scholarly journals Analytical Characterization of 3-MeO-PCP and 3-MMC in Seized Products and Biosamples: The Role of LC-HRAM-Orbitrap-MS and Solid Deposition GC-FTIR

2021 ◽  
Vol 8 ◽  
Author(s):  
Giampietro Frison ◽  
Flavio Zancanaro ◽  
Samuela Frasson ◽  
Laura Quadretti ◽  
Michele Agnati ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Mass Measurement ◽  
Analytical Techniques ◽  
Ftir Spectra ◽  
Accurate Mass ◽  
Positional Isomers ◽  
Product Ions ◽  
Orbitrap Ms ◽  
Solid Deposition

Among the phencyclidine (PCP) and synthetic cathinone analogs present on the street market, 3-methoxyphencyclidine (3-MeO-PCP) is one of the most popular dissociative hallucinogen drugs, while 3-methylmethcathinone (3-MMC) is a commonly encountered psychostimulant. Numerous 3-MeO-PCP- and 3-MMC-related intoxication cases have been reported worldwide. Identification of the positional isomers of MeO-PCP and MMC families are particularly challenging for clinical and forensic laboratories; this is mostly due to their difficult chromatographic separation (particularly when using liquid chromatography–LC) and similar mass spectrometric behaviors. 3-MeO-PCP and 3-MMC were identified in two powders, detained by two subjects and seized by the police, by different analytical techniques, including liquid chromatography-high-resolution accurate-mass Orbitrap mass spectrometry (LC-HRAM-Orbitrap-MS), and solid deposition gas chromatography-Fourier transform infrared spectroscopy (sd-GC-FTIR). LC-HRAM-Orbitrap-MS allowed us to assign the elemental formulae C18H27NO (MeO-PCP) and C11H15NO (MMC) through accurate mass measurement of the two MH+ ions, and the comparison of experimental and calculated MH+ isotopic patterns. However, MH+ collision-induced product ions spectra were not conclusive in discriminating between the positional isomers [(3-MeO-PCP vs. 4-MeO-PCP) and (3-MMC vs. 4-MMC and 2-MMC)]. Likewise, sd-GC-FTIR easily allowed us to differentiate between the MeO-PCP and MMC positional isomers unambiguously, confirming the presence of 3-MeO-PCP and 3-MMC, due to the high-quality match factor of the experimental FTIR spectra against the target FTIR spectra of MeO-PCP and MMC isomers in a dedicated library. 3-MeO-PCP (in contrast to 3-MMC) was also detected in blood and urine samples of both subjects and analyzed in the context of routine forensic casework by LC-HRAM-Orbitrap-MS following a simple deproteinization step. In addition, this untargeted approach allowed us to detect dozens of phase I and phase II 3-MeO-PCP metabolites in all biological specimens. Analysis of the extracted samples by sd-GC-FTIR revealed the presence of 3-MeO-PCP, thus confirming the intake of such specific methoxy-PCP isomer in both cases. These results highlight the effectiveness of LC-HRAM-Orbitrap-MS and sd-GC-FTIR data in attaining full structural characterization of the psychoactive drugs, even in absence of reference standards, in both non-biological and biological specimens.

scholarly journals Searching for Low Molecular Weight Seleno-Compounds in Sprouts by Mass Spectrometry

Molecules ◽  
2020 ◽  
Vol 25 (12) ◽  
pp. 2870 ◽  
Author(s):  
Eliza Kurek ◽  
Magdalena Michalska-Kacymirow ◽  
Anna Konopka ◽  
Olga Kościuczuk ◽  
Anna Tomiak ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Molecular Weight ◽  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Analytical Techniques ◽  
Low Molecular Weight ◽  
Analytical Protocol ◽  
Icp Ms

A fit for purpose analytical protocol was designed towards searching for low molecular weight seleno-compounds in sprouts. Complementary analytical techniques were used to collect information enabling the characterization of selenium speciation. Conceiving the overall characterization of the behavior of selenium, inductively plasma optical mass spectrometry (ICP-MS) was used to determine the total selenium content in entire sprouts as well as in selected extracts or chromatographic fractions. Then, high-performance liquid chromatography combined with ICP-MS (HPLC-ICP-MS) was used to evaluate the presence of inorganic and organic seleno-compounds, with the advantages of being very sensitive towards selenium, but limited by available selenium standard compounds. Finally, ultra-high performance liquid chromatography electrospray ionization triple quadrupole mass spectrometry (UHPLC-ESI-QqQ-MS/MS) and UHPLC-ESI-Orbitrap-MS/MS were used for the confirmation of the identity of selected compounds and identification of several unknown compounds of selenium in vegetable sprouts (sunflower, onion, radish), respectively. Cultivation of plants was designed to supplement sprouts with selenium by using solutions of selenium (IV) at the concentration of 10, 20, 40, and 60 mg/L. The applied methodology allowed to justify that vegetable sprouts metabolize inorganic selenium to a number of organic derivatives, such as seleno-methylselenocysteine (SeMetSeCys), selenomethionine (SeMet), 5′-seleno-adenosine, 2,3-DHP-selenolanthionine, Se-S conjugate of cysteine-selenoglutathione, 2,3-DHP-selenocysteine-cysteine, 2,3-DHP-selenocysteine-cysteinealanine, glutathione-2,3-DHP-selenocysteine, gamma-Glu-MetSeCys or glutamyl-glycinyl-N-2,3-DHP-selenocysteine.

A new potential biomarker for 1-testosterone misuse in human urine by liquid chromatography quadruple time-of-flight mass spectrometry

2015 ◽  
Vol 7 (11) ◽  
pp. 4486-4492 ◽  
Author(s):  
Yang Liu ◽  
Jianghai Lu ◽  
Sheng Yang ◽  
Youxuan Xu ◽  
Xiaobing Wang
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Human Urine ◽  
Mass Measurement ◽  
Time Of Flight ◽  
Accurate Mass ◽  
Metabolic Profiles ◽  
Flight Mass Spectrometry ◽  
Potential Biomarker ◽  
Full Scan

In this study, 1-testosterone urinary metabolic profiles were investigated by liquid chromatography quadruple time-of-flight mass spectrometry (LC-QTOF-MS) using full scan and targeted MS/MS techniques with accurate mass measurement.

Selective and comprehensive characterization of the quinochalcone C-glycoside homologs in Carthamus tinctorius L. by offline comprehensive two-dimensional liquid chromatography/LTQ-Orbitrap MS coupled with versatile data mining strategies

RSC Advances ◽  
2016 ◽  
Vol 6 (1) ◽  
pp. 495-506 ◽  
Author(s):  
Wenzhi Yang ◽  
Wei Si ◽  
Jingxian Zhang ◽  
Min Yang ◽  
Huiqin Pan ◽  
...  
Keyword(s):  
Data Mining ◽  
Liquid Chromatography ◽  
Carthamus Tinctorius ◽  
Two Dimensional ◽  
Data Mining Techniques ◽  
Comprehensive Characterization ◽  
Orbitrap Ms

An offline 2D LC/LTQ-Orbitrap MS approach and versatile data mining techniques were developed to characterize new QCGs from C. tinctorius.

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