CBD Infused Beverages: The Recovery Dilemma…Solved?

CBD infused beverages are everywhere. I see them at the grocery store, gas station, and even at the liquor store. As popular as these beverages are, they are challenging from an analytical standpoint to test for potency. During the formulation process, it takes some finesse to get hydrophobic compounds, such as cannabinoids, to emulsify with a water-based beverage, which makes this type of matrix uniquely challenging to analyze.

Recovery experiments are a routine part of method development, and it is especially important for a sample such as infused beverages, where an emulsion has to be broken before the analyte can be detected. We’d need access to both the base beverage and the stabilized emulsions in order to perform standard addition based recovery, so how can we perform recovery experiments in their absence?

To overcome this obstacle, a potency in beverage matrix proficiency test (PT) was used to confirm the efficacy of the developed sample preparation method. A PT is a great way to measure the performance of your method objectively and to ensure that your methodology is suitable for its intended purpose. In this case, the PT contained 5 cannabinoids at unknown concentrations in a carbonated base beverage. The beverage was taken though the sample preparation process, analyzed, and the results were submitted to the PT provider. The results were confirmed to fall within the acceptable reporting range indicating that our method was working as intended.

Feeling confident in our method now that the recovery dilemma had been addressed, additional samples were obtained locally, tested, and compared with their label value. CBD infused sparkling flavored water, drink powder, concentrated beverage, and juice were obtained for analysis. Carbonated beverages were sonicated for 30 minutes prior to use. Each sample was prepared by aliquoting 10 mL of beverage into a 50 mL centrifuge tube. 10 mL of ACN was added to the sample along with an EN QuEChERS salt packet (catalog number 25849). The sample was then shaken by hand for 1 minute followed by vortexing for 30 seconds. The samples were transferred to a shaker table and shaken for 10 minutes followed by centrifugation at 4200 rpm for 10 minutes. An aliquot was transferred to an autosampler vial. Concentrated samples were further diluted before analysis. All samples were extracted in triplicate and analyzed in triplicate. Below is a summary of the results:

Type of CBD infused beverage	CBD mg label claim per container (mg)	Experimentally determined mg CBD per container (mg)	Concentration label claim (ppm)	Experimentally determined concentration (ppm)	% RSD	% Difference
Flavored Sparkling Water- 1	25	27.4	70.4	77.3	3	10
Flavored Sparkling Water- 2	25	28.5	70.4	80.2	1	14
Drink Powder	10	13.3	40.0	53.1	2	33
Concentrated beverage- 1	50	61.7	848	1045	23	23
Concentrated beverage- 2	50	30.0	848	491	15	42
Juice Drink- 1	10	8.70	40.0	24.9	3	13
Juice Drink- 2	10	11.5	40.0	46.1	2	15

Table 1. Summary of results for CBD infused beverages.

The results of this analysis were very similar to the label claim for both flavored carbonated waters and both juice drinks ranging from 10-15% difference from their label value. Both concentrated beverages and drink powder had higher percent differences from their label claims ranging from 23-42%. The high %RSD for the concentrated beverages suggests that the sample may not be homogenous which could help explain the difference from the label claim.   There could also be an actual discrepancy in CBD concentration in the sample or the QuEChERS methodology may not be fully breaking the emulsion.

While QuEChERS was able to break the emulsion for the PT, this is not a foolproof workflow for determining recovery. The ideal situation would be to perform recovery experiments with each type of beverage using the base beverage and stabilized emulsions, but without having access to these, a good way to demonstrate method effectiveness is to test the workflow using a PT. Is your lab currently running this analysis or interested in running this analysis? Let us know in the comment section below!

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