11-Year Study of Fentanyl in Driving Under the Influence of Drugs (DUID) Casework

2021 ◽  
Author(s):  
Ayako Chan-Hosokawa ◽  
Jolene J Bierly
Keyword(s):  
Drug Class ◽  
Driving Under The Influence ◽  
Prescription Opioids ◽  
Blood Concentrations ◽  
Chromatography Tandem Mass Spectrometry ◽  
Percent Positivity ◽  
Limit Of Quantitation ◽  
Liquid Chromatography Tandem Mass ◽  
Information Change ◽  
Concentration Patterns

Abstract Prior to 2017, heroin and other prescription opioids were the most prevalent opioids implicated in driving under the influence of drugs (DUID) investigation cases and fentanyl was rarely included in the scope of toxicological analysis. Fentanyl has become the most frequently identified opioid in DUID cases with many suspected heroin cases turning out to be only fentanyl. A review of fentanyl positive DUID cases at NMS Labs was performed to provide prevalence information, change in concentration, patterns of combined drug use, indicators of impairment, and driving behavior in order to assist with toxicological interpretation of DUID scenarios involving fentanyl. Fentanyl positive DUID cases received between January 2010 and December 2020 were examined. Blood results were confirmed and quantitated for fentanyl, norfentanyl and acetylfentanyl using a liquid chromatography–tandem mass spectrometry (LC–MS-MS) analysis with a limit of quantitation (LOQ) of 0.10, 0.20 and 0.10 ng/mL, respectively. Of 153,234 blood cases examined for DUID over 11 years, fentanyl confirmed positive in 6,779 (4.4%) cases. However, there were significant changes in positivity over time. Fentanyl percent positivity increased from 0.60% in 2010 to 12% in 2020. Of 5,976 confirmed fentanyl positive cases in 2018 through 2020, blood concentrations greater than 4.0 ng/mL were observed in 44% (2018), 55% (2019), and 59% (2020) of cases. Polypharmacy was common with 87% of blood samples confirming positive for fentanyl and at least one other compound. Stimulants was the most commonly identified drug class in cases where at least one additional drug class was present. This study illustrates the importance of including fentanyl in a routine blood DUID panel.

scholarly journals Determination of Tissue Distribution of Alisol G, a CB1R Antagonist, in Rats by Ultra-High-Performance Liquid Chromatography-Tandem Mass Spectrometry

2021 ◽  
Author(s):  
Chen-Yu Gao ◽  
Jian-Qiang Xi ◽  
Ding-Zhong Song ◽  
Jie Yuan ◽  
Wu-Si Hao ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
High Performance ◽  
Tandem Mass ◽  
Blood Concentrations ◽  
Therapeutic Benefits ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass

AbstractPeripheral CB1R blockers without crossing the blood–brain barrier (BBB) have demonstrated therapeutic benefits in metabolic syndromes, including obesity. Among them is Alisol G, a tetracyclic triterpene from Alismatis rhizoma (zexie), which can effectively reduce the weight of obese mice. Results from CP55940-induced [35S] GTPγS cannabinoid-type 1 receptor (CB1R) binding assay show an IC50 of 34.8 μmol/L for Alisol G, implicating its role as a CB1R antagonist. The purpose of our study is to assess whether Alisol G could serve as a peripheral CB1R antagonist for obesity treatment. In this study, we build a simple, reliable, and sensitive method to detect the concentration of Alisol G in rat tissue by ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). The results showed that Alisol G was mainly distributed in intestinal midgut, mucosa and small intestine, with little brain exposure. We suggested that intestine may be the main acting sites of Alisol G. Through comparison of brain and blood concentrations of Alisol G, our data showed that Alisol G cannot penetrate the BBB easily. In conclusion, Alisol G may represent a peripheral CB1R antagonist for the further treatment of obesity.

scholarly journals Development of a method for the measurement of dehydroepiandrosterone sulphate by liquid chromatography-tandem mass spectrometry

2005 ◽  
Vol 42 (6) ◽  
pp. 468-474 ◽  
Author(s):  
C A Chadwick ◽  
L J Owen ◽  
B G Keevil
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Lower Limit ◽  
Internal Standard ◽  
Tandem Mass ◽  
Dehydroepiandrosterone Sulphate ◽  
Chromatography Tandem Mass Spectrometry ◽  
Limit Of Quantitation ◽  
Liquid Chromatography Tandem Mass

Background: Dehydroepiandrosterone sulphate (DHEAS) is a steroid that is increasingly being recognized as a potential drug of abuse in many countries. This is due to its reputation as a hormone that may be able to retard the ageing process. The measurement of DHEAS is useful in the diagnosis of medical conditions such as congenital adrenal hyperplasia and polycystic ovary syndrome. Thus, a liquid chromatography-tandem mass spectrometry method has been developed to determine DHEAS concentrations in human serum. Method: The chromatography was performed using a WatersTM 2795 Alliance HT LC system coupled to a Mercury Fusion-RP column fitted with a SecurityGuardTM column. Results: DHEAS and the internal standard, deuterated DHEAS, both had a retention time of 1.5 min. The transition determined by the Micromass QuattroTM tandem mass spectrometer for DHEAS was m/z 367.3>96.7 and for the internal standard m/z 369.3>96.6. The method was linear up to 20 µmol/L; the lower limit of detection and the lower limit of quantitation were both 1 µmol/L. The intra- and interassay imprecision were <11% over a concentration range of 1-18 µmol/L for the in-house quality control and <12% for the intra- and interassay imprecision for the Bio-Rad Lyphocheck QC. Conclusion: The measurement of DHEAS by liquid chromatography-tandem mass spectrometry is robust and has a simple sample preparation procedure with a rapid cycle time of only 4 min.

scholarly journals Dried Urine Microsampling Coupled to Liquid Chromatography—Tandem Mass Spectrometry (LC–MS/MS) for the Analysis of Unconjugated Anabolic Androgenic Steroids

Molecules ◽  
2020 ◽  
Vol 25 (14) ◽  
pp. 3210 ◽  
Author(s):  
Michele Protti ◽  
Camilla Marasca ◽  
Marco Cirrincione ◽  
Angelo E. Sberna ◽  
Roberto Mandrioli ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Anabolic Androgenic Steroids ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
Liquid Chromatography Tandem Mass ◽  
Androgenic Steroids

Testing and monitoring anabolic androgenic steroids in biological fluids is a key activity in anti-doping practices. In this study, a novel approach is proposed, based on dried urine microsampling through two different workflows: dried urine spots (DUS) and volumetric absorptive microsampling (VAMS). Both techniques can overcome some common drawbacks of urine sampling, such as analyte instability and storage and transportation problems. Using an original, validated liquid chromatography–tandem mass spectrometry (LC-MS/MS) method, exogenous and endogenous unconjugated steroids were analysed. Despite the limitations of microsampling volume, good sensitivity was obtained (limit of quantitation ≤1.5 ng/mL for all analytes), with satisfactory precision (relative standard deviation <7.6%) and absolute recovery (>70.3%). Both microsampling platforms provide reliable results, in good agreement with those obtained from urine.

Method Validation of Seven Synthetic Cathinones by LC–MS-MS Analysis and the Prevalence of N-Ethylpentylone in Postmortem Casework

2020 ◽  
Author(s):  
Alexander D Giachetti ◽  
Joseph H Kahl ◽  
M Elizabeth Zaney ◽  
George W Hime ◽  
Diane M Boland
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Solid Phase ◽  
Synthetic Cathinones ◽  
Medical Examiner ◽  
Tandem Mass ◽  
Blood Concentrations ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass

Abstract N-ethylpentylone (NEP, ephylone, bk-EBDP) was the most prevalent synthetic cathinone detected by the Miami-Dade Medical Examiner Toxicology Laboratory from 2016 to 2018. There is limited information regarding the toxicity of NEP; however, the few published reports suggest that NEP can cause serious toxic effects and sudden death. The purpose of this publication is to describe a validated liquid chromatography-tandem mass spectrometry (LC–MS-MS) method for seven synthetic cathinones (methylone, ethylone, butylone, dibutylone, alpha-Pyrrolidinopentiophenone (α-PVP), pentylone and NEP) and to present a detailed summary regarding the presence of NEP in postmortem casework at the Miami-Dade Medical Examiner Department. Postmortem iliac blood, serum, liver and brain specimens were prepared by solid-phase extraction with analysis by ultra-high-performance liquid chromatography-tandem mass spectrometry. Analyte linearity was established from 0.01 to 0.5 mg/L on a six-point calibration curve. A total of 101 NEP quantitations were performed using this method. Concentrations in postmortem case samples ranged from 0.01 to 2.7 mg/L. Iliac blood concentrations averaged 0.312 mg/L with a median of 0.137 mg/L (n = 72) across all causes and manners of death. Approximately half of the cases were homicides in which the decedent was the victim of gunshot wounds or stabbing. Two of the three highest concentration cases of NEP (2.7 and 1.7 mg/L) involved 38-year-old white males who were tasered by police prior to death. The psychostimulant effect of NEP may result in an excited delirium and/or hallucinogenic state. The concentration of NEP detected in accidental intoxication and polydrug cases overlapped with those attributed to other causes, including homicides and police-involved deaths.

scholarly journals Reliable and Easy-To-Use Liquid Chromatography-Tandem Mass Spectrometry Assay for Quantification of Olorofim (F901318), a Novel Antifungal Drug, in Human Plasma and Serum

2018 ◽  
Vol 62 (11) ◽  
Author(s):  
Carsten Müller ◽  
Cornelia Fietz ◽  
Philipp Koehler ◽  
Graham Sibley ◽  
Achu Che Awah Nforbugwe ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Human Plasma ◽  
Antifungal Drug ◽  
Selected Reaction Monitoring ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Limit Of Quantitation ◽  
Liquid Chromatography Tandem Mass

ABSTRACT A fast and easy-to-use liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the determination and quantification of a novel antifungal drug, olorofim (F901318), a member of the novel class of orotomides, in human plasma and serum was developed and validated. Sample preparation was based on protein precipitation with acetonitrile and subsequent centrifugation. An isotope-labeled analogue of F901318 was employed as an internal standard. Chromatographic separation was achieved using a 50-mm by 2.1-mm, 1.9-μm, polar Hypersil Gold C18 column and isocratic mobile phase consisting of 0.1% formic acid–acetonitrile (60%-40%, vol/vol) at a flow rate of 330 μl/min. The analyte was detected using a triple-stage quadrupole mass spectrometer operated in selected reaction monitoring (SRM) mode with positive heated electrospray ionization (HESI+) within a single runtime of 2.00 min. The present LC-MS/MS method was validated according to the international guidelines of the International Conference on Harmonisation (ICH) and the U.S. Food and Drug Administration (FDA). Linearity of F901318 concentration ranges was verified by the Mandel test. The calibration curve was tested linear across the range and fitted using least-squares regression with a weighting factor of the reciprocal concentration. The limit of detection was 0.0011 mg/liter, and the lower limit of quantitation was 0.0033 mg/liter. Intraday and interday precisions ranged from 1.17% to 3.23% for F901318, and intraday and interday accuracies (percent bias) ranged from 0.75% to 5.01%. In conclusion, a method was established for the rapid quantitation of F901318 concentrations in serum and plasma samples in patient trials, and it optimizes therapeutic drug monitoring in applying an easy-to-use single method.

scholarly journals Blood Concentrations of Designer Benzodiazepines: Relation to Impairment and Findings in Forensic Cases

2020 ◽  
Vol 44 (8) ◽  
pp. 905-914 ◽  
Author(s):  
Gunhild Heide ◽  
Gudrun Høiseth ◽  
Gerrit Middelkoop ◽  
Åse Marit Leere Øiestad
Keyword(s):  
High Performance ◽  
Clinical Test ◽  
Concentration Data ◽  
Criminal Offenders ◽  
Blood Concentrations ◽  
Blood Samples ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass ◽  
The Relationship ◽  
Designer Benzodiazepines

Abstract The use of designer benzodiazepines appears to be increasing in many countries, but data concerning blood concentrations are scarce, making interpretation of concentrations difficult. The aim of this study was to report blood concentrations of clonazolam, diclazepam, etizolam, flualprazolam, flubromazepam, flubromazolam and phenazepam and to investigate the relationship between blood concentrations and impairment. The concentration data are from blood samples collected from living cases (apprehended drivers and other drug offences) and medico-legal autopsies. The blood samples were analysed for the seven designer benzodiazepines mentioned above by ultra high performance liquid chromatography–tandem mass spectrometry. Positive cases from between 1 June 2016 and 30 September 2019 were included. Blood concentrations and the conclusion from a clinical test of impairment (when available) are reported. The presented seven benzodiazepines were detected in a total of 575 cases, where 554 of these cases concerned apprehended drivers or other criminal offenders. The number of findings and the median (range) concentrations were as follows: clonazolam, n = 22, 0.0041 mg/L (0.0017–0.053 mg/L); diclazepam, n = 334, 0.0096 mg/L (0.0016–0.25 mg/L); etizolam, n = 40, 0.054 mg/L (0.015–0.30 mg/L); flualprazolam, n = 10, 0.0080 mg/L (0.0033–0.056 mg/L); flubromazepam, n = 5, 0.037 mg/L (0.0070–0.70 mg/L); flubromazolam, n = 20, 0.0056 mg/L (0.0004–0.036 mg/L); and phenazepam, n = 138, 0.022 mg/L (0.0018–0.85 mg/L). A designer benzodiazepine was the only drug detected with relevance for impairment in 25 of the 554 living cases. The physician concluded with impairment in 19 of the 25 cases. Most of the concentrations in these cases were relatively similar to or higher than the median reported concentrations. The most frequent other drugs detected were amphetamine, tetrahydrocannabinol, clonazepam and methamphetamine. The presented blood concentrations can be helpful with the interpretation of cases involving one or more of these seven benzodiazepines. The results indicate that concentrations commonly observed in forensic cases are associated with impairment.

Novel and Nonroutine Benzodiazepines and Suvorexant by LC–MS-MS

2020 ◽  
Author(s):  
Luke Garcia ◽  
Nicholas B Tiscione ◽  
Dustin Tate Yeatman ◽  
Lauren Richards-Waugh
Keyword(s):  
Quantitative Analysis ◽  
Limit Of Detection ◽  
Sample Volume ◽  
Calibration Model ◽  
Tandem Mass ◽  
Palm Beach County ◽  
Chromatography Tandem Mass Spectrometry ◽  
Target Analytes ◽  
Limit Of Quantitation ◽  
Liquid Chromatography Tandem Mass

ABSTRACT Benzodiazepines are a commonly prescribed class of drugs that have the potential for abuse. The Palm Beach County Sheriff’s Office received drug seizure submissions that included novel and/or nonroutine benzodiazepines of increasing prevalence from 2017 to 2019. This prompted the development of a method of analysis for these compounds in biological specimens. The method tests for 16 novel and nonroutine benzodiazepines and suvorexant in whole blood by liquid chromatography–tandem mass spectrometry (LC–MS-MS). The target analytes included bromazepam, clobazam, clonazolam, clotiazepam, diclazepam, estazolam, etizolam, flualprazolam, flubromazepam, flubromazolam, loprazolam, lormetazepam, phenazepam, prazepam, suvorexant, tetrazepam and triazolam. The method uses 200 µL of sample, protein precipitation and an instrument run-time of 8 min. The limit of detection was either 1 or 5 ng/mL and the limit of quantitation was either 5 or 25 ng/mL depending on the analyte. The method was validated for quantitative analysis for 15 out of the 17 analytes. Flubromazepam and prazepam were validated for qualitative identification only. A quadratic calibration model (r2 &gt; 0.990) with 1/x weighting was used for all analytes for quantitative analysis. The calibration range was either 5–100 or 25–500 ng/mL depending on the analyte. The coefficient of variation of replicate analyses was within 14% and bias was within ±14%. The method provides a sensitive, efficient and robust procedure for the quantitation and/or qualitative identification of select novel and nonroutine benzodiazepines and suvorexant using LC–MS-MS and a sample volume of 200 µL.

scholarly journals Determination of Cyclamate in Foods by Ultraperformance Liquid Chromatography/Tandem Mass Spectrometry

2008 ◽  
Vol 91 (5) ◽  
pp. 1095-1102 ◽  
Author(s):  
Robert Sheridan ◽  
Thomas King
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Sample Preparation ◽  
Tandem Mass Spectrometry ◽  
Limit Of Detection ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Limit Of Quantitation ◽  
Liquid Chromatography Tandem Mass

Abstract A highly sensitive and selective method that requires minimal sample preparation was developed for the confirmation and quantitation of cyclamate in a variety of foods by high-performance liquid chromatography/tandem mass spectrometry (HPLC/MS/MS). Sample preparation consisted of homogenization followed by extraction and dilution of cyclamate with water. HPLC separation was achieved using a bridged ethyl hybrid C18 high-pressure column with a mobile phase consisting of 0.15 acetic acid and methanol. Under electrospray ionization negative conditions, quantitation was achieved by monitoring the fragment m/z 79.7 while also collecting parent ion m/z 177.9. Two food matrixes, diet soda and jelly, were subjected to a validation procedure in order to evaluate the applicability of the method. The cyclamate limit of detection for both matrixes was determined to be 0.050 g/g with a limit of quantitation of 0.150 g/g. The correlation coefficient of the calibration curves was &gt;0.9998 from 0.0005 to 0.100 g/mL. The method has been used for the determination of cyclamate in several foods and the results are presented.

scholarly journals Analysis of Nicotine Metabolites in Hair and Nails Using QuEChERS Method Followed by Liquid Chromatography–Tandem Mass Spectrometry

Molecules ◽  
2020 ◽  
Vol 25 (8) ◽  
pp. 1763
Author(s):  
Junhee Kim ◽  
Hyun-Deok Cho ◽  
Joon Hyuk Suh ◽  
Ji-Youn Lee ◽  
Eunyoung Lee ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Clinical Samples ◽  
Tandem Mass ◽  
Analytical Sensitivity ◽  
Quechers Method ◽  
Chromatography Tandem Mass Spectrometry ◽  
Limit Of Quantitation ◽  
Liquid Chromatography Tandem Mass

Many studies have analyzed nicotine metabolites in blood and urine to determine the toxicity caused by smoking, and assess exposure to cigarettes. Recently, hair and nails have been used as alternative samples for the evaluation of smoking, as not only do they reflect long-term exposure but they are also stable and easy to collect. Liquid-liquid or solid-phase extraction has mainly been used to detect nicotine metabolites in biological samples; however, these have disadvantages, such as the use of toxic organic solvents and complex pretreatments. In this study, a modified QuEChERS method was proposed for the first time to prepare samples for the detection of nicotine metabolite cotinine (COT) and trans-3′-hydroxycotinine (3-HCOT) in hair and nails. High-performance liquid chromatography–tandem mass spectrometry (LC–MS/MS) was used to analyze traces of nicotine metabolites. The established method was validated for selectivity, linearity, lower limit of quantitation, accuracy, precision and recovery. In comparison with conventional liquid-liquid extraction (LLE), the proposed method was more robust, and resulted in higher recoveries with favorable analytical sensitivity. Using this method, clinical samples from 26 Korean infants were successfully analyzed. This method is expected to be applicable in the routine analysis of nicotine metabolites for environmental and biological exposure monitoring.

scholarly journals Liquid Chromatography/Tandem Mass Spectrometry Method for Quantitation of Cremophor EL and Its Applications

2013 ◽  
Vol 2013 ◽  
pp. 1-11 ◽  
Author(s):  
V. Vijaya Bhaskar ◽  
Anil Middha
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Rat Plasma ◽  
Polypropylene Glycol ◽  
Tandem Mass ◽  
Cremophor El ◽  
Chromatography Tandem Mass Spectrometry ◽  
Limit Of Quantitation ◽  
Liquid Chromatography Tandem Mass

A rapid sensitive and selective MRM based method for the determination of Cremophor EL (CrEL) in rat plasma was developed using liquid chromatography/tandem mass spectrometry (LC-MS/MS). CrEL and polypropylene glycol (internal standard) were extracted from rat plasma with acetonitrile and analysed on C18 column (XBridge, 50 × 4.6 mm, 3.5 μm). The most abundant molecular ions corresponding to PEG oligomers atm/z828, 872, 916 and 960 with daughter ion atm/z89 were selected for multiple reaction monitoring (MRM) in electrospray mode of ionisation. Plasma concentrations of CrEL were quantified after administration through oral and intravenous routes in male sprague dawley rats at a dose of 0.26 g/kg. The standard curve was linear (0.9972) over the concentration range of 1.00 to 200 μg/mL. The lower limit of quantitation for CrEL was 1.00 μg/mL using 50 μL plasma. The coefficient of variation and relative error for inter and intra assay at three QC levels were 0.69 to 9.21 and −7.60 to 4.74 respectively. A novel proposal was conveyed to the scientific community, where formulation excipient can be analysed as qualifier in the analysis of NCEs to address the spiky plasma concentration profiles.

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