4 Del. Admin. Code § 5001-11.0 - Testing and Sampling

11.1 Applicability

11.1.1 Prior to being transferred to a marijuana retail store, all marijuana and marijuana products must be tested by a marijuana testing facility licensed pursuant 4 Del.C. § 1333.

11.1.2 A marijuana establishment that intends to transfer marijuana or marijuana products to a marijuana retail store is responsible for ensuring every required test is conducted in accordance with this section prior to transfer to the marijuana retail store.

11.1.3 The Commissioner may temporarily waive testing requirements for any analyte under this section if it is determined that public health and safety is not at risk.

11.1.4 The Commissioner may require immediate mandatory compliance testing under this regulation, including for any other analyte suspected to be a health hazard or safety threat, to ensure public health and safety.

11.2 Mandatory compliance testing. Marijuana testing facilities must test samples of marijuana and marijuana products for the following:

11.2.1 For pre-rolls, shake, trim, kief, and all other forms of marijuana flower:

11.2.1.1 Cannabinoid profile, including:

11.2.1.1.1 Tetrahydrocannabivarin (THCV);

11.2.1.1.2 Cannabidiol (CBD);

11.2.1.1.3 Cannabichromene (CBC);

11.2.1.1.4 Delta 8 Tetrahydrocannabinol (8-THC);

11.2.1.1.5 Delta 9 Tetrahydrocannabinol (9-THC);

11.2.1.1.6 Cannabigerol (CBG); and

11.2.1.1.7 Cannabinol (CBN).

11.2.1.2 Foreign matter, including hair, insects, or similar adulterants.

11.2.1.3 Microbiological contaminants:

11.2.1.3.1 Aerobic bacterial;

11.2.1.3.2 Molds;

11.2.1.3.3 Yeast;

11.2.1.3.4 Coliform; and

11.2.1.3.5 Escherichia coli.

11.2.1.4 Heavy metals:

11.2.1.4.1 Lead;

11.2.1.4.2 Mercury;

11.2.1.4.3 Arsenic; and

11.2.1.4.4 Cadmium.

11.2.1.5 Terpenes

11.2.1.6 Pesticides

11.2.1.7 Total water activity

11.2.2 For marijuana concentrates, all testing requirements applicable to marijuana flower, as well as:

11.2.2.1 Butane;

11.2.2.2 Methanol;

11.2.2.3 Isopropanol;

11.2.2.4 Acetone;

11.2.2.5 1,1,1-Trichloroethane;

11.2.2.6 11,1-Dichloroethylene;

11.2.2.7 1,2-dichloroethane;

11.2.2.8 Carbon Tetrachloride;

11.2.2.9 Benzene;

11.2.2.10 Cyclohexane;

11.2.2.11 M-xylene;

11.2.2.12 Methylcyclohexane;

11.2.2.13 Trans-1,2-dichloroethylene;

11.2.2.14 Cis-1,2-dichloroethylene;

11.2.2.15 Toluene;

11.2.2.16 Tetrahydrofuran;

11.2.2.17 Methylene Chloride;

11.2.2.18 Acetonitrile;

11.2.2.19 1,4-Dioxane;

11.2.2.20 Ethylbenzene;

11.2.2.21 Chlorobenzene;

11.2.2.22 P-xylene;

11.2.2.23 Isopropyl benzene;

11.2.2.24 O-xylene;

11.2.2.25 Ethanol; and

11.2.2.26 Residual solvents.

11.2.3 For edible marijuana products, all testing requirements applicable to marijuana flower and marijuana concentrates, as well as validation of the stated cannabinoid content.

11.2.4 For inhalable or vaporizable marijuana products other than marijuana flower, all testing requirements applicable to marijuana flower and concentrates, as well as:

11.2.4.1 Medium-chain triglycerides (MCT);

11.2.4.2 Polyethylene glycol (PEG);

11.2.4.3 Vegetable glycerin (VG);

11.2.4.4 Vitamin E acetate;

11.2.4.5 Diacetyl; and

11.2.4.6 Squalene.

11.3 Testing failure thresholds. A sample of marijuana or marijuana products must be found to fail a laboratory test if it contains contaminants in quantities or concentrations as follows:

11.3.1 For foreign matter, including hair, insects, or similar adulterants, 1% or greater.

11.3.2 For microbiological contaminants:

11.3.2.1 Total Coliform, if detected;

11.3.2.2 Escherichia coli, if detected;

11.3.2.3 Molds; 400cfu/g or greater; and

11.3.2.4 Yeast, 400cfu/g or greater.

11.3.3 For heavy metals:

11.3.3.1 Lead, 0.5ppm or greater;

11.3.3.2 Mercury, 0.1ppm or greater;

11.3.3.3 Arsenic, 0.2ppm or greater; and

11.3.3.4 1 Cadmium, 0.2ppm or greater.

11.3.4 Pesticides, 10ppb or greater.

11.3.5 Residual solvents, if detected

11.3.6 For additional contaminants:

11.3.6.1 Butane, if detected;

11.3.6.2 Methanol, if detected;

11.3.6.3 Isopropanol, if detected;

11.3.6.4 Acetone, if detected;

11.3.6.5 1,1,1-Trichloroethane, if detected;

11.3.6.6 1,1-Dichloroethylene, if detected;

11.3.6.7 1,2-dichloroethane, if detected;

11.3.6.8 Carbon Tetrachloride, if detected;

11.3.6.9 Benzene, if detected;

11.3.6.10 Cyclohexane, if detected;

11.3.6.11 M-xylene, if detected;

11.3.6.12 Methylcyclohexane, if detected;

11.3.6.13 Trans-1,2-dichloroethylene, if detected;

11.3.6.14 Cis-1,2-dichloroethylene, if detected;

11.3.6.15 Toluene, if detected;

11.3.6.16 Tetrahydrofuran, if detected;

11.3.6.17 Methylene Chloride, if detected;

11.3.6.18 Acetonitrile, if detected;

11.3.6.19 1,4-Dioxane, if detected;

11.3.6.20 Ethylbenzene, if detected;

11.3.6.21 Chlorobenzene, if detected;

11.3.6.22 P-xylene, if detected;

11.3.6.23 Isopropyl benzene, if detected;

11.3.6.24 O-xylene, if detected; and

11.3.6.25 Ethanol, 10% concentration or greater.

11.4 Sample collection procedures

11.4.1 The Commissioner will publish a Best Practices Guide for Sample Collection. All marijuana establishments collecting samples for mandatory compliance testing must comply with the Best Practices Guide.

11.4.2 Marijuana establishments must coordinate with the Division for the collection of samples. The samples must be randomly selected by the marijuana establishment, under the supervision of the Division, for each given batch of marijuana and marijuana products.

11.4.2.1 In the case of emergency or extraordinary circumstances, the Commissioner may temporarily allow a marijuana establishment to self-sample and transport samples for mandatory compliance testing to a marijuana testing facility.

11.4.2.2 In the event the Commissioner temporarily waives these requirements, a marijuana establishment must select samples in plain view of video surveillance cameras and in accordance with the requirements of this regulation and the Best Practices Guide for Sample Collection.

11.4.3 Required sample sizes based upon matrix type and batch type are as follows:

11.4.3.1 Pre-rolls, shake, trim, kief, and all other forms of marijuana flower must be batch tested at approximately 0.25% of the batch weight, in accordance with TABLE 1 of this regulation.

11.4.3.1.1 Maximum flower batch weight is 10 pounds.

11.4.3.1.2 Minimum sample size is 3 grams.

11.4.3.1.3 Apportioned sample weights must be recorded on the manifest.

11.4.3.2 Marijuana concentrates must be batch tested at approximately .25% of the batch weight, in accordance with TABLE 1 of this regulation.

11.4.3.3 Marijuana product in individual retail units must be batch tested in accordance with TABLE 1 of this regulation.

TABLE 1: Example of Sample Size Based Upon Matrix Type and Batch Type:

Matrix Type	Batch Weight	Batch Units	Sample Amount [(Portion)]
Marijuana Flower	<= 5lbs		3 grams
	5.1lbs < w <= 10lbs		11 grams
Marijuana Concentrates	<= 1lbs		1.5 grams
	1.1bls < w <= 2lbs		2 grams
	2.1bls < w <= 3lbs		3 grams
	3.1bls < w <= 4lbs		4 grams
	4.1bls < w <= 5lbs		5 grams
Marijuana Products	-	1-250	1 unit
	-	251-500	2 units
	-	501-1,000	4 units
	-	1001-3,000	7 units
	-	3,001-10,000	11 units
	-	>10,001	16 units

11.4.4 All edible marijuana products must be packaged in accordance with subsection 9.3 of this regulation prior to sample collection. Depending on the number of units in the batch, at a minimum, 1 packaged unit for each edible marijuana product scheduled for testing, must be selected as a sample for mandatory compliance testing. The edible marijuana product will be collected in the final packaging for retail sale. The Commissioner shall require 1 unit sample for every product variety produced.

11.4.5 Marijuana establishments must ensure all samples for mandatory compliance testing and research and development purposes are packaged in accordance with Section 9.0 of this regulation.

11.4.6 Marijuana establishments must follow all tracking, transportation and record keeping requirements in accordance with Section 7.0 of this regulation.

11.5 Reporting requirements

11.5.1 For the purpose of testing, a marijuana testing facility must enter samples of marijuana and marijuana products, into the applicable laboratory section of the seed-to-sale tracking system.

11.5.2 The marijuana testing facility must enter mandatory compliance testing results into the seed-to-sale tracking system.

11.5.3 If a sample fails testing, the marijuana testing facility must report the failed test to both the Commissioner and the marijuana establishment that submitted the sample within 48 hours. The marijuana establishment that submitted the sample may retest or remediate and retest the batch in accordance with subsection 11.6 of this regulation.

11.5.4 If a sample passes testing, the marijuana testing facility must enter "pass" into the inventory seed-to-sale tracking system for the batch from which the sample came. The batch is then released for transfer to a marijuana retail store.

11.5.5 The marijuana testing facility is not required to report to the Commissioner the results of any tests if the requester notifies the marijuana testing facility in advance of transferring the sample of marijuana or marijuana product that the testing is for research development purposes and agrees not to use the results to satisfy any mandatory compliance testing requirements.

11.6 Retesting and remediation of failed marijuana or marijuana products

11.6.1 Batches of marijuana and marijuana products that have failed testing in accordance with subsection 11.3 of this regulation may be retested with or without remediation.

11.6.2 Edible marijuana products that fail initial testing may be re-tested 1 time. Any edible marijuana products that fail twice must be destroyed in accordance with Section 12.0 of this regulation.

11.6.3 A marijuana establishment seeking retesting of a batch that failed mandatory compliance testing without remediation must submit 2 samples from the batch that failed to the same marijuana testing facility that issued the initial failed test result.

11.6.3.1 Both samples submitted for retesting must pass all required testing required for any analyte that failed initial mandatory testing.

11.6.3.2 If either sample submitted for retesting fails any required test for any analyte that failed initial mandatory compliance testing, a batch of marijuana flower or trim may be transferred to a licensed marijuana manufacturing facility for extraction following a failed retest and subsequently tested in accordance with this regulation.

11.6.3.3 If either sample submitted for retesting fails any required test for any analyte that failed initial mandatory testing, the batch of marijuana concentrates, or marijuana products may not be remediated or retested and must be destroyed.

11.6.4 For marijuana establishments seeking retesting of a batch of marijuana or marijuana products that failed mandatory testing without remediation, the Division must submit the new samples from the batch that failed mandatory testing to the same marijuana testing facility that issued the initial failed test result.

11.6.5 A marijuana establishment may attempt to remediate any batch that fails mandatory testing, except for batches that fail due to pesticide contamination.

11.6.5.1 If a failed batch is remediated using a remediation method that does not change the marijuana or marijuana product into a different matrix of marijuana or marijuana product, then the marijuana establishment must submit 2 samples from the remediated batch to the same marijuana testing facility that issued the initial failed test result.

11.6.5.1.1 Both samples submitted for retesting must pass all required testing required for any analyte category that failed initial mandatory testing.

11.6.5.1.2 If either sample submitted for retesting fails any required test for any analyte category that failed initial mandatory testing, the batch of marijuana or marijuana products may be remediated in accordance with this section or destroyed.

11.6.5.2 If a failed batch is remediated using a remediation method that changes the marijuana or marijuana product into a different matrix of marijuana or marijuana product, then the marijuana establishment must submit 1 sample from the remediated batch to the marijuana testing facility that issued the initial failed test result.

11.6.5.2.1 The sample from the remediated batch must pass all mandatory testing required for the marijuana or marijuana product in the matrix it is in after remediation, including any tests previously passed, if applicable.

11.6.5.2.2 If the remediated batch, that is in a new matrix, fails mandatory compliance testing, the failed test is treated as an original failed mandatory compliance test and the remediated batch may be retested or remediated in accordance with this section.

11.6.6 If extraction is the remediation method and the marijuana or marijuana product must be transferred to a marijuana manufacturing facility, the licensed marijuana cultivation facility must first contact the Commissioner for approval.

11.6.7 Batches of marijuana flower or trim that have failed mandatory testing may not be remediated in a manner that involves the combination of the batch that failed testing with a batch, or batches, of marijuana flower or trim that has not been tested or that has passed testing.

11.6.8 Any retests of marijuana or marijuana products that failed initial testing are subject to the same testing requirements of the initial sample, except for heavy metals, if heavy metal testing passed in initial testing.

11.6.9 Any batches of marijuana and marijuana products that have failed initial testing where no remediation method is available must be destroyed in accordance with Section 12.0 of this regulation.

11.6.10 A marijuana establishment that remediates any failed batch must appropriately record all remediation steps and processes in the seed-to-sale tracking system. Approved remediation processes include pascalization, ozone, non-ionizing radiation, and ionizing radiation. Marijuana products exposed to ionizing radiation must identify the exposure on package label in accordance with subsection 9.2 of this regulation.

11.6.11 A marijuana establishment must act to retest, remediate, or destroy a batch of marijuana or marijuana products within 30 days of receiving notice from the marijuana testing facility of the initial failed test result. If the marijuana establishment does not record an action on the failed batch within 30 days, the Commissioner may order destruction.

11.7 Testing for research and development purposes

11.7.1 Any marijuana establishment may submit samples of marijuana and marijuana products for research and development testing. Testing under this subsection does not have to comply with the mandatory compliance testing requirements of this regulation. Any sample transferred to a marijuana testing facility for testing purposes must be deemed a sample for research and development purposes prior to being transferred.

11.7.2 All samples for research and development testing must be transferred to a marijuana testing facility in accordance with Section 7.0 of this regulation.

11.7.3 The test results for the research and development sample may only be entered into the notes for a particular plant, batch, or barcodes within the seed-to-sale tracking system.

11.8 Test categories for marijuana and marijuana products

11.8.1 This subsection adopts and incorporates the following guidance on incorporated materials:

11.8.1.1 The Codex Alimentarius Commission, "General Guidelines on Sampling" CAC/GL50-2004 not including any further editions or amendments thereof and only to the extent that the provisions therein are not inconsistent with this regulation;

11.8.1.2 The Association of American Feed Control Officials (AAFCO) "Guidance on Obtaining Defensible Samples" or "GOODS" (2015) by reference, not including any further editions or amendments thereof and only to the extent that the provisions therein are not inconsistent with this regulation; and

11.8.1.3 The U.S. Department of Agriculture, National Organic Program, "National Organic Program Handbook: Guidance and Instructions for Accredited Certifying Agents and Certified Operations" (2014), not including any further editions or amendments thereof and only to the extent that the provisions therein are not inconsistent with this regulation.

11.8.2 Marijuana testing facilities may be approved to conduct testing as follows:

11.8.2.1 For pre-rolls, shake, trim, kief, and all other forms of marijuana flower:

11.8.2.1.1 Cannabinoid potency. A quantitative analysis including the amounts of cannabinoids present in accordance with subsection 11.2 of this regulation, expressed as a percentage of total cannabinoids present. Amounts of other cannabinoids may be reported but are not required;

11.8.2.1.2 Foreign matter. A quantitative analysis including the total amount of hair, insects, or similar adulterants present in accordance with this regulation;

11.8.2.1.3 Microbiological. A quantitative analysis including the total viable aerobic bacteria and total coliform present in accordance with this regulation;

11.8.2.1.4 Total water activity;

11.8.2.1.5 Pesticides. A quantitative analysis including the presence and amounts of residues of any pesticides or growth regulators in accordance with this regulation;

11.8.2.1.6 Metals. A quantitative analysis of the amounts of heavy metals present in accordance with this regulation; and

11.8.2.1.7 Residual solvents. A quantitative analysis of the presence and amounts of residual solvents in accordance with this regulation.

11.8.2.2 For marijuana concentrates, the same test categories as marijuana flower, as well as a quantitative analysis including the presence and amounts of any additional contaminants specified in subsection 11.2.2 of this regulation.

11.8.2.3 For edible marijuana products, the same test categories as marijuana flower and marijuana concentrates, as well as:

11.8.2.3.1 An analysis of the product's package to ensure it meets the requirements in Section 9.0 of this regulation; and

11.8.2.3.2 A quantitative analysis that validates the cannabinoid content stated on the product.

11.9 Sampling requirements

11.9.1 Marijuana testing facilities receiving samples from the Division must complete the chain of custody forms to record receiving and internal tracking of samples, including the following information:

11.9.1.1 The laboratory internal tracking number or other identification;

11.9.1.2 Printed name and signature of the person receiving the samples;

11.9.1.3 Date and time of sample receipt;

11.9.1.4 Condition of sample upon receipt;

11.9.1.5 Type of tests requested;

11.9.1.6 The name, address, and license number of the marijuana testing facility to which samples are forwarded for procedures not performed on the premises, each of which must be numbered or otherwise appropriately identified;

11.9.1.7 Sample tracking through each stage of storage, analysis, and disposal;

11.9.1.8 Date laboratory tests are performed;

11.9.1.9 The marijuana testing facility test results;

11.9.1.10 Date of reporting;

11.9.1.11 Sample test reports; and

11.9.1.12 The records of samples must contain the completed chain of custody forms and original completed sample collection forms.

11.9.2 Sample preparation. Each marijuana testing facility must adhere to the following:

11.9.2.1 Marijuana testing facilities must have a designated area of the facility dedicated to preparing marijuana and marijuana product samples for analysis. Sample preparation areas must be equipped with the supplies and equipment to properly handle samples during preparation, including:

11.9.2.1.1 Disposable gloves;

11.9.2.1.2 Decontaminated tools such as disposable pipettes and plastic or stainless-steel spatulas, knives, and sampling spears;

11.9.2.1.3 Decontaminated stainless-steel bowls and implements to homogenize the product by stirring, chopping, or grinding;

11.9.2.1.4 Clean, decontaminated surfaces for sample processing;

11.9.2.1.5 Decontaminated sample containers appropriate for the analyses required;

11.9.2.1.6 Container labels and pens with indelible ink; and

11.9.2.1.7 Supplies to thoroughly clean, decontaminate, and dry sample preparation equipment between samples.

11.9.2.2 Marijuana testing facilities must adhere to the following procedures when preparing each sample type:

11.9.2.2.1 Personnel handling samples must wear disposable gloves to avoid contamination and should not wear creams or perfumes.

11.9.2.2.2 Sample preparation area must be clean and decontaminated and tools and equipment laid out.

11.9.2.2.3 The sample must be placed in the stainless-steel bowl or on a decontaminated cutting surface for homogenizing the sample using either the sample collection tool or separate clean, decontaminated implement.

11.9.2.2.4 The sample must be prepared for analysis using an appropriate decontaminated tool. The sample should not be touched with bare hands or allowed to touch anything that might cause cross contamination.

11.9.2.2.5 Any tools or equipment that come in contact with the finished plant material or other marijuana or marijuana products must be cleaned before preparing the next sample.

11.9.2.2.6 All samples must be placed in clean, airtight sample containers that are large enough to hold the prescribed sample quantity with minimal headspace. Sample containers must be closed and labeled.

11.9.2.2.7 Samples must be refrigerated between 2-6º C to preserve the chemical and biological composition of the samples.

11.9.2.2.8 Ensure samples of marijuana and marijuana products are homogenous with respect to distribution of cannabinoids or contaminants.

11.9.2.2.9 Samples must be thoroughly stirred or mixed before quantitatively measuring for analysis. Solid and semi-solid products must be ground and thoroughly mixed. Grinding devices that minimize loss (e.g., leaching of resins) must be used and thoroughly cleaned after each use.

11.9.2.2.10 For marijuana and marijuana products that are distributed in a ground form, the product batch sample must be quartered. Quartering involves heaping the ground product, dividing the heap into 4 equal quarters, and selecting samples from 2 of the quarters, which are then combined and mixed. The remaining quarters may then be combined and mixed and used for microbiological and contaminant testing.

11.9.2.2.11 Resin and other solids may not be melted as a means of homogenization. Heating the product may alter the cannabinoid profile or contamination levels thereby rendering the sample unrepresentative of the source product.

11.9.2.2.12 Laboratory samples of edible marijuana products must be homogenized prior to testing so that the sample is representative of the finished product batch. Mix or quarter homogenized samples as described in subsection 11.9.2.2.10 of this regulation. If individually packaged edible marijuana products are sampled from a production batch, multiple packaged products should be combined and prepared so that the distribution of cannabinoids or contaminants is representative of the production batch.

11.9.2.2.13 When subsamples are required, subsamples must be composited and mixed to obtain a quantity sufficient for evaluation. The quantity sufficient for evaluation may vary by analytical method and laboratory-specific procedures, therefore the marijuana testing facility must define the minimum sample quantity required for evaluation.

11.9.2.2.14 Compositing subsamples may be impractical for some product types (e.g., hard "candies" or other products in discrete solid units). In these cases, individual product units must be collected by the marijuana testing facility as samples for analysis. In some cases, the marijuana testing facility may combine extracts or digestates prepared from the solid subsamples and analyze the volumetrically combined extract/digestate as a composite.

11.9.3 Sample analysis. All marijuana and marijuana product samples described in this regulation must be analyzed by marijuana testing facilities licensed by the Commissioner. Each marijuana testing facility must:

11.9.3.1 Use only chemical standards manufactured by a provider acceptable to the Commissioner to prepare calibration and quality control standards;

11.9.3.2 Maintain standard preparation records and the certificates of analysis for all chemical standards, reference materials and reagents for at least 5 years; and

11.9.3.3 Demonstrate the ability to perform the quantitative analytical methods approved by the Commissioner, and to provide defensible documentation and quality assurance.

11.10 Approved methods and technical requirements for testing

11.10.1 Approved methods. Methods approved by the Commissioner for the analysis of cannabinoids and contaminants in marijuana and marijuana products are listed in Table 2. Equivalent test procedures may be followed if the marijuana testing facility has demonstrated the analysis is an acceptable alternative to normally used reference methods to the satisfaction of the Commissioner.

TABLE 2: List of Approved Methods for the Analysis of Cannabinoids and Contaminants

Analytical Component	Methodology
[DELTA]9-THC, [DELTA]8-THC, THCA, CBD, CBDA	LC-DAD
CBC, CBCA, CBG, CBGA, CBN, CBNA	LC - MS, LC-MS/MS
	GC/ FID
Arsenic-Total mg/L	Digestion followed by ICP/MS
Cadmium-Total mg/L	Digestion followed by ICP/MS
	Digestion followed by Flame AA
	Digestion followed by Graphite Furnace
Lead-Total, mg/L	Digestion followed by ICP/MS
	Digestion followed by Flame AA
	Digestion followed by Graphite Furnace
Mercury-Total, mg/L	Digestion followed by ICP/MS
	Cold Vapor AA
Pesticides and Plant Growth Regulators - mg/L	QuEChERS, GC-MS, GC-MS/MS
	QuEChERS,LC-MS, LC- MS/MS
	QuEChERS GC-ECD, GC-NPD, LC-FLD
Water Activity	Humidity Meter, Hygrodynamic Hygrometer
Total Viable Aerobic Bacteria	Culture and enumeration
Total Yeast and Mold	Culture and enumeration
Total Coliforms	Culture and enumeration
Residual Solvents	Headspace GC/FID

11.10.1.1 Table 2 Key:

11.10.1.1.1 AA = Atomic absorption

11.10.1.1.2 DAD = Photodiode-array detection

11.10.1.1.3 ECD = Electron capture detector

11.10.1.1.4 FLD = Fluorescence detector

11.10.1.1.5 FID = Flame ionization detector

11.10.1.1.6 GC = Gas chromatography

11.10.1.1.7 ICP = Inductively coupled plasma

11.10.1.1.8 LC = Liquid chromatography

11.10.1.1.9 MS = Mass spectrometry

11.10.1.1.10 NPD = Nitrogen phosphorous detector

11.10.1.1.11 QuEChERS = Quick, easy, cheap, rugged, and safe

11.10.1.2 Procedures and notes for Table 2:

11.10.1.2.1 A quantitative analysis must include the amounts of cannabinoids present in accordance with subsection 11.2 of this regulation, expressed as a percentage of total cannabinoids present. Amounts of other cannabinoids may be reported but are not required.

11.10.1.2.2 AHP. 2014. Cannabinoids by LC-Diode Array Detector, GC-Flame Ionization Detector or modified to use LC-Mass Spectrometer instead of LC-DAD. If GC/FID option is used, samples must be derivatized prior to analysis due to decarboxylation and degradation of the delta-9-THC

11.10.1.2.3 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)

11.10.1.2.4 FDA Elemental Analysis Manual for Food and Related Products Section 4.3 "Graphite Furnace Atomic Absorption Spectrometric Determination of Cadmium and Lead in Food Using Microwave Assisted Digestion"

11.10.1.2.5 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"

11.10.1.2.6 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"

11.10.1.2.7 AOAC Official Method 2013.06 3- Arsenic, Cadmium, Mercury, and Lead in Foods - Pressure Digestion and Inductively Coupled Plasma-Mass Spectrometry (First Action 2013)

11.10.1.2.8 AOAC Official Method 2015.01 4- Heavy Metals in Food - Inductively Coupled Plasma-Mass Spectrometry (First Action 2015)

11.10.1.2.9 AOAC Official Method 999.1 Pb, Cd, Zn Cu, and Fe in Foods Atomic Absorption Spectrophotometry after Microwave Digestion (First Action 1999, Second Action 2005)

11.10.1.2.10 Second Supplement to USP 35-NF 30 (Chapter 233) Elemental Impurities Procedures

11.10.1.2.11 FDA KAN-LAB-PES.053. Analysis of Pesticides and Industrial Chemicals by the QuEChERS Procedure

11.10.1.2.12 AOAC Official Method 2007.01. Pesticide residues in foods by acetonitrile extraction and partitioning with Magnesium Sulfate

11.10.1.2.13 AOAC Official Method 2014.09. Determination and Confirmation of Residues of 653 Multiclass Pesticides and Chemical Pollutants in Tea

11.10.1.2.14 AOAC Official Method 998.01-2003 Synthetic pyrethroids in agricultural products.

11.10.1.2.15 USDA NOP 2611. Instructions for Laboratory Selection Criteria for Pesticide Residue Testing

11.10.1.2.16 EPA Index of Residue Analytical Methods (RAM)

11.10.1.2.17 Official Methods of Analysis of the AOAC. 978.18. Water Activity: 16th Edition,1995

11.10.1.2.18 FDA. 2001. Biological Analytical Manual. Chapter 3 Total Viable Aerobic Bacteria

11.10.1.2.19 FDA. 2015. Biological Analytical Manual. Chapter 18 Total Yeast and Mold

11.10.1.2.20 FDA. 2013. Biological Analytical Manual, Chapter 4 Enumeration of Escherichia coli and Coliform

11.10.1.2.21 FDA. 2016. Biological Analytical Manual, Chapter 4A Diarrheagenic Escherichia coli

11.10.1.2.22 FDA. 2016. Biological Analytical Manual, Chapter 5 Salmonella

11.10.1.2.23 USP. 2008. "Microbiological Examination of Nonsterile Products: Microbial Enumeration Tests." USP 31, Chapter 61

11.10.1.2.24 USP. 2008. "Microbiological Examination of Nonsterile Products: Tests for specified Microorganisms." USP 31, Chapter 62

11.10.1.2.25 USP. Undated-b. "Articles of Botanical Origin." USP 36, chapter 561

11.10.1.2.26 WHO 2007 guidelines for assessing quality of herbal medicines regarding contaminants and residues. Annex 5

11.10.1.2.27 1 USP. Chemical Tests. Chapter 467 Residual Solvents

11.10.2 Cannabinoid profile analysis additional information and requirements. All marijuana and marijuana products must be quantitatively analyzed following methods described in this regulation, to determine the total THC and its cannabinoid profile in the product. Although many cannabinoids and related compounds are present in the marijuana plant, characterization of the cannabinoid profile of the total THC in the marijuana product must include, at a minimum, the amounts of cannabinoids present in accordance with subsection 11.2.1.1 of this regulation, expressed as a percentage of total cannabinoids present. Amounts of other cannabinoids may be reported but are not required.

11.10.3 Heavy metal analysis additional information and requirements. Marijuana and marijuana products must be tested for metals including arsenic, cadmium, lead, and mercury following methods described in this regulation. Quantitative analyses of arsenic, cadmium, and lead must be performed using atomic absorption spectrometry, inductively coupled plasma-optical emission spectrometry (ICP-OES) or ICP-mass spectrometry (ICP-MS). The analysis of mercury must be performed using cold vapor atomic absorption analysis (CVAA) or by ICP-MS. Analytical results which exceed these upper limits shall be reported with a qualifier indicating the contaminant measured in the marijuana or marijuana product is above the concentration allowable for the intended use. The analytical limit for marijuana products including marijuana and marijuana concentrates is specified in Table 3.

TABLE 3: Analysis Requirements for Metals in Marijuana and Marijuana Products for All Uses.

METAL	ALL USES* Upper Limit (ppm)	MARIJUANA-INFUSED PRODUCTS ONLY Upper Limit (ppm)
Arsenic (inorganic)	<0.2	<0.2
Cadmium	<0.2	<0.2
Lead	<0.5	<0.5
Mercury	<0.1	<0.1
* These limits apply to finished marijuana plant material, marijuana resin, and marijuana concentrates intended for ingestion, inhalation, or dermal application. These limits are based on inhalation limits described in USP<232> Elemental Impurities-Limits.

11.10.4 Pesticides residues analysis additional information and requirements. Marijuana testing facilities must conduct a quantitative analysis including the presence and amounts of residues of any pesticides or growth regulators in accordance with subsection 11.10.4 of this regulation. At a minimum, samples of marijuana or marijuana products must be tested for the pesticides, including plant growth regulators, included in Table 4 of this regulation, which includes the appropriate analytical methods for each of the listed pesticides. These pesticides were identified by AHP (2014) as commonly used in marijuana cultivation.

TABLE 4: Minimum Analysis Requirements for Residues of Pesticides and Plant Growth Regulators:

PESTICIDE	CAS #	USE	RESIDUE ANALYTICAL METHODS
Abamectin (Avermectins B1a and B1b)	71751-41-2	Insecticide/acaricide	LC-FLD; LC-MS/MS
Acequinocyl	57960-19-7	Insecticide/acaricide	LC/MS/MS
Bifenazate	149877-41-8	Acaricide	LC; LC-MS/MS
Bifenthrin (synthetic pyrethroid)	82657-04-3	Insecticide	GC-ECD; GC-MS/MS LC- MS/MS
Chlormequat chloride	7003-89-6	Plant growth regulator	IC, LC-MS/MS
Cyfluthrin (synthetic pyrethroid)	6859-37-5	Insecticide	LC; GC-MS/MS; LC-MS/MS
Daminozide (Alar)	1596-84-5	Plant growth regulator	LC/UV; LC-MS/MS
Etoxazole	153233-91-1	Acaricide	GC-MS(/MS); LC-MS/MS
Fenoxycarb	72490-01-8	Insecticide	LCUV; LC-MS/MS
Imazalil	35554-44-0	Fungicide	GC-ECD; LC-MS/MS
Imidacloprid	138261-41-3	Insecticide	LC-MS/MS
Myclobutanil	88671-89-0	Fungicide	GC-ECD; GC-NPD; GSMS/MS; LC-MS/MS
Paclobutrazol	76738-62-0	Plant growth regulator; fungicide	LC-MS/MS
Spinosad	168316-95-8	Insecticide	LC-MS/MS
Spiromesifen	283594-90-1	Insecticide	GC-MS; LC-MS/MS
Spirotetramat	20313-25-1	Insecticide	LC/LC-MS/MS
Trifloxystrobin	141517-21-7	Fungicide	GC-NPD; GC-MS/MS; LCMS/MS
Acequinocyl	57960-19-7	Insecticide/acaricide	LC/MS/MS
Bifenazate	149877-41-8	Acaricide	LC; LC-MS/MS
Bifenthrin (synthetic pyrethroid)	82657-04-3	Insecticide	GC-ECD; GC-MS/MS LC- MS/MS
Chlormequat chloride	7003-89-6	Plant growth regulator	IC, LC-MS/MS
Cyfluthrin (synthetic pyrethroid)	6859-37-5	Insecticide	LC; GC-MS/MS; LC-MS/MS
Daminozide (Alar)	1596-84-5	Plant growth regulator	LC/UV; LC-MS/MS
Etoxazole	153233-91-1	Acaricide	GC-MS(/MS); LC-MS/MS
Fenoxycarb	72490-01-8	Insecticide	LC/UV; LC-MS/MS
Imazalil	35554-44-0	Fungicide	GC-ECD; LC-MS/MS
Imidacloprid	138261-41-3	Insecticide	LC-MS/MS
Myclobutanil	88671-89-0	Fungicide	GC-ECD; GC-NPD; GSMS/MS; LC-MS/MS
Paclobutrazol	76738-62-0	Plant growth regulator; fungicide	LC-MS/MS
Spinosad	168316-95-8	Insecticide	LC-MS/MS
Spiromesifen	283594-90-	Insecticide	GC-MS; LC-MS/MS
Spirotetramat	20313-25-1	Insecticide	LC/LC-MS/MS
Trifloxystrobin	141517-21-7	Fungicide	GC-NPD; GC-MS/MS; LCMS/MS

11.10.4.1 Table 4 Key:

11.10.4.1.1 ECD = Electron capture detector

11.10.4.1.2 FLD = Fluorescence detector

11.10.4.1.3 GC = Gas chromatography

11.10.4.1.4 MS = Mass spectrometry

11.10.4.1.5 NPD = Nitrogen phosphorous detector

11.10.4.1.6 LC = Liquid chromatography

11.10.4.2 Marijuana testing facilities must analyze pesticides in addition to those in Table 4 based on the approach that USDA uses to analyze 195 prohibited pesticides it has targeted in organic food. With the understanding that no single analytical method currently exists to analyze all 195 prohibited pesticides, marijuana testing facilities conducting marijuana testing in Delaware must analyze as many compounds on the USDA target analyte list for organic food as possible. Analytical laboratories must follow procedures listed in this regulation or their equivalents.

11.10.4.3 The upper limit for pesticides and plant growth regulators is less than or equal to 10 parts per billion (ppb).

11.10.4.4 A marijuana testing facility that is unable to perform the required testing of pesticide residues at or below the 10 parts per billion (ppb) criteria may determine compliance by ensuring that any pesticide residues are present at a level less than or equal to 5% of the US EPA tolerance for the specific residue. EPA pesticide tolerances are available from Title 40 of the Code of Federal Regulations (C.F.R.). In these circumstances, the Commissioner must be notified regarding the specific pesticides to which this method is being applied.

11.10.5 Water activity analysis additional information and requirements. Pre-rolls, shake, trim, kief, and all other forms of marijuana flower shall be tested for water activity following methods described in this regulation. The water activity upper limit for unbound water is equal to or less than 0.6aW.

11.10.6 Microbiological contaminants analysis additional information and requirements. Marijuana flower, pre-rolls, shake, trim, kief, and all other forms of raw marijuana must be tested for microbiological contaminants following methods described in this regulation. Methods used must be consistent with the following United States Pharmacopeia Chapters: USP Chapter <61>: Microbiological Examination of Non-sterile Products: Microbial Enumeration Tests. USP 36, Chapter 6 and USP Chapter <62>: Microbiological Examination of Non-sterile Products: Tests for specified Microorganisms. USP 36, Chapter 62. Limits for microbiological contaminants are listed in Table 5.

TABLE 5: Upper Limits for Microbiological Contaminants

MARIJUANA MATERIAL	TOTAL VIABLE AEROBIC BACTERIA (CFU*/g)	TOTAL YEAST AND MOLD (CFU/g)	TOTAL COLIFORMS [AND Escherichia coli] (CFU/g)
Finished plant material	400 CFU/g	400 CFU/g	IF DETECTED]
* CFU means colony forming unit.

11.10.7 Residual solvent analysis additional information and requirements. Marijuana concentrates must be tested for residual solvents when solvents have been used in the production process following methods described in this regulation. Marijuana testing facilities are required to test for the residual solvents listed in Table 6 of this regulation, unless it can document that no solvents were used in the marijuana concentrate production process:

TABLE 6: Analysis Requirements for Residual Solvents

SOLVENT	CAS #	UPPER LIMIT (mg/kg)*	SOLVENT	CAS #	UPPER LIMIT (mg/kg)*
Acetone	67-64-1	5000	Heptane	142-82-5	5000
Acetonitrile	75-05-8	410	Hexane	110-54-3	290
Benzene **	71-43-2	2	Isobutane	75-28-5	5000
Butane	106-97-8	5000	Isopropyl acetate	108-21-4	5000
1-Butanol	71-36-3	5000	Methanol	67-56-1	3000
2-Butanol	78-92-2	5000	Methylbutylketone	591-78-6	50
2-Butanone	78-93-3	5000	Methylcyclohexane	108-87-2	1180
Carbon tetrachloride**	56-23-5	4	Methylethylketone	78-93-3	5000
Cumene	98-82-8	70	Methylisobutylketone	108-10-1	5000
Cyclohexane	110-82-7	3880	Methylpropane	75-28-5	5000
1,2-Dichlorethane**	107-06-2	5	2-Methyl-1- propanol	78-83-1	5000
1,1-Dichloroethene**	75-35-4	8	2-Methylbutane	78-78-4	5000
1,2-Dichloroethene	540-59-0	1870	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	2170	Nitromethane	75-52-5	50
1,3-Dimethylbenzene	108-38-3	2170	Pentane	109-66-0	5000
1,4-Dimethylbenzene	106-42-3	2170	1-Pentanol	71-41-0	5000
2,2-Dimethylbutane	75-83-2	290	1-Propanol	71-23-8	5000
2,3-Dimethylbutane	79-29-8	290	2-Propanol	67-63-0	5000
N,N-Dimethylacetamide	127-19-5	1090	Propane	74-98-6	5000
N,N-Dimethylformamide	68-12-2	880	Propyl acetate	109-60-4	5000
Dimethyl sulfoxide	67-68-5	5000	Pyridine	110-86-1	200
1,4-Dioxane	123-91-1	380	Sulfolane	126-33-0	160
Ethanol	64-17-5	5000	Tetrahydrofuran	109-99-9	720
2-Ethoxyethanol	110-80-5	160	Tetralin	119-64-2	100
Ethyl acetate	141-78-6	5000	Toluene	108-88-3	890
Ethylbenzene	100-41-4	70	1,1,1-Trichloroethane**	71-55-6	1500
Ethylene glycol	107-21-1	620	1,1,2-Trichloroethylene	79-01-6	80
Ethylene oxide	75-21-80	50	Xylene	1330-20-7	2170
Ethyl ether	60-29-7	5000	1,1,2-Trichloroethylene	79-01-6	80
* See Section 6.0 of this regulation for further information.
** Class 1 solvents provided by USP Chapter <467> shall not be used in the production of any marijuana or marijuana product.

11.10.7.1 The upper limits for residual solvents in Table 6 are given as milligrams of residual solvent per kilogram of marijuana concentrate. The upper limits in Table 6 are based on residual solvent standards provided by the USP Chapter <467>, the International Conference on Harmonization (ICH, 2011), and AHP (2014).

11.10.7.2 Class 1 solvents shall not be used in the production of any marijuana or marijuana product.

11.10.7.3 Analyses to determine residual solvent concentrations in marijuana or marijuana products must be performed in accordance with the methods identified in USP Chapter <467>.

11.10.7.4 Any detection of solvents at any level must be reported to customers.

11.10.8 Quality control. Marijuana testing facilities must prepare and analyze samples in batches of up to 20 samples that include a laboratory reagent blank, a laboratory fortified blank, a sample duplicate, and a laboratory fortified sample for chemical tests.

11.10.8.1 For initial calibration, the analytical sequence must include initial and continuing instrument calibrations performed per the approved method requirements. If the approved method does not specify calibration requirements, then marijuana testing facilities must at a minimum perform a 3-point initial calibration spanning a concentration range from below to above the maximum allowable contaminant concentration. Marijuana testing facilities are required to achieve a linear response for all cannabinoids, metals, and pesticides analyses. The initial calibration for each analyte must have a relative standard deviation of 15% or a correlation factor of 0.995.

11.10.8.2 For continuing calibration, if approved analytical methods do not specify calibration requirements, the analytical sequence must include a continuing calibration standard and continuing calibration instrument blank before and after every 10 samples (including quality control samples). The percent difference of the continuing calibration response for all analytes must be equal to or less than 15% compared to the expected continuing calibration standard response. Marijuana testing facilities must document the calibration performance and quality control results for all analyses.

11.10.8.3 For quality control secondary, all calibrations must be verified with a standard obtained from a second manufacturer or a separate lot prepared independently by the same manufacturer at least quarterly. This verification is performed by analyzing a test solution of known analyte concentration after calibration and prior to sample analysis. Verification must be +/-20% of the known value.

11.10.9 Test reporting. Marijuana testing facilities must:

11.10.9.1 Report all testing results including all information necessary to determine product compliance to the Commissioner and the marijuana or marijuana product producer, including marijuana product manufacturers, marijuana micro-businesses, and marijuana cultivators.

11.10.9.2 Include the following in the laboratory data package:

11.10.9.2.1 A case narrative, written on marijuana testing facility letterhead, must describe any sample receipt, preparation, or analytical issues encountered as well as any method non-conformances or exceedance of quality assurance or quality control criteria used by the marijuana testing facility. The narrative must identify the preparation and analytical methods utilized by the marijuana testing facility. The narrative must include a signed statement by an authorized marijuana testing facility representative as to the accuracy, completeness, and compliance with the methods of the results presented;

11.10.9.2.2 Chain-of-custody information or other paperwork indicating requested analyses and documentation of sample collection and receipt must be reported with the marijuana testing facility's results;

11.10.9.2.3 Marijuana testing facility reports must clearly identify the name, address, and license number of the marijuana testing facility that performed the test and must include the results and the date of the reporting;

11.10.9.2.4 Multipage reports must be paginated;

11.10.9.2.5 A summary of analytical results including sample identifier, methods performed, target compounds, sample result or reporting limit, proper qualifier according to laboratory standard procedures, units of measure, preparation dates, where applicable, and analysis dates;

11.10.9.2.6 Analytical results which exceed the upper limit described in this regulation must be reported with a qualifier indicating the contaminant measured in the marijuana or marijuana product is above the allowable concentration; and

11.10.9.2.7 The marijuana testing facility data package must include sufficient data to evaluate the laboratory results, including a summary of laboratory quality assurance or quality control results.

Notes

4 Del. Admin. Code § 5001-11.0

28 DE Reg. 226 (9/1/2024) (Final)