Analysis of cannabinoids in oral fluid by liquid chromatography–tandem mass spectrometry

Fabritius, Marie; Staub, Christian; Mangin, Patrice; Giroud, Christian

doi:10.1007/s11419-012-0168-z

Cited by 29 publications

(38 citation statements)

References 49 publications

(59 reference statements)

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“…On the other hand, THC and its metabolites are only poorly excreted from the blood and tissues into this matrix. In line with these observations, analysis of OF revealed very high concentrations of THC in OF just after cannabis smoking, while 11-hydroxy-THC (11-OH-THC) was not detected and only trace amounts of 11-nor-9-carboxy-THC (THCCOOH) were measured [8]. Studies that used intravenous administration of THC have suggested that the transfer of THC from the blood into OF is limited [9].…”

Section: Introductionmentioning

confidence: 63%

“…Analyses of OF samples were performed according to a previously published procedure [8]. The collection devices were weighed before and after OF sampling to determine the quantity of OF collected.…”

Section: Methods Of Analysismentioning

confidence: 99%

“…Since THCCOOH is not found in cannabis plants, neither in joints nor in cannabis smoke, its presence in OF could result only from human metabolism. THCOOH is very likely poorly excreted from the plasma into the saliva as a free molecule [8]. Its concentration in OF is related to that found in plasma.…”

Section: μG/l)mentioning

confidence: 99%

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Comparison of cannabinoid concentrations in oral fluid and whole blood between occasional and regular cannabis smokers prior to and after smoking a cannabis joint

et al. 2013

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A cross-over controlled administration study of smoked cannabis was carried out on occasional and heavy smokers. The participants smoked a joint (11 % Δ9-tetrahydrocannabinol (THC)) or a matching placebo on two different occasions. Whole blood (WB) and oral fluid (OF) samples were collected before and up to 3.5 h after smoking the joints. Pharmacokinetic analyses were obtained from these data. Questionnaires assessing the subjective effects were administered to the subjects during each session before and after the smoking time period. THC, 11-hydroxy-THC (11-OH-THC) and 11-nor-9-carboxy-THC (THCCOOH) were analyzed in the blood by gas chromatography or liquid chromatography (LC)-tandem mass spectrometry (MS/MS). The determination of THC, THCCOOH, cannabinol (CBN), and Δ9-tetrahydrocannabinolic acid A (THC-A) was carried out on OF only using LC-MS/MS. In line with the widely accepted assumption that cannabis smoking results in a strong contamination of the oral cavity, we found that THC, and also THC-A, shows a sharp, high concentration peak just after smoking, with a rapid decrease in these levels within 3 h. No obvious differences were found between both groups concerning THC median maximum concentrations measured either in blood or in OF; these levels were equal to 1,338 and 1,041 μg/L in OF and to 82 and 94 μg/L in WB for occasional and heavy smokers, respectively. The initial WB THCCOOH concentration was much higher in regular smokers than in occasional users. Compared with the occasional smokers, the sensation of confusion felt by the regular smokers was much less while the feeling of intoxication remained almost unchanged.

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Section: Introductionmentioning

confidence: 63%

Section: Methods Of Analysismentioning

confidence: 99%

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Comparison of cannabinoid concentrations in oral fluid and whole blood between occasional and regular cannabis smokers prior to and after smoking a cannabis joint

et al. 2013

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“…This makes THC a drug of abuse and correct identification of this compound is thus important from a forensic point of view. The two cannabinoids, can be separated using chromatographic or electrophoretic methods, such as planar chromatography [35], LC-UV [36], LC-MS(MS) [37,38], CE-LED-induced fluorescence detection [39], which require a considerable analysis time (5-30 min). In the present study, we studied the potential of TIMS for the fast separation of THC and CBD.…”

Section: Separation Of Isomers Employing Cation Adduct Formationmentioning

confidence: 99%

Adduct-ion formation in trapped ion mobility spectrometry as a potential tool for studying molecular structures and conformations

Zietek

Mengerink

Jordens

et al. 2017

Int. J. Ion Mobil. Spec.

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Recent developments in the field of ion mobility spectrometry provide new possibilities to explore and understand gas-phase ion chemistry. In this study, hyphenated trapped ion mobility spectrometry-mass spectrometry (TIMS-MS) was applied to investigate analyte ion mobility as function of adduct ion formation for twelve pharmaceutically relevant molecules, and for tetrahydrocannabinol (THC) and its isomer cannabidiol (CBD). Samples were introduced by direct infusion and ions were generated with positive electrospray ionization (ESI+) observing protonated and sodiated ions. Measurements were performed with and without addition of cesium-, lithium-, silver-and sodium ions to the samples. For the tested compounds, metal adduct ions with the same m/z but with different mobility and collision cross section (CCSs) were observed, indicating different molecular conformations. Formation of analyte dimers was also observed, which could be associated with molecular geometry of the compounds. By optimizing the range and speed of the electric field gradient and ramp, respectively, the separation of THC and CBD was achieved by employing the adduct formation. This study demonstrates that the favorable resolution of TIMS combined with the ability to detect weakly bound counter ions is a valuable means for rapid detection, separation and structural assignment of molecular isomers and analyte conformations.

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“…The use of LC-MS/MS eliminates the need of costly and time-consuming alkaline and/ or enzymatic glucuronide hydrolysis, enabling direct measurement of free and glucuronidated THCCOOH. As native and isotopically labeled THCCOOH-glucuronide standards have become available only recently, few LC-MS/MS for quantifying THCCOOH-glucuronide in biological fluids exist [25,[29][30][31][32][33]. Schwope et al [25] and Gronewold et al [31] reported the only two existing methods for simultaneously measuring free and glucuronidated THCCOOH in whole blood, along with free and glucuronidated THC, 11-OH-THC, cannabinol and cannabidiol.…”

Section: Introductionmentioning

confidence: 99%

Development of a rapid column-switching LC-MS/MS method for the quantification of THCCOOH and THCCOOH-glucuronide in whole blood for assessing cannabis consumption frequency

et al. 2016

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The concentration of 11-nor-9-carboxy-Δ 9 -tetrahydrocannabinol (THCCOOH) in whole blood is used as a parameter for assessing the consumption behavior of cannabis consumers. The blood level of THCCOOH-glucuronide might provide additional information about the frequency of cannabis use. To verify this assumption a column-switching liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the rapid and direct quantification of free and glucuronidated THCCOOH in human whole blood was newly developed. The method comprised protein precipitation, followed by injection of the processed sample onto a trapping column and subsequent gradient elution to an analytical column for separation and detection. The total LC run time was 4.5 min. Detection of the analytes was accomplished by electrospray ionization in positive ion mode and selected reaction monitoring using a triple stage quadrupole mass spectrometer. The method was fully validated by evaluating the following parameters: linearity, lower limit of quantification, accuracy and imprecision, selectivity, extraction efficiency, matrix effect, carry-over, dilution integrity, analyte stability and re-injection reproducibility. All acceptance criteria were analyzed and the predefined criteria met. Linearity ranged from 5.0 -500 µg/L for both analytes. The method was successfully applied to whole blood samples from a large collective of cannabis consumers, demonstrating its applicability in the forensic field.

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Analysis of cannabinoids in oral fluid by liquid chromatography–tandem mass spectrometry

Cited by 29 publications

References 49 publications

Comparison of cannabinoid concentrations in oral fluid and whole blood between occasional and regular cannabis smokers prior to and after smoking a cannabis joint

Comparison of cannabinoid concentrations in oral fluid and whole blood between occasional and regular cannabis smokers prior to and after smoking a cannabis joint

Adduct-ion formation in trapped ion mobility spectrometry as a potential tool for studying molecular structures and conformations

Development of a rapid column-switching LC-MS/MS method for the quantification of THCCOOH and THCCOOH-glucuronide in whole blood for assessing cannabis consumption frequency

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