Development and validation of an assay to measure cannabidiol and Δ9-tetrahydrocannabinol in human EDTA plasma by UHPLC-MS/MS

Ocque, Andrew J.; Hagler, Colleen E.; DiFrancesco, Robin; Lombardo, Jeffrey; Morse, Gene D.

doi:10.1016/j.jchromb.2019.03.002

Cited by 17 publications

(13 citation statements)

References 10 publications

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“…Marijuana or hashish, a cocktail of at least 30 different major cannabinoids, generally prepared from crushing the leaves, flowers (inflorescenses) and even stems of C. sativa , is one of the oldest recreational and addictive natural products used by humans for centuries . However, the non‐medical use of Cannabis or marijuana is illegal in many countries, which prompts the use of analytical tools, like HPLC and UPLC, to analyse biological and forensic samples like blood, oral liquid, hair and urine, to confirm marijuana usage (Tables ) . After consumption of marijuana, THCA ( 13 ), which is present in the crude marijuana, but converted to THC ( 12 ) by heat during smoking, is excreted in the urine as its glucuronide conjugate, and can be analysed comfortably by LC methods.…”

Section: Hplc and Uplc (Or Uhplc) Analysis Of Naturally Occurring Canmentioning

confidence: 99%

“…In fact, blood, plasma and serum samples are quite extensively used in forensic analysis to detect the consumption of cannabinoids . HPLC and UPLC methods are commonly used for the analysis of cannabinoids in blood samples …”

Section: Hplc and Uplc (Or Uhplc) Analysis Of Naturally Occurring Canmentioning

confidence: 99%

“…Blood plasma samples are quite often used in forensic analysis for the detection of illegal cannabinoids consumption, and the use of HPLC and UPLC methods, both applying simple UV‐PDA or ESI‐MS/MS detection technologies is common . An HPLC method utilising APCI (atmospheric pressure chemical ionisation)‐MS/MS in positive ion mode associated with extensive ion suppression was employed to analyse naturally occurring cannabinoids in 352 human plasma samples, providing simultaneous quantification of several cannabinoids and their biotransformed products including CBC ( 1 ), CBD ( 3 ), CBDV ( 5 ), CBN ( 8 ), CBG ( 6 ), THC ( 12 ), 11‐OH‐THC ( 9 ), THCV ( 14 ), 11‐nor‐9‐carboxy‐Δ 9 ‐tetrahydrocannbinol (THC‐COOH, 10 ), Δ 9 ‐tetrahydrocannabivarin‐carboxylic acid (THCV‐COOH, 15 ), and THC‐COOH‐glucuronide .…”

Section: Hplc and Uplc (Or Uhplc) Analysis Of Naturally Occurring Canmentioning

confidence: 99%

“…The only two UPLC methods reported since 2010 for the analysis of cannabinoids in human plasma samples used MS detection technology, applying the ESI‐MS/MS technique …”

Section: Hplc and Uplc (Or Uhplc) Analysis Of Naturally Occurring Canmentioning

confidence: 99%

“…. While Ocque et al . used an isocratic elution with 18:82:0.02 water–MeOH–HCOOH over 8.5 min to identify cannabinoids 3 , 4 , 8 , 9 and 12 – 14 , the other study employed a gradient elution with water–MeOH (containing 0.1% HCOOH) offering the quantification of CBD ( 3 ), 11‐OH‐THC ( 9 ), THC‐COOH ( 10 ) and THC ( 12 ).…”

Section: Hplc and Uplc (Or Uhplc) Analysis Of Naturally Occurring Canmentioning

confidence: 99%

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A review on the recent advances in HPLC, UHPLC and UPLC analyses of naturally occurring cannabinoids (2010–2019)

Nahar

Önder

Sarker

2019

Phytochemical Analysis

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Introduction Organic molecules that bind to cannabinoid receptors are called cannabinoids, and they have similar pharmacological properties like the plant, Cannabis sativa L. Hyphenated liquid chromatography (LC), incorporating high‐performance liquid chromatography (HPLC) and ultra‐performance liquid chromatography (UPLC, also known as ultrahigh‐performance liquid chromatography, UHPLC), usually coupled to an ultraviolet (UV), UV‐photodiode array (PDA) or mass spectrometry (MS) detector, has become a popular analytical tool for the analysis of naturally occurring cannabinoids in various matrices. Objective To review literature on the use of various LC‐based analytical methods for the analysis of naturally occurring cannabinoids published since 2010. Methodology A comprehensive literature search was performed utilising several databases, like Web of Knowledge, PubMed and Google Scholar, and other relevant published materials including published books. The keywords used, in various combinations, with cannabinoids being present in all combinations, in the search were Cannabis, hemp, cannabinoids, Cannabis sativa, marijuana, analysis, HPLC, UHPLC, UPLC, quantitative, qualitative and quality control. Results Since 2010, several LC methods for the analysis of naturally occurring cannabinoids have been reported. While simple HPLC‐UV or HPLC‐UV‐PDA‐based methods were common in cannabinoids analysis, HPLC‐MS, HPLC‐MS/MS, UPLC (or UHPLC)‐UV‐PDA, UPLC (or UHPLC)‐MS and UPLC (or UHPLC)‐MS/MS, were also used frequently. Applications of mathematical and computational models for optimisation of different protocols were observed, and pre‐analyses included various environmentally friendly extraction protocols. Conclusions LC‐based analysis of naturally occurring cannabinoids has dominated the cannabinoids analysis during the last 10 years, and UPLC and UHPLC methods have been shown to be superior to conventional HPLC methods.

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Section: Hplc and Uplc (Or Uhplc) Analysis Of Naturally Occurring Canmentioning

confidence: 99%

Section: Hplc and Uplc (Or Uhplc) Analysis Of Naturally Occurring Canmentioning

confidence: 99%

Section: Hplc and Uplc (Or Uhplc) Analysis Of Naturally Occurring Canmentioning

confidence: 99%

“…The only two UPLC methods reported since 2010 for the analysis of cannabinoids in human plasma samples used MS detection technology, applying the ESI‐MS/MS technique …”

Section: Hplc and Uplc (Or Uhplc) Analysis Of Naturally Occurring Canmentioning

confidence: 99%

Section: Hplc and Uplc (Or Uhplc) Analysis Of Naturally Occurring Canmentioning

confidence: 99%

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A review on the recent advances in HPLC, UHPLC and UPLC analyses of naturally occurring cannabinoids (2010–2019)

Nahar

Önder

Sarker

2019

Phytochemical Analysis

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Pharmacokinetic and metabolic analysis of an Alzheimer's disease therapeutic in rat serum via microfluidic CZE–MS

Kelley

Lovell

Lynn

2021

Biomedical Chromatography

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Sensitive, high‐throughput methods for pharmacokinetic (PK) profiling are essential for potential therapeutics during critical stages of clinical trials. The application of a microfluidic capillary zone electrophoresis mass spectrometry (CZE–MS) method for PK profiling allows for rapid, sensitive and in‐depth analysis of multiple samples within a short timeframe. Here, a CZE–MS approach for PK analysis was compared with a traditional UHPLC–MS approach when analyzing serum extracts from rats treated with a potential Alzheimer's disease therapeutic, BNC‐1. Resulting PK data generated from both methods displayed statistical similarities. Additionally, the separation efficiency attributed to the use of the CZE–MS method provided substantial metabolic regulation data that was not apparent in the UHPLC–MS method. Additionally, the coupling of the CZE–MS method to the data processing software, MZmine2, was used to monitor changes in metabolism and observe putative BNC‐1‐derived metabolites. The ability to perform fast analyses without sacrificing sensitivity or metabolic information suggests that this CZE–MS method is ideal for metabolomics‐inclusive, high‐throughput PK profiling.

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Quantitative analysis of tetrahydrocannabinol isomers and other toxicologically relevant drugs in blood

Mantinieks,

Di Rago,

Drummer

et al. 2023

Drug Testing and Analysis

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A multi‐analyte liquid chromatography‐tandem mass spectrometry (LC‐MS/MS) method is described, involving the separation of delta‐9‐tetrahydrocannabinol (delta‐9‐THC) and delta‐8‐THC in addition to other commonly encountered drugs and metabolites. Briefly, sample preparation involved an alkaline liquid–liquid extraction (methyl tert‐butyl ether) of blood (100 μl). The solvent layer was transferred, evaporated to dryness, reconstituted, and samples then separated on an Agilent Poroshell 120 EC‐C18 100 Å (50 mm × 3.0 mm, 2.7 μm) analytical column using a multi‐step gradient elution of 50 mM ammonium formate in water (pH 3.5) and 0.1% formic acid in methanol over 14 min. A SCIEX Triple Quad 6500+ system operating in scheduled multiple reaction monitoring and positive electrospray ionization was used for detection. There were no interferences, and matrix effects were generally acceptable (±20% of neat response). Linearity was achieved within the calibration range, including methylamphetamine (MA) (10–1000 ng/ml), 3,4‐methylenedioxy‐N‐methylamphetamine (MDMA) (10–1,000 ng/ml), cocaine (10–1000 ng/ml), and two THC isomers (1–100 ng/ml). Accuracies of MA, MDMA, cocaine, and two THC isomers were 3.6 to 8.9%, −1.2 to 4%, −5.3 to 5.8%, and −11 to 14%, respectively; while precision estimates of the same were 1.6 to 5.4%, 1.7 to 5.3%, 1.2 to 4.5%, and 2 to 10%, respectively. Autosampler stability and dilution integrity were within acceptable limits, and no carryover was detected at the limit of detection. This validated LC‐MS/MS method made the routine identification of both delta‐9‐THC and delta‐8‐THC in blood possible.

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Development and validation of an assay to measure cannabidiol and Δ9-tetrahydrocannabinol in human EDTA plasma by UHPLC-MS/MS

Cited by 17 publications

References 10 publications

A review on the recent advances in HPLC, UHPLC and UPLC analyses of naturally occurring cannabinoids (2010–2019)

A review on the recent advances in HPLC, UHPLC and UPLC analyses of naturally occurring cannabinoids (2010–2019)

Pharmacokinetic and metabolic analysis of an Alzheimer's disease therapeutic in rat serum via microfluidic CZE–MS

Quantitative analysis of tetrahydrocannabinol isomers and other toxicologically relevant drugs in blood

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