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Quantification of 14-Cannabinoids in Gummy Edibles using GummyPak SPK with Cann-ID™ Potency Testing Solution


     Recovery and potency results are shown for 14 cannabinoids in hemp infused gummy edibles using GummyPak Sample Prep Kit (SPK) with Cann-ID Potency Testing Solution. Two sample preparation methods, traditional extraction by sonication in extraction solvent and extraction by the GummyPak SPK method, are compared. Recovery data of 14-cannabinoids from spiked gummy matrix is shown and CBD label claims are determined for four different gummy products. Results from Cann-ID with GummyPak SPK are compared to 3rd Party COAs showing good agreement.

Technology Benefits:

  • Cann-ID GummyPak SPK presents a simplified application solution for the analysis of 14-cannabinoids in gummy edibles
  • Cann-ID Potency Testing Solution with GummyPak SPK provides recoveries between 91% and 109% for all 14-cannabinoids in the Cann-ID standard cannabinoid panel
  • Cann-ID with GummyPak SPK decreases capital cost and lowers the barrier to entry for deploying sophisticated HPLC technology in-house for testing cannabis infused gummy products
  • Cloud-based automated reporting instantly shares results across client networks and between industry stakeholders
  • Dedicated application support from Ionization Labs’ team of chemists ensures clients remain operational, generating valuable potency data for gummies and a range of other cannabis-based consumer product goods
  • These results show that Cann-ID with GummyPak SPK is well suited for the routine QA/QC analysis of cannabis infused gummies

Introduction:

     Gummies have become a major driver of growth for cannabis (low THC hemp and high THC marijuana) brands over the last 2 years [2]. As a result, manufacturers of cannabis infused gummy products desire simple, robust potency testing solutions for verifying the cannabinoid composition of their products. This is especially important since the price and therapeutic (or recreational) user experience is often tied directly to the potency of the product.

     Traditional HPLC sample preparation techniques, such as those utilized for flower and extracts or concentrates, struggle to liberate the oily (hydrophobic) cannabinoids from the sugary (hydrophilic) gummy matrix (Table 1). This results in low extraction efficiency, poor recovery of cannabinoids from gummy products, and inconsistent analytical potency results. This variability has traditionally complicated the analysis of these popular consumer products and limited widespread adoption of internal QA/QC procedures for these products. As a result, product manufacturers are forced to outsource gummy potency testing to third party labs for routine quality and consistency analysis. The problem of poor extraction efficiency and inconsistent potency results is resolved for most gummy matrices with the Cann-ID Potency Testing Solution with GummyPak SPK. Standardizing and simplifying the sample preparation and analysis process for cannabis infused gummy products allows manufacturers to deploy Cann-ID Potency Testing Solution with confidence for in-house potency testing of infused gummy products.


Technology Summary:

     The Cann-ID Potency Testing Solution [1] is a subscription based in-house analytical testing solution provided by Ionization Labs. The Cann-ID Potency Testing Solution consists of High-Performance Liquid Chromatography (HPLC) and laboratory testing hardware, Cann-ID instrument control and cloud-based reporting software, and recurring analysis consumables and analytical standards all billed on a per test subscription basis. The result is fully supported laboratory-grade HPLC potency results generated in-house with the full-support of Ionization Labs, an ISO 17025 accredited potency testing laboratory.

     At a fraction of the cost compared to 3rd party analytical testing, Cann-ID is built for high-volume potency testing in-house throughout the cannabis product development lifecycle. Cann-ID Software simplifies the hardware-reporting interface, making complex potency analysis, results interpretation, and data validation accessible to users with little to no analytical experience. Results are published to the cloud so they can be easily shared with stakeholders inside and outside the organization. Cann-ID comes with sample preparation, analysis, and data validation methods built in, and dedicated support from Ionization Labs’ team of application chemists included.

 

     As an addition to the standard Cann-ID platform, the GummyPak Sample Prep Kit (SPK) provides Cann-ID users the ability to generate reliable laboratory grade potency results for cannabis infused gummy edibles. The GummyPak SPK allows gummy product manufacturers to utilize Cann-ID for in-house research and development and QA/QC of their gummy products. Moving these routine but necessary tests in-house and simplifying the sample preparation and data validation process lowers the cost of maintaining a robust quality program for gummy product manufacturers. Testing in-house significantly decreases the necessity of expensive and time-consuming 3rd party analyses; this saves time and money while improving gummy product quality, consistency, and end-user experience.


Experimental Description and Results:

     Traditional extraction techniques using 5 different extraction solvents with heated sonication was evaluated for the extraction of cannabinoids from gummies and compared to the GummyPak SPK method (Table 1). Three gummies from the same package were cut into small pieces, mixed, and distributed equally for the six tests. The CBD recoveries from each test were normalized by dividing each test result by the result from the GummyPak SPK extraction method. These results show that traditional extraction techniques are not adequate for extracting CBD from gummy products for quantitative analysis, with relative recoveries ranging from 57% to 84% compared to the GummyPak SPK method.

Table 1. Extraction of CBD from gummy matrix. Five different extraction solvents are normalized and compared to the Cann-ID GummyPak extraction method for cannabis infused gummy products.

Extraction Solvent, 4 mL CBD (mg/g) % Relative Recovery
MeOH 4.72 84.4%
ACN 3.18 56.9%
IPA 3.84 68.7%
ACN/Water (1:1) 3.49 62.4%
MeOH/Water (1:1) 3.51 62.8%
GummyPak SPK 5.59 100.0%

     A matrix spike recovery test was performed on 14-cannabinoids in gummy matrix utilizing the GummyPak SPK extraction method (Figure 1, Supporting Data Table 3). One gummy was spiked with 50 ug of each cannabinoid (~20 ppm each) and assayed using the Cann-ID with GummyPak SPK test method. Recoveries were calculated ranging from 91% to 109%, with an average cannabinoid recovery of 96%. Recovery of important analytes CBD, d9-THC, and d8-THC was calculated at 96%, 95%, and 96% respectively (Supporting Data Table 3).

Figure 1. Recovery of 14-cannabinoids from gummy matrix using GummyPak SPK method. Each cannabinoid was spiked at approximately 20 ppm.

     Four different retail gummy samples were tested using the Cann-ID Potency Testing Solution with GummyPak SPK and compared to 3rd party lab results provided with the product documentation (Table 2). For all samples, the difference between the Cann-ID results and 3rd party lab results are less than 20%. To put this between lab variation in perspective for this matrix, a recent proficiency test for cannabinoids in gummy matrix from Absolute Standards [3] accepted a reported (test) value ±40% of the assigned value for CBD and THC as “passing”. It is also worth noting that test results on one gummy from a batch can vary significantly from another gummy in that batch, highlighting the need for product manufacturers to perform thorough sampling and quality testing throughout the product manufacturing lifecycle.

Table 2. Comparison of CannID with GummyPak SPK results to 3rd party analytical results and manufacturer label claims for four different CBD infused gummy products.


Milligrams of CBD per Gummy

Cann-ID Result 3rd Party COA Package Claim
Gummy 1 8.62 8.47 8
Gummy 2 14.20 16.7 25
Gummy 3 28.12 23 20
Gummy 4 29.11 25.35 23

Summary:

     Cannabis infused gummy products are some of the most popular cannabis products on the market, and they are also some of the most difficult cannabis products to assay. As a result, simple, standardized, and robust sample preparation and analysis methods are needed for routine quality testing in-house. The Cann-ID Potency Testing Solution with GummyPak SPK was deployed for the quantification of 14-cannabinoids in cannabis infused gummy edibles. Traditional sample preparation extraction techniques were shown to be inadequate, extracting 57% to 84% of the available CBD compared to 96% using the GummyPak SPK method. Four different retail gummy products were tested using Cann-ID with GummyPak SPK and compared to 3rd party lab results showing good agreement for all products tested. These results show significant improvement over traditional sample preparation techniques for the analysis of cannabinoids in gummy products. As a result, gummy product manufacturers can deploy Cann-ID Potency Testing Solution with GummyPak SPK for routine testing of gummy products in-house.


Supporting Data:

Table 3. Recovery study for 14-cannabinoids from gummy matrix using Cann-ID GummyPak SPK.

Analyte Spiked Amount, ug Recovered Amount, ug Percent Recovery
CBDV 51.503 47.344 91.9%
CBDVA 51.355 49.698 96.8%
THCV 51.354 55.99 109.0%
CBD 51.388 49.445 96.2%
CBG 51.354 46.893 91.3%
CBDA 51.476 49.94 97.0%
CBG 50.645 48.697 96.2%
CBN 50.812 47.927 94.3%
d9-THC 50.936 48.136 94.5%
d8-THC 50.925 48.983 96.2%
CBC 51.245 47.784 93.2%
CBNA 51.175 49.181 96.1%
THCA 51.346 49.434 96.3%
CBCA 50.957 47.586 93.4%

References:

  1. Cann-ID by Ionization Labs, www.IonizationLabs.com
  2. Gummies are as popular as ever (link), BDSA, July 22, 2019, accessed online October 7, 2020
  3. Proficiency Test, Cannabinoids in Gummy Matrix PT (link), PN: 38468, Absolute Standards Inc., accessed online October 9, 2020