scholarly journals How to perform spectrum-based LC-HR-MS screening for more than 1,000 NPS with HighResNPS consensus fragment ions

PLoS ONE ◽  
2020 ◽  
Vol 15 (11) ◽  
pp. e0242224
Author(s):  
Anders Davidsen ◽  
Marie Mardal ◽  
Kristian Linnet ◽  
Petur Weihe Dalsgaard
Keyword(s):  
High Resolution Mass Spectrometry ◽  
Absolute Intensity ◽  
New Psychoactive Substances ◽  
Identification Rate ◽  
Data Independent Acquisition ◽  
Fragment Ions ◽  
Three Samples ◽  
Two Samples ◽  
Screening Software

Introduction The ever-changing market of new psychoactive substances (NPS) poses challenges for laboratories worldwide. Analytical toxicologists are constantly working to keep high-resolution mass spectrometry (HR-MS) screening libraries updated for NPS. This study sought to use the online crowd-sourced HighResNPS database for spectrum comparison screening, thereby broadening its utility to all HR-MS instruments. Method HighResNPS allows formation of a set of consensus fragment ions for a NPS and prioritises among multiple entries of collision-induced fragment ions. A subset of 42 NPS samples was analysed in data-independent acquisition (DIA) and data-dependent acquisition (DDA) modes on two different instruments. HighResNPS-computed spectra were generated with either Absolute (all fragment ions set to 100%) or Fractional (50% intensity reduction of former fragment ion) intensity. The acquired NPS data were analysed using the consensus library with computed ion intensities and evaluated with vendor-neutral screening software. Results Overall, of the 42 samples, 100% were identified, with 88% identified as the top candidate. Three samples had the correct candidate proposed as the second highest ranking NPS. In all three of those samples, the top proposed candidate was a positional isomer or closely related compound. Absolute intensity assignment provided identical scoring between the top two proposed compounds in two samples with DIA. DDA had a slightly higher identification rate in the spectra comparison screening with fractional intensity assignment, but no major differences were observed. Conclusion The fractional intensity assignment was slightly more advantageous than the absolute assignment. It was selective between proposed candidates, showed a high identification rate and had an overall higher fragmentation scoring. The candidates proposed by the HighResNPS library spectra comparison simplify the determination of NPS for researchers and toxicologists. The database provides free monthly updates of consensus spectra, thereby enabling laboratories to stay at the forefront of NPS screening by LC-HR-MS with spectra screening software.

scholarly journals HighResNPS.com: An Online Crowd-Sourced HR-MS Database for Suspect and Non-targeted Screening of New Psychoactive Substances

2019 ◽  
Vol 43 (7) ◽  
pp. 520-527 ◽  
Author(s):  
Marie Mardal ◽  
Mette Findal Andreasen ◽  
Christian Brinch Mollerup ◽  
Peter Stockham ◽  
Rasmus Telving ◽  
...  
Keyword(s):  
High Resolution Mass Spectrometry ◽  
New Psychoactive Substances ◽  
Psychoactive Substances ◽  
Suspect Screening ◽  
Fragment Ions ◽  
Diagnostic Fragment ◽  
Targeted Screening ◽  
Screening Coverage ◽  
Low Prevalence ◽  
Screening Software

Abstract The number of new psychoactive substances (NPS) is constantly increasing. However, although the number might be large, most NPS have a low prevalence of use, so keeping screening libraries updated with the relevant analytical targets becomes a challenge. One way to ensure sufficient screening coverage is to use shared high resolution-mass spectrometry (HR-MS) databases, such as HighResNPS.com: a free, online, spreadsheet-format, crowd-sourced HR-MS database for NPS screening. The aims of this study were (i) to present the database to the scientific community and (ii) to verify that the HighResNPS database can be utilized in suspect screening workflows for LC–HR-MS instruments and software from four different instrument vendors. A sample was spiked with 10 NPS, and participating laboratories then analyzed the sample with their respective HR-MS vendor platforms and the HighResNPS database. The HighResNPS data were obtained via a spreadsheet converted to fit the import specifications of the different vendor platforms. Suspect screening was performed using LC–HR-MS vendor platforms from Thermo Fisher, Waters, Bruker and Agilent. All 10 NPS were identified in at least three workflows used for the four different vendor platforms. Multiple users have submitted data to HighResNPS for the same NPS, which resulted in multiple true-positive identifications for these NPS. Suspect screening with LC–HR-MS can be based on diagnostic fragment ions reported by users of different vendor platforms and can support NPS identification in biological samples and/or seizure analyses when no reference standard is available in-house. The present work clearly demonstrates that HighResNPS data is compatible with instruments and screening software from at least four different vendor platforms. The database can thus serve as a useful add-on in LC–HR-MS screening workflows.

scholarly journals Reaktive E=C(p–p)π Systeme, XXXIV Addition von Alkoholen oder primären Aminen an Phosphaalkene F3CP=C(F)OR. Neue Trifluormethylphosphane und -phosphaalkene/Reactive E = C( p – p ) π-Systems, XXXIV Addition of Alcohols or Primary Amines to Phosphaalkenes F3CP= C(F)OR . Novel Trifluoromethylphosphanes and Phosphaalkenes

1993 ◽  
Vol 48 (1) ◽  
pp. 58-67 ◽  
Author(s):  
Joseph Grobe ◽  
Duc Le Van ◽  
Gudrun Lange
Keyword(s):  
High Resolution Mass Spectrometry ◽  
Molar Ratio ◽  
Primary Amines ◽  
The Novel ◽  
Experimental Conditions ◽  
Pull System ◽  
Fragment Ions ◽  
New Compounds ◽  
C Nmr

The course of the reactions o f fluorophosphaalkenes F3CP = C (F)OR [R = Me (1), Et (2)] with methanol or ethanol strongly depends on the experimental conditions. Thus at 70 °C a mixture of the 2-phosphapropionic acid ester F3CP (H )CO2R [R = Me (3), Et (4)] and trifluoromethylphosphane H2PCF3 is formed [molar ratio: 3 or 4 /H2 CF3 ≈1/1]. If the precursors F3CP (H )CO2R [R = Me (3), Et) are used as starting materials, the reaction with ROH under the same conditions affords 3 and 4, respectively, (90 to 95% yield) with only traces of H2PCF 3. In the presence o f iPr2NH these precursors react with R′OH to give the novel trifluoromethylphosphaalkenes F3CP = C (OR )OR [R /R′: Me/Me (6); E t/E t (7); Me/Et (8)]. With Et2NH , 3 undergoes an addition/elimination process yielding the interesting push/pull system Et2N(F)C = P-CO2Me (5). 1 and 2 react with primary amines R′NH2 (R′= tBu, Me) with stereoselective formation of the fairly labile phosphaalkenes F3CP = C(OR)NHR′ [R /R′: Me/tBu (9), Et/tBu(10), Me/Me (11)] with trans-positions for CF3 and NHR′.The new compounds 3 -11 were characterized by spectroscopic investigations (1H , 19F, 31P, 13C NMR ; IR, MS) and determination of M+ or typical fragment ions [M+ -OR ] by high resolution mass spectrometry.

Determination of Heavy Metals in Wheat and Barley Grains Using ICP-MS/MS

2020 ◽  
Vol 103 (5) ◽  
pp. 1277-1281
Author(s):  
Tamer M A M Thabit ◽  
Shokr Abdelsalam Shokr ◽  
Dalia I H Elgeddawy ◽  
Medhat A H El-Naggar
Keyword(s):  
Heavy Metals ◽  
Acid Digestion ◽  
Validation And Verification ◽  
European Origin ◽  
Three Samples ◽  
Icp Ms ◽  
Two Samples ◽  
Low Levels ◽  
Barley Grains

Abstract Wheat and barley grains are two of the most important nutritional grains for humans and animals and they play an essential role in the nutritional cycle by different ratios according to people's nutritional habits. This work aimed to monitor ten of the most important heavy metals in some European-origin wheat and barley grains during the season of 2018. The measured elements, Al, As, Cd, Co, Cr, Hg, Mo, Ni, Pb, and V, are of importance ecologically and biologically and may be involved in many health disorders affecting the human body. Moisture, protein, and specific grain weights were checked. Samples were digested using microwave acid digestion and the elements measured with ICP-MS/MS in He mode to increase sensitivity, lower the background, and avoid interference. Method validation and verification were carried out through spiking at two levels (2.0 and 10 ppb), then RSD, LOD, and LOQ were calculated. Recoveries were >97% for all elements at both levels with an RSD of <7.6%. Results revealed that As, Cd, Hg, and Pb were not detected in most wheat and barley samples, whereas Cd was detected in one sample of Ukrainian wheat and two samples of Estonian barley (but in very small traces). Pb was detected in three samples of Polish wheat (in very small traces). Al, Mo, and Ni were detected in some samples of wheat and barley of all origins, whereas other elements were at very low levels considered to be negligible concentrations.

Metabolism Study of N-Methyl 2-Aminoindane (NM2AI) and Determination of Metabolites in Biological Samples by LC–HRMS

2020 ◽  
Author(s):  
Serena Mestria ◽  
Sara Odoardi ◽  
Sofia Federici ◽  
Sabrine Bilel ◽  
Micaela Tirri ◽  
...  
Keyword(s):  
Biological Samples ◽  
In Silico ◽  
High Resolution Mass Spectrometry ◽  
New Drugs ◽  
New Psychoactive Substances ◽  
Hair Samples ◽  
Metabolism Study ◽  
Fragmentation Patterns

Abstract Since the widespread diffusion of new psychoactive substances, forensic laboratories are often required to identify new drugs and their metabolites for which information or reference standards are lacking. We performed a study on N-methyl-2-aminoindane (NM2AI) metabolism in silico and in vivo, in order to identify the main metabolites to be screened in the different biological samples. We performed the in silico metabolism prediction of NM2AI using MetaSiteTM software and subsequently verified the presence of metabolites in the blood, urine and hair of mice after NM2AI administration. The samples were analyzed by liquid chromatography–high-resolution mass spectrometry (LC–HRMS) with a benchtop Orbitrap Exactive mass detector. This allowed the evaluation of the agreement between software prediction and experimental results in biological samples. LC–HRMS analysis identified seven main metabolites in the urine. They were identified, by their accurate masses and fragmentation patterns, as 2-aminoindane (2AI), two hydroxy-2AI and four hydroxy-NM2AI; one of the hydroxy-NM2AI and one of the hydroxy-2AI underwent also to conjugation. NM2AI and 2AI were also detected by LC–HRMS in the hair and blood. Based on these findings, we developed an LC–HRMS method for the screening of NM2AI and metabolites in urine, blood and hair samples. This can be of primary effectiveness to uncover the abuse of NM2AI and related possible intoxications.

scholarly journals Simultaneous determination of 137 drugs of abuse, new psychoactive substances, and novel synthetic opioids in meconium by UHPLC-QTOF

2021 ◽  
Author(s):  
Ángela López-Rabuñal ◽  
Daniele Di Corcia ◽  
Eleonora Amante ◽  
Marta Massano ◽  
Angelines Cruz-Landeira ◽  
...  
Keyword(s):  
Drugs Of Abuse ◽  
Limit Of Detection ◽  
New Psychoactive Substances ◽  
Range Limit ◽  
Psychoactive Substances ◽  
Childbearing Age ◽  
Two Samples ◽  
Novel Synthetic Opioids ◽  
Substances Of Abuse

AbstractNew psychoactive substances (NPS) have been introduced into the market in recent years, with new analytes reported every year. The use of these substances in women can occur at any stage of life, even in the childbearing age. Drug use during pregnancy presents significant risks for the mother and the fetus, so it is important to have tools that allow to detect prenatal exposure to these substances of abuse. Therefore, an analytical method for the determination of 137 NPS and other drugs of abuse in meconium by UHPLC-QTOF was developed and validated for semi-quantitative purpose. Linearity range, limit of detection (LOD), precision, matrix effect, selectivity, and specificity were evaluated. For all analytes, the calibration curves were studied in the ranges between 2, 10, or 50 ng/g and 750 or 1000 ng/g, (depending on the analyte) and the LOD ranged between 0.04 and 2.4 ng/g. The method was applied to 30 meconium specimens from cases in which fentanyl had been administered as epidural anesthesia at the time of delivery or cases in which the maternal hair was positive to other drug of abuse. Four meconium samples tested positive for fentanyl (range concentration = 440–750 ng/g) and two samples tested positive to acetylfentanyl (range concentration = 190–1400 ng/g).

scholarly journals Application of the UHPLC-DIA-HRMS Method for Determination of Cheese Peptides

Foods ◽  
2020 ◽  
Vol 9 (8) ◽  
pp. 979
Author(s):  
Georg Arju ◽  
Anastassia Taivosalo ◽  
Dmitri Pismennoi ◽  
Taivo Lints ◽  
Raivo Vilu ◽  
...  
Keyword(s):  
Selection Criteria ◽  
High Performance ◽  
Milk Protein ◽  
High Resolution Mass Spectrometry ◽  
Peptide Mapping ◽  
Mapping Method ◽  
Data Independent Acquisition ◽  
Cheese Peptides ◽  
Analytical Gradients

Until now, cheese peptidomics approaches have been criticised for their lower throughput. Namely, analytical gradients that are most commonly used for mass spectrometric detection are usually over 60 or even 120 min. We developed a cheese peptide mapping method using nano ultra-high-performance chromatography data-independent acquisition high-resolution mass spectrometry (nanoUHPLC-DIA-HRMS) with a chromatographic gradient of 40 min. The 40 min gradient did not show any sign of compromise in milk protein coverage compared to 60 and 120 min methods, providing the next step towards achieving higher-throughput analysis. Top 150 most abundant peptides passing selection criteria across all samples were cross-referenced with work from other publications and a good correlation between the results was found. To achieve even faster sample turnaround enhanced DIA methods should be considered for future peptidomics applications.

scholarly journals Microbiological analysis for drug resistant pathogenic microorganisms with determination of the antibacterial properties found in Fragaria x ananassa (strawberry) samples

2017 ◽  
Vol 6 (1) ◽  
pp. 16-19
Author(s):  
Nazneen Piangka ◽  
Tasnia Ahmed ◽  
Mrityunjoy Acharjee
Keyword(s):  
Pathogenic Bacteria ◽  
Antibacterial Properties ◽  
Microbiological Analysis ◽  
Drug Resistant ◽  
E Coli ◽  
Three Samples ◽  
Wide Range ◽  
Two Samples ◽  
Health Related

Strawberry is a popular fruit item consumed by people all over the world for its exceptional flavor and aroma. This fruit is being used to prepare a wide range of food items. Strawberries when consumed by people without undergoing any processing, the condition may not be good enough. People may get sick after consuming raw strawberries. Our current study identified several pathogenic bacteria which are very known in causing health related problems. E. coli was found in one sample (1.0×102 cfu/g), Staphylococcus aureus was commonly present in all of the five samples (up to 1.2×106 cfu/g), Klebsiella spp. was found to be present in two samples (within 1.0×103 cfu/g) and Pseudomonas spp. was present in three samples (8.2×104 cfu/g), respectively. All isolated bacteria showed some degree of drug resistant traits against some commonly used antibiotics. The most important and promising part of the study was to successfully find the antimicrobial activity of strawberries against seven types of pathogenic bacteriaStamford Journal of Microbiology, Vol.6(1) 2016: 16-19

Determination of quaternary ammonium compounds in food products by the method of ultra-performance liquid chromatography/high resolution mass-spectrometry

2020 ◽  
Vol 86 (8) ◽  
pp. 23-31
Author(s):  
V. G. Amelin ◽  
D. S. Bolshakov
Keyword(s):  
Mass Spectrometry ◽  
High Resolution ◽  
Quaternary Ammonium ◽  
High Resolution Mass Spectrometry ◽  
Food Products ◽  
Quaternary Ammonium Compounds ◽  
High Resolution Mass ◽  
Ammonium Compounds ◽  
Resolution Mass

The goal of the study is developing a methodology for determination of the residual amounts of quaternary ammonium compounds (QAC) in food products by UHPLC/high-resolution mass spectrometry after water-acetonitrile extraction of the determined components from the analyzed samples. The identification and determination of QAC was carried out on an «UltiMate 3000» ultra-high-performance liquid chromatograph (Thermo Scientific, USA) equipped with a «maXis 4G» high-resolution quadrupole-time-of-flight mass spectrometric detector and an ion spray «ionBooster» source (Bruker Daltonics, Germany). Samples of milk, cheese (upper cortical layer), dumplings, pork, chicken skin and ground beef were used as working samples. Optimal conditions are specified for chromatographic separation of the mixture of five QAC, two of them being a mixture of homologues with a linear structure (including isomeric forms). The identification of QAC is carried out by the retention time, exact mass of the ions, and coincidence of the mSigma isotopic distribution. The limits for QAC detection are 0.1 – 0.5 ng/ml, the determination limits are 1 ng/ml for aqueous standard solutions. The determinable content of QAC in food products ranges within 1 – 100 ng/g. The results of analysis revealed the residual amount of QAC present in all samples, which confirms data of numerous sources of information about active use of QAC-based disinfectants in the meat and dairy industry. The correctness of the obtained results is verified by introduction of the additives in food products at a level of 10 ng/g for each QAC. The relative standard deviation of the analysis results does not exceed 0.18. The duration of the analysis is 30 – 40 min.

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