Quantitative evaluation of the matrix effect in bioanalytical methods based on LC–MS: A comparison of two approaches

Rudzki, Piotr J.; Gniazdowska, Elżbieta; Buś-Kwaśnik, Katarzyna

doi:10.1016/j.jpba.2018.03.052

Cited by 38 publications

(18 citation statements)

References 15 publications

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“…Extraction efficiency and matrix effect were determined by comparison of plasma spiked with analytes pre-and post-extraction, in conjunction with neat mobile phase (40:60 0.1% formic acid in water: methanol) spiked with analytes. 24,25 For each condition, (preextraction, post-extraction and mobile phase), six replicates were prepared at QCL, QCM and QCH concentrations.…”

Section: Extraction Efficiency and Matrix Effectmentioning

confidence: 99%

A validated method for the simultaneous quantification of cannabidiol, Δ⁹‐tetrahydrocannabinol, and their metabolites in human plasma and application to plasma samples from an oral cannabidiol open‐label trial

Kevin

Vogel

Doohan

et al. 2020

Drug Testing and Analysis

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Cannabidiol (CBD) and Δ9‐tetrahydrocannabinol (THC) are the two best known and most extensively studied phytocannabinoids within Cannabis sativa. An increasing number of preclinical studies and clinical trials have been conducted with one or both compounds, often probing their therapeutic effects in conditions such as paediatric epilepsy, anxiety disorders or chronic pain. Accurate monitoring of THC and CBD and their metabolites is essential for tracking treatment adherence and pharmacokinetics. However, fully validated methods for the comprehensive analysis of major Phase I CBD metabolites are yet to be developed due to a historical lack of commercially available reference material. In the present study, we developed, optimised and validated a method for the simultaneous quantification of CBD, THC and their major Phase I metabolites 6‐hydroxy‐CBD (6‐OH‐CBD), 7‐hydroxy‐CBD (7‐OH‐CBD), 7‐carboxy‐CBD (7‐COOH‐CBD), 11‐hydroxy‐tetrahydrocannabinol (11‐OH‐THC) and 11‐carboxy‐tetrahydrocannabinol (11‐COOH‐THC) as per Food and Drug Administration (FDA) guidelines for bioanalytical method validation. The method is accurate, reproducible, sensitive and can be carried out in high‐throughput 96‐well formats, ideal for larger scale clinical trials. Deuterated internal standards for each analyte were crucial to account for variable matrix effects between plasma lots. The application of the method to plasma samples, taken from people who had been administered oral CBD as part of an open‐label trial of CBD effects in anxiety disorders, demonstrated its immediate utility in ongoing and upcoming clinical trials. The method will prove useful for future studies involving CBD and/or THC and can likely accommodate the inclusion of additional metabolites as analytical reference materials become commercially available.

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Section: Extraction Efficiency and Matrix Effectmentioning

confidence: 99%

A validated method for the simultaneous quantification of cannabidiol, Δ⁹‐tetrahydrocannabinol, and their metabolites in human plasma and application to plasma samples from an oral cannabidiol open‐label trial

Kevin

Vogel

Doohan

et al. 2020

Drug Testing and Analysis

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“…Process efficiency and matrix effects: The total process efficiency (PE) was determined by comparing area counts of blank matrix fortified with low QC, and IS prior to sample processing were compared to area counts of "neat" sample containing low QC and IS in the elution solvent [18]. At least three replicates of three concentrations across the analytical measuring range were used for both sets.…”

Section: Qc Bias and Imprecisionmentioning

confidence: 99%

Validation of a liquid chromatography tandem mass spectrometry (LC-MS/MS) method to detect cannabinoids in whole blood and breath

Hubbard

Smith²,

Sobolesky

et al. 2019

Clinical Chemistry and Laboratory Medicine (CCLM)

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BackgroundThe widespread availability of cannabis raises concerns regarding its effect on driving performance and operation of complex equipment. Currently, there are no established safe driving limits regarding ∆9-tetrahydrocannabinol (THC) concentrations in blood or breath. Daily cannabis users build up a large body burden of THC with residual excretion for days or weeks after the start of abstinence. Therefore, it is critical to have a sensitive and specific analytical assay that quantifies THC, the main psychoactive component of cannabis, and multiple metabolites to improve interpretation of cannabinoids in blood; some analytes may indicate recent use.MethodsA liquid chromatography tandem mass spectrometry (LC-MS/MS) method was developed to quantify THC, cannabinol (CBN), cannabidiol (CBD), 11-hydroxy-THC (11-OH-THC), (±)-11-nor-9-carboxy-Δ9-THC (THCCOOH), (+)-11-nor-Δ9-THC-9-carboxylic acid glucuronide (THCCOOH-gluc), cannabigerol (CBG), and tetrahydrocannabivarin (THCV) in whole blood (WB). WB samples were prepared by solid-phase extraction (SPE) and quantified by LC-MS/MS. A rapid and simple method involving methanol elution of THC in breath collected in SensAbues® devices was optimized.ResultsLower limits of quantification ranged from 0.5 to 2 μg/L in WB. An LLOQ of 80 pg/pad was achieved for THC concentrations in breath. Calibration curves were linear (R2>0.995) with calibrator concentrations within ±15% of their target and quality control (QC) bias and imprecision ≤15%. No major matrix effects or drug interferences were observed.ConclusionsThe methods were robust and adequately quantified cannabinoids in biological blood and breath samples. These methods will be used to identify cannabinoid concentrations in an upcoming study of the effects of cannabis on driving.

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“…The potential impact of post mortem matrix-related effects on standard analytical methods and the interpretation of results are examples of issues relating to forensic toxicology (2), that is why, although the guide used as a reference for the validation of the qualitative method did not suggest the evaluation of the matrix effect, this parameter has been evaluated. Besides that, according to several authors (21)(22)(23), LC method coupled to the ESI ionization source suffers more influence of the matrix components. Table 3 shows the FMN obtained for the substances that presented CV% around 15, considered satisfactory.…”

Section: Matrix Effectmentioning

confidence: 99%

Development and validation of a LC-ESI-MS/MS method for simultaneous whole blood analysis of 51 new psychoactive substances

2019

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In recent years, there has been a great increase in seizures and forensic analysis of new psychotropic substances (NPS) in the state of Rio Grande do Sul. The analysis of these compounds needs to be performed in biological samples in cases of violent deaths. A sensitive and reliable liquid chromatography-tandem mass spectrometry with electrospray ionization interface (LC-ESI-MS/MS) method was developed and validated for qualitative analysis of 51 NPS in whole blood forensic samples. Synthetic cathinones, phenethylamines, opioids, tryptamines, synthetic cannabinoids, and other hallucinogens and stimulants were included in the method. The validation parameters assessed were speciﬁcity, limit of detection, retention time precision, and matrix effect. Drug free pools (n=6) were used for validation, including post mortem samples as well as from living individuals. Adulterants, pharmaceuticals, metabolites, and other illicit drugs, totalling 39 compounds, were analyzed and no interference was noticed. The detection limits obtained were suitable for evaluation at recreational and non-fatal levels of consumption, mostly. The results revealed an appropriate matrix effect in 24 out of 51 substances tested, indicating the potential for future quantitative analysis with this method for these drugs. The developed and validated method is easy to implement, fast, with low cost, and suitable for use in routine forensic toxicology laboratory analysis.

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Quantitative evaluation of the matrix effect in bioanalytical methods based on LC–MS: A comparison of two approaches

Cited by 38 publications

References 15 publications

A validated method for the simultaneous quantification of cannabidiol, Δ⁹‐tetrahydrocannabinol, and their metabolites in human plasma and application to plasma samples from an oral cannabidiol open‐label trial

A validated method for the simultaneous quantification of cannabidiol, Δ⁹‐tetrahydrocannabinol, and their metabolites in human plasma and application to plasma samples from an oral cannabidiol open‐label trial

Validation of a liquid chromatography tandem mass spectrometry (LC-MS/MS) method to detect cannabinoids in whole blood and breath

Development and validation of a LC-ESI-MS/MS method for simultaneous whole blood analysis of 51 new psychoactive substances

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Quantitative evaluation of the matrix effect in bioanalytical methods based on LC–MS: A comparison of two approaches

Cited by 38 publications

References 15 publications

A validated method for the simultaneous quantification of cannabidiol, Δ9‐tetrahydrocannabinol, and their metabolites in human plasma and application to plasma samples from an oral cannabidiol open‐label trial

A validated method for the simultaneous quantification of cannabidiol, Δ9‐tetrahydrocannabinol, and their metabolites in human plasma and application to plasma samples from an oral cannabidiol open‐label trial

Validation of a liquid chromatography tandem mass spectrometry (LC-MS/MS) method to detect cannabinoids in whole blood and breath

Development and validation of a LC-ESI-MS/MS method for simultaneous whole blood analysis of 51 new psychoactive substances

Contact Info

Product

Resources

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A validated method for the simultaneous quantification of cannabidiol, Δ⁹‐tetrahydrocannabinol, and their metabolites in human plasma and application to plasma samples from an oral cannabidiol open‐label trial

A validated method for the simultaneous quantification of cannabidiol, Δ⁹‐tetrahydrocannabinol, and their metabolites in human plasma and application to plasma samples from an oral cannabidiol open‐label trial