10.1371/journal.pone.0196396.g001 Fig 1 LC-MS/MS profiles of cannabinoids in matrix.
The validated method was applied to 40 finished products labelled as hemp-containing and available in Canada, ordered online or purchased in-store. The test articles included a variety of oils, plant materials, and creams in the forms of cosmetics, personal care products, hemp oils marketed for cooking, massage oil, body butter, tinctures, and supplements ( Fig 2 and S1 Table ). Within the 40 products tested, 38 products had THC levels well below the Canadian legal limit of 10 μg/g, one hemp oil (10.01 μg/g) contained slightly above that limit, and only one tincture (337 μg/g) was tremendously higher. That suggested the current regulations are working to limit access to high-THC C . sativa products marketed as hemp. The hemp products had a wide range of measured CBD concentrations, from below the limit of quantification (< 0.19 μg/g) to 8,410 μg/g. The product with the highest measured THC and CBD content contained 337 μg/g and 8,410 μg/g respectively ( Fig 2 , product # 17). The oil-based products were found to have overall higher levels of CBD and CBDA than the non-oil products in general. Most of the cosmetic products did not contain cannabinoid levels above the very low LLOQ, although they were marketed as hemp-containing. There was a large difference in the CBD content of the three products with the highest CBD content ( Fig 2 , products # 13, 15, and 17; >2,800 μg/g) and the remaining products (<20 μg/g). An interesting trend emerged between the concentration of CBD in a commercial sample and the ratio of the CBD:CBDA within the same sample. 90% of CBD and CBDA containing products had higher concentrations of CBDA than CBD. In stark contrast, the three products with the highest concentrations of CBD had very low relative levels of CBDA with CBD:CBDA ratios between 1,000:1.4 and 1,000,000:1.7. The ratio of THC:THCA or CBD:CBDA can vary in plants from strain to strain, but the lack of CBDA in the CBD-rich samples suggests an adulteration in the sample, either through a significant difference in processing methods or the addition of pure CBD to the end product.
Extraction recoveries for THC, CBD, CBDA, and THCA-A from olive oil were between 87.5–98.5%, 86.9–109.6%, 91.6–100.0%, and 83.7–102.3%, indicating a satisfactory extraction procedure ( Table 5 ). Matrix effects of THC, CBD, CBDA and THCA-A were 110.4–116.0%, 105.4–112.2%, 96.3–117.8%, and 92.7–107.8%, therefore no significant matrix effect in oil was observed.
* Quality control samples of 200 ng/mL were diluted 1/10 with extraction solvent before injection
High performance liquid chromatography- tandem mass spectrometry was carried out on 5500 QTRAP Mass spectrometer (ABSciex, Concord, Canada) with a TurboV source, equipped with Agilent 1260 (Agilent Technologies, Santa Clara CA, USA) HPLC. Other equipment included Biofuge Fresco Heraeus centrifuge, Mettler Toledo analytical balance and mini vortexer.
10.1371/journal.pone.0196396.g002 Fig 2 Comparative concentrations of cannabinoids in 40 commercial hemp finished products.
A solution of 50 ng/mL of each of CBD, THC, CBDA, THCA-A and 10 ng/mL of CBD-d3, THC-d3 and THCCOOH-d3 was serial diluted with an equal volume of a solution of 10 ng/mL of CBD-d3, THC-d3 and THCCOOH-d3 to give a calibration curve with concentrations of CBD, THC, CBDA, THCA-A of 50, 25, 12.5, 6.25, 3.12, 1.56, 0.78, 0.39 and 0.19 ng/mL and a constant concentration of CBD-d3, THC-d3, and THCCOOH-d3 (10 ng/mL each). The peak area ratio of the analytes to their corresponding IS vs. concentration of analytes was fit with a weighted quadratic curve or linear curve using Analyst software 1.6.2. Quality control samples were prepared from olive oil at concentrations of 0.5, 5, 50 and 200 ng/mg for every batch of commercial products test.
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2021-02-17 true journals.sagepub.com 10.1177/0269881120986393