Screening and confirmation methods for the qualitative identification of nine phytocannabinoids in urine by LC-MS/MS

Reber, Jami D; Karschner, Erin L.; Seither, Joshua Z; Knittel, Jessica L.; Walterscheid, Jeffrey P.

doi:10.1016/j.clinbiochem.2021.09.005

Cited by 11 publications

(5 citation statements)

References 23 publications

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“…The current method achieves lower or similar LODs than the literature for: CBD [ 38 , 39 , 40 , 41 , 42 ]; THC [ 33 , 38 , 39 , 40 , 41 , 42 , 43 , 44 , 45 ]; CBN [ 41 ]; 11-OH-THC [ 33 , 38 , 39 , 40 , 41 , 42 , 43 , 44 ]; and THC-COOH [ 38 , 46 , 47 ]. The same LLOQs are reported for: CBD [ 39 , 40 , 41 , 42 , 48 , 49 ]; THC [ 33 , 39 , 40 , 41 , 42 , 43 , 44 , 45 , 48 , 49 ]; CBN [ 39 , 40 , 41 , 48 , 49 ]; 11-OH-THC [ 33 , 39 , 40 , 41 ,…”

Section: Resultsmentioning

confidence: 81%

“…When using a GC–MS system [ 41 , 43 , 44 ], the authors report greater LODs and LLOQs than those obtained with the herein proposed technique. The same happens when using systems with greater sensitivity, such as LC–MS/MS [ 38 , 39 , 40 , 42 , 45 , 46 , 47 , 48 , 49 ]. Nonetheless, some authors report lower LLOQs than those obtained with our MEPS–GC–MS, mostly using techniques with greater sensitivity, including GC–MS/MS [ 50 , 51 , 52 , 53 ] and LC–MS/MS [ 38 , 39 , 42 , 46 , 54 , 55 , 56 , 57 , 58 , 59 ]; several of these approaches also used larger sample volumes.…”

Section: Resultsmentioning

confidence: 98%

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The Determination of Cannabinoids in Urine Samples Using Microextraction by Packed Sorbent and Gas Chromatography-Mass Spectrometry

et al. 2022

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Cannabis is the most consumed illicit drug worldwide, and its legal status is a source of concern. This study proposes a rapid procedure for the simultaneous quantification of Δ9-tetrahydrocannabinol (THC), 11-hydroxy-Δ9-tetrahydrocannabinol (11-OH-THC), 11-nor-9-carboxy-Δ9-tetrahydrocannabinol (THC-COOH), cannabidiol (CBD), and cannabinol (CBN) in urine samples. Microextraction by packed sorbent (MEPS) was used to pre-concentrate the analytes, which were detected by gas chromatography–mass spectrometry. The procedure was previously optimized, and the final conditions were: conditioning with 50 µL methanol and 50 µL of water, sample load with two draw–eject cycles, and washing with 310 µL of 0.1% formic acid in water with 5% isopropanol; the elution was made with 35 µL of 0.1% ammonium hydroxide in methanol. This fast extraction procedure allowed quantification in the ranges of 1–400 ng/mL for THC and CBD, 5–400 ng/mL for CBN and 11-OH-THC, and 10–400 ng/mL for THC-COOH with coefficients of determination higher than 0.99. The limits of quantification and detection were between 1 and 10 ng/mL using 0.25 mL of sample. The extraction efficiencies varied between 26 and 85%. This analytical method is the first allowing the for determination of cannabinoids in urine samples using MEPS, a fast, simple, and low-cost alternative to conventional techniques.

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Section: Resultsmentioning

confidence: 81%

Section: Resultsmentioning

confidence: 98%

The Determination of Cannabinoids in Urine Samples Using Microextraction by Packed Sorbent and Gas Chromatography-Mass Spectrometry

et al. 2022

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“…Several assays for determining CBD in different biological matrices such as peripheral capillary blood, plasma, serum, saliva, urine, breast milk and hair have been reported recently ( Pérez Montilla et al, 2021 ; Sempio et al, 2021b ; Cliburn et al, 2021 ; da Silva et al, 2020 ; Desrosiers et al, 2015 ; Cobo-Golpe et al, 2021 ; Reber et al, 2021 ). Although a few of these assays have also been validated for measuring the active metabolite 7-hydroxy-CBD in plasma or serum samples ( Sempio et al, 2021a ; Malaca et al, 2021 ), to our knowledge the present HPLC-MS/MS method is the first reported assay that permits the simultaneous determination of CBD and its active metabolite 7-hydroxy-CBD in both human serum and saliva.…”

Section: Discussionmentioning

confidence: 99%

On-Line Solid Phase Extraction High Performance Liquid Chromatography Method Coupled With Tandem Mass Spectrometry for the Therapeutic Monitoring of Cannabidiol and 7-Hydroxy-cannabidiol in Human Serum and Saliva

Franco

Palmisani²,

Marchiselli

et al. 2022

Front. Pharmacol.

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Cannabidiol is a novel antiseizure medication approved in Europe and the US for the treatment of seizures associated with Lennox-Gastaut syndrome, Dravet syndrome and tuberous sclerosis complex. We describe in this article a new and simple liquid chromatography-mass spectrometry method (LC-MS/MS) for the determination of cannabidiol and its active metabolite 7-hydroxy-cannabidiol in microvolumes of serum and saliva (50 μl), to be used as a tool for therapeutic drug monitoring (TDM) and pharmacokinetic studies. After on-line solid phase extraction cannabidiol, 7-hydroxy-cannabidiol and the internal standard cannabidiol-d3 are separated on a monolithic C18 column under gradient conditions. Calibration curves are linear within the validated concentration range (10–1,000 ng/ml for cannabidiol and 5–500 ng/ml for 7-hydroxy-cannabidiol). The method is accurate (intraday and interday accuracy within 94–112% for cannabidiol, 91–109% for 7-hydroxy-cannabidiol), precise (intraday and interday precision <11.6% for cannabidiol and <11.7% for 7- hydroxy-cannabidiol) and sensitive, with a LOQ of 2.5 ng/ml for cannabidiol and 5 ng/ml for 7-hydroxy-cannabidiol. The stability of the analytes was confirmed under different storage conditions. Extraction recoveries were in the range of 81–129% for cannabidiol and 100–113% for 7-hydroxy-cannabidiol. The applicability of the method to TDM was demonstrated by analysis of human serum and saliva samples obtained from patients with epilepsy treated with cannabidiol.

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“…To date, more than 100 phytocannabinoids have been successfully chemically characterized. These compounds, through their interaction with the endocannabinoid system, serve as a cornerstone for the therapeutic use of Cannabis species [ 5 , 6 ].…”

Section: Introductionmentioning

confidence: 99%

The Potential of Hemp Extracts to Modify the Course of Oxidative-Stress Related Conditions

Bijelić,

Srdjenović Čonić,

Prpa

et al. 2024

Plants

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The leaves of industrial hemp, which have long been considered as a waste product, have been proven to contain numerous compounds that possess potential biological activity. One of the most interesting groups of compounds present are polyphenolic compounds, which, due to their specific structure, have a pronounced antioxidant and antihyperglycemic potential. This study aimed to detect biological activity, including antioxidant and antihyperglycemic potential, of water and water–alcoholic extracts of five commercially available hemp teas, followed by phytochemical profiling. Hemp aqueous and ethanolic extracts demonstrate potent antioxidant properties. Ethanol extracts are better scavengers of DPPH• and OH•, while aqueous extracts neutralize NO• better. Both types of extracts exhibit antioxidant potential in the catalase test and moderate XOD inhibition. Furthermore, aqueous extracts are potent α-amylase inhibitors, while ethanolic extracts demonstrate stronger anti-α-glucosidase activity, suggesting therapeutic potential for chronic diseases like insulin resistance or diabetes. Further detailed chemical characterization and in vivo studies are needed to validate these findings.

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Screening and confirmation methods for the qualitative identification of nine phytocannabinoids in urine by LC-MS/MS

Cited by 11 publications

References 23 publications

The Determination of Cannabinoids in Urine Samples Using Microextraction by Packed Sorbent and Gas Chromatography-Mass Spectrometry

The Determination of Cannabinoids in Urine Samples Using Microextraction by Packed Sorbent and Gas Chromatography-Mass Spectrometry

On-Line Solid Phase Extraction High Performance Liquid Chromatography Method Coupled With Tandem Mass Spectrometry for the Therapeutic Monitoring of Cannabidiol and 7-Hydroxy-cannabidiol in Human Serum and Saliva

The Potential of Hemp Extracts to Modify the Course of Oxidative-Stress Related Conditions

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