A Comprehensive HPLC–MS-MS Screening Method for 77 New Psychoactive Substances, 24 Classic Drugs and 18 Related Metabolites in Blood, Urine and Oral Fluid

2020 ◽  
Vol 44 (8) ◽  
pp. 769-783
Author(s):  
Annagiulia Di Trana ◽  
Giulio Mannocchi ◽  
Filippo Pirani ◽  
Nunzia La Maida ◽  
Massimo Gottardi ◽  
...  
Keyword(s):  
Mobile Phase ◽  
Oral Fluid ◽  
Multiple Reaction Monitoring ◽  
Screening Method ◽  
Internal Standard ◽  
New Psychoactive Substances ◽  
Spectrometric Analysis ◽  
Blood Proteins ◽  
Psychoactive Substances ◽  
Better Than

Abstract To date, more than 800 molecules are classified as New Psychoactive Substances (NPS), and it is reported that this number increases every year. Whereas several cases of polydrug consumption that led to acute intoxication and death are reported, a lack of effective analytical screening method to detect NPS and classical drug of abuse in human matrices affects the prompt identification of the probable cause of intoxication in emergency department of hospitals. In this concern, a fast, simple and comprehensive high-performance liquid chromatography–tandem mass spectrometry (HPLC–MS-MS) screening method to detect and quantify 77 NPS, 24 classic drugs and 18 related metabolites has been successfully developed and validated in blood, urine and oral fluid. A small volume (100 µL) of whole blood samples spiked with internal standard deuterated mixture was added to 70 µL of M3® buffer, and after precipitation of blood proteins, the supernatant was evaporated to dryness and reconstituted in 1 mL of mobile phase. Same volume (100 µL) of urine and oral fluid samples spiked with internal standard deuterated mix were only diluted with 500 µL of M3® reagent. One microliter of samples of each matrix was injected into HPLC–MS-MS equipment. The run time lasted 10 min with a gradient mobile phase. Mass spectrometric analysis was performed in positive ion multiple reaction monitoring mode. The method was linear for all analytes under investigation with a determination coefficient always better than 0.99. The calibration range for blood and oral fluid was from limits of quantification (LOQs) to 200 ng/mL, whereas that for urine was LOQs to 1000 ng/mL. Recovery and matrix effect were always higher than 80%, whereas intra-assay and inter-assay precision were always better than 19% and accuracy was always within 19% of target in every matrix. Applicability of the method was verified by analysis of samples from real cases.

Screening of 104 New Psychoactive Substances (NPS) and Other Drugs of Abuse in Oral Fluid by LC–MS-MS

2020 ◽  
Vol 44 (7) ◽  
pp. 697-707
Author(s):  
Kelly Francisco da Cunha ◽  
Karina Diniz Oliveira ◽  
Marilyn A Huestis ◽  
Jose Luiz Costa
Keyword(s):  
Oral Fluid ◽  
Drugs Of Abuse ◽  
Matrix Effects ◽  
Synthetic Cannabinoids ◽  
Screening Method ◽  
Simultaneous Detection ◽  
New Psychoactive Substances ◽  
Major Public Health Problem ◽  
Psychoactive Substances ◽  
Wide Range

Abstract New psychoactive substances (NPS) are a major public health problem, primarily due to the increased number of acute poisoning cases. Detection of these substances is a challenge. The aim of this research was to develop and validate a sensitive screening method for 104 drugs of abuse, including synthetic cannabinoids, synthetic cathinones, fentanyl analogues, phenethylamines and other abused psychoactive compounds (i.e., THC, MDMA, LSD and their metabolites) in oral fluid by liquid chromatography–tandem mass spectrometry (LC–MS-MS). The Quantisal™ oral fluid device was used to collect oral fluid samples. The oral fluid–elution buffer mixture (500-μL sample) was extracted with t-butyl methyl ether, and chromatographic separation was performed on a Raptor™ biphenyl column (100 × 2.1 mm ID, 2.7 μm), with a total run time of 13.5 min. Limits of detection were established at three concentrations (0.05, 0.1 or 1 ng/mL) for most analytes, except for acetyl norfentanyl and mescaline (5 ng/mL). Matrix effects were generally <20% and overall extraction recoveries >60%. The highest matrix effect was observed within the synthetic cannabinoid group (PB22, −55.5%). Lower recoveries were observed for 2C-T (47.2%) and JWH-175 (58.7%). Recoveries from the Quantisal™ device were also evaluated for all analytes (56.7–127%), with lower recoveries noted for 25I-NBOMe, valerylfentanyl and mCPP (56.7, 63.0 and 69.9%, respectively). Drug stability in oral fluid was evaluated at 15, 60 and 90 days and at 25, 4 and −20°C. As expected, greater stability was observed when samples were stored at −20°C, but even when frozen, some NPS (e.g., synthetic cannabinoids) showed more than 20% degradation. The method was successfully applied to the analysis of seven authentic oral fluid samples positive for 17 different analytes. The method achieved good sensitivity and simultaneous detection of a wide range of NPS.

scholarly journals Pharmacokinetics and bioavailability of liensinine in mouse blood by UPLC-MS/MS

2020 ◽  
Author(s):  
Shuhua Tong ◽  
Yuqi Zeng ◽  
Jianshe Ma ◽  
Congcong Wen
Keyword(s):  
Pharmacokinetic Study ◽  
Mobile Phase ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Quantitative Detection ◽  
Reaction Monitoring ◽  
Mouse Blood ◽  
Blood Samples ◽  
The Matrix ◽  
Better Than

AbstractLiensinine is a bisbenzyltetrahydroisoquinoline alkaloid extracted from lotus (Nelumbo nucifera GAERTNER., Nelumbonaceae), especially in its embryo loti “Lien Tze Hsin” (green embryo of mature seed). A rapid and simple UPLC-MS/MS method was developed to determine liensinine in mouse blood and its application to a pharmacokinetic study. The blood samples were preprocessed by protein precipitation using acetonitrile. Midazolam (internal standard, IS) and liensinine were gradient eluted by mobile phase of methanol and water (0.1% formic acid) in a Waters UPLC BEH C18 column. The multiple reaction monitoring of m/z 611.3 → 206.1 for liensinine and m/z 326.2 → 291.1 for IS with an electrospray ionization (ESI) source was used for quantitative detection. The calibration curve ranged from 0.5 to 400 ng/mL (r > 0.995). The accuracy ranged from 92.2 to 108.2%, the precision of intra-day and inter-day was less than 14%, and the matrix effect was between 100.0% and 109.6%, the recovery was better than 71.0%. The developed UPLC-MS/MS method was successfully used for a pharmacokinetic study of liensinine in mice after oral (5 mg/kg) and intravenous administration (1 mg/kg), and the absolute availability of liensinine was 1.8%.

scholarly journals Ultra-High Performance Liquid Chromatography-High Resolution Mass Spectrometry and High-Sensitivity Gas Chromatography-Mass Spectrometry Screening of Classic Drugs and New Psychoactive Substances and Metabolites in Urine of Consumers

2021 ◽  
Vol 22 (8) ◽  
pp. 4000
Author(s):  
Emilia Marchei ◽  
Maria Alias Ferri ◽  
Marta Torrens ◽  
Magí Farré ◽  
Roberta Pacifici ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Mobile Phase ◽  
High Performance ◽  
High Resolution Mass Spectrometry ◽  
High Sensitivity ◽  
Gas Chromatography Mass Spectrometry ◽  
New Psychoactive Substances ◽  
Psychoactive Substances ◽  
Resolution Mass

The use of the new psychoactive substances is continuously growing and the implementation of accurate and sensible analysis in biological matrices of users is relevant and fundamental for clinical and forensic purposes. Two different analytical technologies, high-sensitivity gas chromatography-mass spectrometry (GC-MS) and ultra-high-performance liquid chromatography-high-resolution mass spectrometry (UHPLC-HRMS) were used for a screening analysis of classic drugs and new psychoactive substances and their metabolites in urine of formed heroin addicts under methadone maintenance therapy. Sample preparation involved a liquid-liquid extraction. The UHPLC-HRMS method included Accucore™ phenyl Hexyl (100 × 2.1 mm, 2.6 μm, Thermo, USA) column with a gradient mobile phase consisting of mobile phase A (ammonium formate 2 mM in water, 0.1% formic acid) and mobile phase B (ammonium formate 2 mM in methanol/acetonitrile 50:50 (v/v), 0.1% formic acid) and a full-scan data-dependent MS2 (ddMS2) mode for substances identification (mass range 100–1000 m/z). The GC-MS method employed an ultra-Inert Intuvo GC column (HP-5MS UI, 30 m, 250 µm i.d, film thickness 0.25 µm; Agilent Technologies, Santa Clara, CA, USA) and electron-impact (EI) mass spectra were recorded in total ion monitoring mode (scan range 40–550 m/z). Urine samples from 296 patients with a history of opioid use disorder were examined. Around 80 different psychoactive substances and/or metabolites were identified, being methadone and metabolites the most prevalent ones. The possibility to screen for a huge number of psychotropic substances can be useful in suspected drug related fatalities or acute intoxication/exposure occurring in emergency departments and drug addiction services.

Rapid and Sensitive Bioanalytical Method Development and Validation for Quantification of Metoprolol Using LC-MS/MS in Human Plasma

2020 ◽  
Vol 42 (2) ◽  
pp. 171-171
Author(s):  
Beludari Mohammed Ishaq Beludari Mohammed Ishaq ◽  
Lingareddygari Siva Sanker Reddy Lingareddygari Siva Sanker Reddy ◽  
Gajula Mahaboob Basha Gajula Mahaboob Basha ◽  
Munna Sreenivasulu Munna Sreenivasulu ◽  
Challa Madhusudhana Chetty and Hindustan Abdul Ahad Challa Madhusudhana Chetty and Hindustan Abdul Ahad
Keyword(s):  
Human Plasma ◽  
Method Development ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Vascular Diseases ◽  
Storage Conditions ◽  
Spectrometric Analysis ◽  
Myocardial Infraction ◽  
Tandem Mass Spectrometric ◽  
Cardio Vascular

A novel, accurate, simple and selective LC-MS/MS method was developed and validated for the determination of metoprolol in human plasma. Due to structural resemblance Propranolol was selected as internal standard. Anti coagulant used was K2 EDTA. Metoprolol, used in the therapy and management of hypertension, myocardial infraction and other cardio vascular diseases. Liquid – liquid extraction technique with tert-butyl methyl ether was applied for the extraction of analyte from human plasma. Kromasil C18 column (5and#181;, 100 and#215; 4.6 mm) with an isocratic mobile phase of 5mM Ammonium Formate pH 3.5 and Acetonitrile (15:85 % V/V) was used for the resolution. Sample ionization was done with Electrospray ionization technique in positive ion mode. Selectivity was enhanced by tandem mass spectrometric analysis via two multiple reaction monitoring (MRM) transitions, m/z 268.15→115.90 for metoprolol and 260.17→115.90 for Propranolol respectively. The linearity of the method was established over a concentration range of 1.505 – 538.254 ng/mL, in human plasma, with the precision and accuracy ranging from 4.67 to 7.41% and 90.66 to 98.15% respectively. The stability of the analyte was evaluated in plasma under different storage conditions.

Oral fluid drug analysis in the age of new psychoactive substances

Bioanalysis ◽  
2016 ◽  
Vol 8 (7) ◽  
pp. 691-710 ◽  
Author(s):  
Elisabeth Leere Øiestad ◽  
Åse Marit Leere Øiestad ◽  
Astrid Gjelstad ◽  
Ritva Karinen
Keyword(s):  
Oral Fluid ◽  
Drug Analysis ◽  
New Psychoactive Substances ◽  
Psychoactive Substances

Prevalence of new psychoactive substances (NPS) in Brazil based on oral fluid analysis of samples collected at electronic music festivals and parties

2021 ◽  
pp. 108962
Author(s):  
Kelly Francisco da Cunha ◽  
Karina Diniz Oliveira ◽  
Marilia Santoro Cardoso ◽  
Ana Carolina Furiozo Arantes ◽  
Pedro Henrique Piras Coser ◽  
...  
Keyword(s):  
Electronic Music ◽  
Oral Fluid ◽  
New Psychoactive Substances ◽  
Psychoactive Substances ◽  
Music Festivals ◽  
Fluid Analysis

Green Liquid Chromatographic Methods with Ultraviolet and Tandem Mass Spectrometry Detection: An Application to Ternary Mixture of Paracetamol, Pseudoephedrine, and Cetirizine in Capsules

2020 ◽  
Vol 103 (1) ◽  
pp. 148-155 ◽  
Author(s):  
Souha H Youssef ◽  
Dalia Mohamed ◽  
Maha A Hegazy ◽  
Amr Badawey
Keyword(s):  
Mobile Phase ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Hplc Method ◽  
Green Solvents ◽  
Chromatographic Methods ◽  
Combination Methods ◽  
Significant Difference ◽  
Acid Aqueous Solution ◽  
Liquid Chromatographic

Abstract Background: Effective chromatographic methods were developed for the determination of a multicomponent capsule prescribed for treating the common cold. Greening approaches were adopted as opposed to conventional methods. Objectives: Two novel, green chromatographic methods were established to quantitatively analyze the combination. Methods: First, an HPLC/UV method utilizing green solvents (water and ethanol) and acetic acid to adjust pH at 5 was accomplished. The stationary phase was a ZorbaxSB-C18 column (150 × 4.6 mm, 5 μm), and peaks were detected at 215 nm. The second method is a highly sensitive ultra-performance LC (UPLC)-MS/MS method in which the greening approach was established through the reduction of the analysis time (2 min), decreased solvent consumption (flow rate 300 μL/min), and the utilization of a small volume of samples (injection volume 2 μL). The mixture was separated using a UPLC-BEH C18 column (50 × 2.1 mm, 1.7 μm) with an isocratic elution using methanol–0.1% formic acid aqueous solution (60+40, v/v) as mobile phase and utilizing diphenhydramine as an internal standard. Positive-ion electrospray ionization and multiple reaction monitoring were applied for detection. Results: Recovery percentages for paracetamol, pseudoephedrine, and cetirizine were 101.70 ± 0.969, 100.18 ± 1.563, and 99.67 ± 1.429 for the HPLC method and 99.18 ± 1.172, 100.03 ± 0.883, and 99.82 ± 0.912 for the UPLC-MS/MS method, respectively. Conclusions: The proposed methods efficiently analyzed paracetamol, pseudoephedrine, and cetirizine in Allercet Cold® capsules. Validation of the proposed methods was in accordance with the International Conference on Harmonization recommendations, and statistical comparison with the reported method displayed no significant difference regarding accuracy and precision. Highlights: Paracetamol, pseudoephedrine, and cetirizine were successfully quantified using two chromatographic methods. The HPLC method developed is considered green, using water and ethanol as a mobile phase. The UPLC-MS/MS method was rapid and determined the three drugs with accuracy at nanogram levels.

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