Cannabis Analysis

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The cannabis industry has been taking a hard look at the science behind their products and the various contaminants that can inadvertently be added to consumer goods. As testing laboratories begin to implement new state-mandated regulations and other consensus methods for best practices, there is a need to review the analytical instruments and methods that can deliver the most accurate results in a timely fashion. Anthony Macherone, senior scientist at Agilent Technologies and visiting scientist at the Johns Hopkins University School of Medicine, recently spoke to us about his research in this area and the chromatographic techniques he has found to be most effective for profiling cannabinoids and terpenes, detecting pesticides, and residual solvents testing.

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The medicinal qualities of cannabinoids contained in hemp have been described in detail. Pain mitigation and reduced severity of nausea and seizures are just a few of the therapeutic benefits reported by medical cannabis patients. There is evidence that a combination of CBD, a host of other minor cannabinoids, and a complex array of terpenoids as contained in hemp oil may be the most beneficial, which is why CBD-rich oil for oral intake has become increasingly popular. The FDA has issued warning letters to firms that market unapproved new drugs allegedly containing CBD. As part of these actions, the cannabinoid content of some hemp products was determined and many were found to contain levels of CBD largely deviating from the label claim. Like cannabis, hemp oil can be analyzed easily and effectively for its cannabinoid content. This article highlights the use of a fast and simple HPLC–UV assay for separation and quantification of 11 important cannabinoids, including CBD in hemp oil.

The presence of capable students and researchers, each with a technical niche to offer, prepares us for future opportunities. On top of that structure, we also aim to maintain this mindset for our instrument selection before beginning projects. The installment of core labs at UT Arlington (www.uta.edu/sirt), making a wide range of instruments available to all research groups, has allowed our students to brainstorm about which instrument is the most appropriate for a specific analysis rather than how to make a measurement work with a given instrument.

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As a result of the rapid growth of the cannabis industry, many testing laboratories are looking for efficient, reliable, and cost-effective analytical methods to analyze chemical residues, such as pesticides, mycotoxins, solvent residues, terpenes, and heavy metals, as well as cannabinoid concentration in cannabis-infused edibles and beverages. In this article, QuEChERS (quick, easy, cheap, effective, rugged, and safe), a sample preparation technique widely adopted in the food testing industry, is introduced to the discipline of forensic testing as a viable method for the extraction of pesticides and cannabinoids in various complex sample matrices. The claimed amounts of cannabinoids versus the actual amounts are compared, as well as the pesticide residue levels in edible and beverage samples.

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Giuseppe Cannazza and Cinzia Citti from the University of Modena and Reggio Emilia discuss the growing interest in the use of medicinal cannabis in Europe and the analytical challenges involved.

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A primary impediment to cannabinoid research is the fact that materials possessing psychoactive Δ-9-tetrathydrocannabinol are considered Schedule I drugs as defined in the U.S. Controlled Substances Act. An alternative source of cannabinoids may be found in hemp oil extracts. Hemp contains a low percentage of Δ-9-tetrathydrocannabinol (THC) by weight but relatively high amounts of non-psychoactive cannabinoids. The liquid chromatography-time of flight mass spectrometry (LC-TOF) method presented herein allows for the accurate, precise and robust speciation, profiling and quantification of cannabinoids in hemp oil extracts and commercial cannabinoid products for research and development laboratories. The method was determined to chromatographically separate 11 cannabinoids including differentiation of Δ-8-tetrahdrocannabinol and THC with excellent linear dynamic range, specificity and sensitivity.

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As the legalization of medicinal cannabis continues to sweep across the United States, an urgent need has developed for fast, accurate and efficient analytical testing. In addition to testing for contaminants and potency, there is also interest in the determination of terpene identity and concentration levels present in different strains of cannabis. Terpenes have been shown to have therapeutic uses for treatment of different medical conditions ranging from cancer and inflammation, to anxiety and sleeplessness. It is believed that the combination of terpenes and cannabinoids in cannabis produce a synergistic effect with regards to medical benefits. The traditional testing method for terpenes in plant materials involves a solvent-based extraction followed by GC analysis. In this work, headspace solid phase microextraction (HS-SPME) was used to identify and quantify terpene content in cannabis. The HS-SPME method provided several advantages over solvent extraction in that it provided a cleaner analysis, free of interferences from co-extracted matrix, and was non-destructive to the sample. A cannabis sample of unknown origin was first analyzed qualitatively by HS-SPME and GC-MS. Spectral library matching and retention indices were used to identify 42 different terpenes. Quantitative analysis was then performed for several selected terpenes using spiked samples. Method accuracy was >90%, with reproducibility of

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While systems for growing, production and sale of cannabis and cannabis related products are well established, regulation and enforcement of quality and safety testing have lagged behind. However, state governments and private labs are focusing on product safety testing with special emphasis on pesticide analysis. This is partially the result of various product recalls, media attention and concern from patient advocacy groups. We evaluated a modified QuEChERS LC-MS/MS method for analysis of multiresidue pesticides. The AOAC QuEChERS method was used for a reduced 1.5 g amount of plant material and processed with a universal dSPE formulation. LC-MS/MS analysis used constant polarity switching ESI and monitored at least two transitions per analyte. Matrix-matched calibration was used for quantitation and both method and instrument internal standards were used. Analyte recovery validation was performed according to FDA guidelines by testing three matrices at three fortification levels in triplicate for over 200 pesticides. For the large majority of pesticides, in all three matrices and at all three fortification levels, recovery was between 70-120%.

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Research scientists in the cannabis field are tasked with validating robust methods that can be seamlessly transitioned into production laboratories. Unlike typical disciplines where controls are easily (and legally) obtained through known manufacturers, analytical chemists working for both consumable vendors as well as cannabis laboratories must do their best to develop methods often without such resources at their disposal. As the industry matures and additional regulations are adopted, the evolution of the pesticide testing subsection continues to be vastly different depending on the jurisdiction one does business in. This creates an interesting challenge for commercial scientists tasked with developing methods that will appeal to a majority of their consumers, while also generating unexpected hurdles to said laboratories once the methods are placed into production. Ace Analytical Laboratory, located in Las Vegas, Nevada, has successfully adopted and validated pesticide testing methods for their cannabis laboratories and has gained valuable insight into how to best work with such a difficult matrix. In conjunction with UCT, LLC, an overview of best practices and method development techniques for pesticide testing in cannabis is discussed below and told from a technical perspective.

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This study will focus on an ICP-MS sample preparation procedure and analytical methodology optimized for both toxic and nutritional elements in dried hops, a surrogate for the cannabis family of flowering plants. It will show that the wide dynamic range of the technique allows it to be used for the simultaneous determination of parts per billion (ppb) levels of heavy metals including Pb, As, Cd and Hg, together with high parts per million (ppm) levels of nutritional elements, such as P, Ca, K and Mg.

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In recent years, synthetic cannabinoids (or “spice”) have experienced a boom in popularity. The negative health effects of these drugs coupled with their increasing popularity led to placement onto Schedule I by the DEA. In response, the chemists behind these illicit compounds frequently invent new compounds to circumvent the law. Thus, new classes and new examples within classes of “spice” continue to become available for illicit use. In this paper, we examine the use of two different column chemistries (C18 and phenyl-hexyl) in an effort to definitively identify synthetic cannabinoid compounds in patient samples.

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Gas chromatography (GC) is an established and well-understood technique. As the cannabis industry grows, demand for analytical robustness is increasing for analytes such as pesticides, residual solvents, and terpenes. GC and GC coupled to mass spectrometry (GC–MS) are effective tools to address the demands of laboratories, growers, manufacturers, and consumers. This article provides an overview of the types of compounds that can be analyzed by GC, reviews the strengths and weaknesses of the analytical methods, and discusses areas of opportunity for chromatography.

The variance in the toxic effects of designer cannabis drugs marketed throughout Europe and the USA as "K2" or "Spice" could be the result of stereoselective metabolism of enantiomers by lung and liver enzymes, according to a study published in Analytical Chemistry.

Designer Cannabinoids

The variance in the toxic effects of designer cannabis drugs marketed throughout Europe and the USA as "K2" or "Spice" could be the result of stereoselective metabolism of enantiomers by lung and liver enzymes, according to a study published in Analytical Chemistry.