A growing need is emerging for testing to detect the presence of mycotoxins in both raw plant materials and finished cannabis products in order to protect consumer health and safety. The analysis of mycotoxins in cannabis oils is particularly challenging because the sample lipids can contribute isobaric matrix interferences in addition to general ion suppression, which can reduce accuracy especially at low levels. In this video, a simple pass-through SPE sample cleanup was applied to lipid-rich CBD oils. Excellent chromatographic results were obtained for both aflatoxins and ochratoxins even at 2 ng/g, indicating that the simplified sample prep technique effectively removed lipid interferences. The SPE sample cleanup was paired with a rapid LC-MS/MS analysis utilizing a Raptor Biphenyl column.
- High-Throughput Analysis of Mycotoxins in Cannabis CBD Oil Pairs Simplified Cleanup with LC-MS/MS Sensitivity
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Thanks for joining us for this Restek video where we’ll discuss a simple workflow solution for analyzing mycotoxins in CBD oil.
Our first step is to weigh 0.25 g of CBD oil into a 2.0 mL amber vial. We’ll then add 10 µL of our working internal standard into the sample and vortex for 10 seconds. Now, we want to concurrently precipitate the matrix and extract our analytes of interest, so we will add 1 mL of 45:55 water:methanol to the sample vial and vortex again, this time for 30 seconds. We’ll then centrifuge the sample for five minutes to pull the solids to the bottom of the tube. Also, we want to centrifuge at 10 °C to ensure analyte stability.
Our last cleanup step will help us remove any remaining matrix interferences. We’ll use a Resprep C18 SPE cartridge for this. You need to first condition the cartridge with our loading solvent which is 45:55 water:methanol. Once our cartridge is ready, we’ll transfer 750 µL of our sample to it. Then we will use a vacuum manifold to pull the sample through the cartridge and into an autosampler vial.
Now we are ready for our LC-MS/MS analysis. We also used a guard column to help protect our analytical column against any contaminants that remain. The Raptor Biphenyl analytical column gives us the necessary retention, while allowing us to complete the run in under three minutes. Once you’ve established the method according to your lab’s validation SOPs, you’re ready to run your samples and collect data.
Thank you for watching. You can find more details of the workflow at this link. And, if you want to see more videos about cannabis analysis, please let us know in the comments and don’t forget to like this video!