scholarly journals New Method for the Monitoring of Antidepressants in Oral Fluid Using Dried Spot Sampling

2021 ◽  
Vol 14 (12) ◽  
pp. 1284
Author(s):  
Sofia Soares ◽  
Tiago Rosado ◽  
Mário Barroso ◽  
Eugenia Gallardo

The increase in the consumption of antidepressants is a public health problem worldwide, as these are a class of compounds widely used in the treatment of several illnesses, such as depression and anxiety. This work aimed to develop and optimize a method for the quantification of a number of antidepressants and their metabolites (fluoxetine, venlafaxine, O-desmethylvenlafaxine, citalopram, sertraline, and paroxetine) in 100 µL of oral fluid using the dried saliva spots (DSS) sampling approach and gas chromatography coupled with tandem mass spectrometry (GC–MS/MS). The method was validated, presenting linearity within the studied range, with detection and quantification limits ranging between 10 and 100 ng/mL, and coefficients of determination (R2) of at least 0.99 for all analytes. Recoveries were between approximately 13 and 46%. The analysis of precision and accuracy presented acceptable coefficients of variation and relative errors, considering the criteria usually accepted in the validation of bioanalytical procedures. The method herein described is the first to be reported using DSS for the extraction of antidepressants, proving to be a sensitive, simple, and fast alternative to conventional techniques, and capable of being routinely applied in clinical and forensic toxicology scenarios.

Molecules ◽  
2021 ◽  
Vol 27 (1) ◽  
pp. 112
Author(s):  
Brian Rossi ◽  
Francesca Freni ◽  
Claudia Vignali ◽  
Cristiana Stramesi ◽  
Giancarlo Collo ◽  
...  

Sensitive and specific immunoassay screening methods for the detection of benzodiazepines in urine represent an important prerequisite for routine analysis in clinical and forensic toxicology. Moreover, emerging designer benzodiazepines force labs to keep their methodologies updated, in order to evaluate the reliability of the immunochemical techniques. This study aimed at evaluating the sensitivity and specificity of two different immunoassay methods for the detection of benzodiazepines in urine, through a comparison with the results obtained by a newly developed liquid chromatographic tandem mass spectrometric (LC-MS/MS) procedure. A cohort of authentic urine samples (N = 501) were processed, before and after a hydrolysis procedure, through two immunoassays and an LC-MS/MS method. The LC-MS/MS target procedure was optimized for monitoring 25 different molecules, among traditional and designer benzodiazepines, including some metabolites. At least one of the monitored substances was detected in 100 out of the 501 samples. A good specificity was observed for the two immunoassays (>0.99), independently of the cut-offs and the sample hydrolysis. The new kit demonstrated a fairly higher sensitivity, always higher than 0.90; in particular, a high cross-reactivity of the new immunoassay was observed for samples that tested positive for lorazepam and 7-aminoclonazepam. The two immunoassays appeared adequate to monitor not only traditional benzodiazepines but also new designer ones.


Metabolites ◽  
2021 ◽  
Vol 11 (8) ◽  
pp. 521
Author(s):  
Moritz Losacker ◽  
Michael Kraemer ◽  
Alexandra Philipsen ◽  
Kristina Duecker ◽  
Nadine Dreimueller ◽  
...  

In forensic toxicology, amphetamine intoxications represent one of the most common case groups and present difficult questions for toxicologists. Estimating the time of consumption and the current influence of the stimulant is particularly difficult when only total amphetamine concentrations are considered. Stereoselective analysis and the consideration of metabolites can provide valuable information to facilitate interpretation. An enantioselective liquid chromatography−tandem mass spectrometry (LC-MS/MS) method for detection of amphetamine, norephedrine and 4-hydroxyamphetamine was developed. Validation showed satisfactory selectivity, sensitivity, linearity (0.5–250 ng/mL), precision and accuracy for all enantiomers. The method was applied to a collective of 425 forensic serum samples and 30 serum samples from psychiatric inpatients stating their last time of amphetamine consumption. Norephedrine and 4-hydroxyamphetamine were detected more frequently at higher amphetamine concentrations and at lower amphetamine (R)/(S) concentration ratios, possibly indicating recent consumption. Mean (R)/(S) ratio of amphetamine was 1.14, whereas higher ratios (mean 1.36) were found for amphetamine concentrations below 100 ng/mL. The (R)/(S) ratios of psychiatric inpatients significantly correlated with the reported time intervals to last consumption. The use of amphetamine (R)/(S) ratios and the simultaneous detection of metabolites are promising factors that can facilitate estimation of consumption time and current impairment.


Author(s):  
Lin Lin ◽  
Piyadarsha Amaratunga ◽  
Jerome Reed ◽  
Pornkamol Huang ◽  
Bridget Lorenz Lemberg ◽  
...  

Abstract Quantitative analysis of Δ9-tetrahydrocannabinol (Δ9-THC) in oral fluid has gained increasing interest in clinical and forensic toxicology laboratories. New medicinal and/or recreational cannabinoid products require laboratories to distinguish different patterns of cannabinoid use. This study validated a high-performance liquid chromatography-tandem mass spectrometry method for 13 different cannabinoids, including (-)-trans-Δ8-tetrahydrocannabinol (Δ8-THC), (-)-trans-Δ9-tetrahydrocannabinol (Δ9-THC), cannabidiol (CBD), Δ9-tetrahydrocannabinolic acid-A (Δ9-THCA-A), cannabidiolic acid (CBDA), 11-hydroxy-Δ9-tetrahydrocannabinol (11-OH-Δ9-THC), 11-nor-9-carboxy-Δ9-tetrahydrocannabinol (Δ9-THCCOOH), tetrahydrocannabivarin (THCV), cannabidivarin (CBDV), cannabidiorcol (CBD-C1), cannabichromene (CBC), cannabinol (CBN) and cannabigerol (CBG), in oral fluid. Baseline separation was achieved in the entire quantitation range between Δ9-THC and its isomer Δ8-THC. The quantitation range of Δ9-THC, Δ8-THC and CBD was from 0.1 to 800 ng/mL. Two hundred human subject oral fluid samples were analyzed with this method after solid phase extraction. Among the 200 human subject oral fluid samples, all 13 cannabinoid analytes were confirmed in at least one sample. Δ8-THC was confirmed in 11 samples, with or without the presence of Δ9-THC. A high concentration of 11-OH-Δ9-THC or Δ9-THCCOOH (>400 ng/mL) was confirmed in three samples. CBD, Δ9-THCA-A, THCV, CBN and CBG were confirmed in 74, 39, 44, 107 and 112 of the 179 confirmed Δ9-THC-positive samples, respectively. The quantitation of multiple cannabinoids and metabolites in oral fluid simultaneously provides valuable information for revealing cannabinoid consumption and interpreting cannabinoid-induced driving impairment.


Author(s):  
Ana Carolina Furiozo Arantes ◽  
Kelly Francisco da Cunha ◽  
Marilia Santoro Cardoso ◽  
Karina Diniz Oliveira ◽  
Jose Luiz Costa

Abstract Purpose We developed and validated a method for quantitative analysis of 50 psychoactive substances and metabolites (antidepressants, benzodiazepines and opioids) in oral fluid samples using simple liquid–liquid extraction procedure followed by liquid chromatography–tandem mass spectrometry (LC–MS/MS). Method Oral fluid samples were collected using Quantisal™ device and extracted by liquid–liquid extraction with 1.0 mL of methyl tert-butyl ether and then analyzed using LC–MS/MS. Results The method attended method validation criteria, with limits of quantification as low as 0.5 and 1.0 ng/mL, and linearity between 0.5–50.0 ng/mL for antidepressants, 0.5–25.0 ng/mL for benzodiazepines and 1.0–50.0 ng/mL to opioids. During method validation, bias and imprecision values were not greater than 16 and 20%, respectively. Ionization suppression/enhancement bias results were not greater than 25%. No evidence of carryover was observed. Sample stability studies showed that almost all analytes were stable at 25 °C for 3 days and at 4 °C for 7 days. Freeze–thaw cycles stability showed that most antidepressants and opioids were stable under these conditions. Autosampler stability study showed that all analytes were stable for 24 h, except for nitrazepam and 7-aminoclonazepam. Thirty-eight authentic oral fluid samples were analyzed; 36.8% of the samples were positive for 2 drugs. Citalopram was the most common drug found, followed by venlafaxine. Conclusions The method was validated according to international recommendations for the 50 analytes, showing low limits of quantification, good imprecision and bias values, using simple liquid–liquid extraction, and was successfully applied to authentic oral fluid samples analysis.


2011 ◽  
Vol 83 (8) ◽  
pp. 2897-2905 ◽  
Author(s):  
Sara C. McGrath ◽  
David M. Schieltz ◽  
Lisa G. McWilliams ◽  
James L. Pirkle ◽  
John R. Barr

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