
2,3-Dimethylbutane | 79-29-8 | 290 | 2-Propanol | 67-63-0 | 5,000 |
N,N-Dimethylacetamide | 127-19-5 | 1,090 | Propane | 74-98-6 | 5,000 |
N,N-Dimethylformamide | 68-12-2 | 880 | Propyl acetate | 109-60-4 | 5,000 |
Dimethyl sulfoxide | 67-68-5 | 5,000 | Pyridine | 110-86-1 | 200 |
1,4-Dioxane | 123-91-1 | 380 | Sulfolane | 126-33-0 | 160 |
Ethanol | 64-17-5 | 5,000 | Tetrahydrofuran | 109-99-9 | 720 |
2-Ethoxyethanol | 110-80-5 | 160 | Tetralin | 119-64-2 | 100 |
Ethyl acetate | 141-78-6 | 5,000 | Toluene | 108-88-3 | 890 |
Ethylbenzene | 100-41-4 | 70 | 1,1,1-Trichloroethane ** | 71-55-6 | 1,500 |
Ethylene glycol | 107-21-1 | 620 | 1,1,2-Trichloroethylene | 79-01-6 | 80 |
Ethylene oxide | 75-21-80 | 50 | Xylene | 1330-20-7 | 2,170 |
Ethyl ether | 60-29-7 | 5,000 | 1,1,2-Trichloroethylene | 79-01-6 | 80 |
* See § 6.21(H)(4) of this Part for further information. |
** Class 1 solvents provided by USP Chapter <467> may not be used in the production of any cannabis product. |
4. The upper limits for residual solvents in Table 5 are given as milligrams of 17residual solvent per kilogram of cannabis oil. The upper limits in Table 5 are based on residual solvent standards provided by the USP Chapter <467>, the International Conference on Harmonization (ICH, 2011), and AHP (2014). a. Class 1 solvents may not be used in the production of any cannabis product.5. Analyses to determine residual solvent concentrations in cannabis products must be performed in accordance with the methods identified in USP Chapter <467>.216 R.I. Code R. 216-RICR-60-05-6.21
Amended effective 12/7/2023