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Zolpidem, N,N-dimethyl-2-[6-methyl-2-(4-methylphenyl)imidazo[1,2-a]pyridin-3-yl] acetamide, is a hypnotic agent widely used in clinical practice but is detected in many clinical cases of fatal intoxication and suicide. In forensic toxicology, the precise determination of zolpidem concentration in blood is a must to provide concrete evidence of death by zolpidem poisoning. However, the concentrations of zolpidem in blood at autopsy often differ from those at the estimated time of death. In the present study, we found that zolpidem was degraded by hemoglobin (Hb) via the Fenton reaction at various temperatures. The mechanism underlying zolpidem degradation involved the oxidation of its linker moiety. The MS and MS/MS spectra obtained by liquid chromatography quadrupole-Orbitrap mass spectrometry (LC-Q-Orbitrap-MS) showed the formation of 2-hydroxy-N,N-dimethyl-2-(6-methyl-2-(p-tolyl) imidazo[1,2-a]pyridin-3-yl)acetamide (2-OH ZOL) in Hb/H2O2 solution incubated with zolpidem and in the blood of several individuals who died from ingestion of zolpidem. These results suggest that 2-OH ZOL is the post-mortem product of zolpidem degradation by Hb via the Fenton reaction. [ABSTRACT FROM AUTHOR]

The actual DOM in Chaohu Lake was used to feed cyanobacterial to explore the changes of microbial communities, fluorescence spectral characteristics and molecular composition of DOM during the degradation of cyanobacteria. It is found that cyanobacterial grow periodically depending on the concentration of nutrients with the decreasing concentration of nutrient salts. Both Bacteroidetes and Actinobacteria have strong correlation with algae growth. Bacteroidetes has a positive correlation with algae growth, relationship on the contrary, Actinobacteria has a negative relationship. The humus-like components in the four groups are similar, but the protein-like component (C3) shows periodic changes with the life process of cyanobacteria. The average molecular weight of each sample detected by Orbitrap high-resolution mass spectrometer increases slightly and the DOM increase aromaticity in the end. In this study, the molecule of Carboxyl-Rich Alicyclic Molecules (CRAM) is difficult to be done by photodegradation and biodegradation in the early periods, but some molecules of CRAM are selectively degraded by microorganisms in the final period. The growth of cyanobacterial lead to increasing the concentration of protein-like and carbohydrate-like molecule of DOM in the water. In the final stage, the molecule group of CHO disappear significantly and the molecule group of heteroatomic group increase. HIGHLIGHTS Dynamic changes of DOM and microbial communities during the proliferation and decline of live cyanobacteria through incubation.; DOM characteristics are analyzed by ultra-high-resolution mass spectrometry and EEMs-PARAFAC.; Incubating a single dominant algal species can simplify the complex ecological processes in nature, providing a more intuitive representation of the impact of dominant algae on DOM.;

Extreme weather events, such as tropical storms and hurricanes, are known to deliver large amounts of freshwater (surface runoff) and associated inorganic and organic nutrients to estuaries and the coastal ocean, affecting water quality and nutrient budgets. However, while Hurricane Harvey produced an unprecedented 1,000-year flood event in 2017 that inundated areas north of the landfall, like the Houston/Galveston region (Texas, United States), the impact on the Corpus Christi area, south of the landfall, was an intermittent negative surge (∼0.5 m below mean sea level (MSL)), caused by the southerly direction of winds and limited freshwater inflows. With the use of pre- and post-landfall surface-water, porewater, and groundwater nutrient measurements and dissolved organic matter (DOM) molecular characterization analyses, this study assessed the influence of negative storm surge on groundwater–surface water interactions and nutrient composition. Within 2 weeks following the first landfall, the forms and inputs of inorganic and organic nutrients fluctuated significantly nearshore Corpus Christi Bay. Sudden drops in sea level were correlated with pulses of NH4+ and disproportionately more dissolved organic carbon (DOC) than dissolved organic nitrogen (DON), likely from a carbon-rich groundwater or benthic source with slightly lower labile characteristics. Recovery to MSL drove higher proportions of nitrogenous DOM and lower dissolved inorganic nitrogen (DIN) inputs. An increased presence of sulfurized DOM derived from anaerobic microbial processing of organic matter mineralization in marine sediments post-landfall was facilitated by enhanced groundwater inputs and flushing of porewater due to considerable drops in sea level and steepening hydraulic gradients toward the coast. The induced pulses of higher groundwater advective fluxes are also hypothesized to have intermittently enhanced flushing of anoxic DIN and biodegraded DOM from porewater and groundwater and suggested that dynamic hurricane-induced negative surge events affect net nutrient budgets in estuarine and coastal seas.

Neuropeptide Y (NPY) is a transmitter molecule in nerve system, and it was an over 4‐kDa large peptide with the C‐terminal end amidation. NPY is biosynthesized through many maturation processes from a large pre‐pro‐peptide with peptide‐cleavages and amidation that is important to study the biosynthesis regulation. Previously, it was reported that cathepsin L participates in the production of NPY and that cathepsin L generates both of amidated and non‐amidated NPYs. However, the non‐amidated NPY (NPY‐COOH) has not been reported in brain tissues until now. In this study, endogenous NPY‐COOH in mouse brain tissue was detected and identified by using nano flow liquid chromatography (nanoLC) orbitrap Fourier transform mass spectrometry (FT‐MS) after the effective purification and separation of NPY‐COOH from NPY‐amide and other peptides using two different gel‐filtration chromatography. Amidated NPY was eluted earlier than non‐amidated NPY‐COOH in the C18 reversed phase nanoLC and the silica‐based gel‐filtration chromatogram with hydrophobic interaction. The amount of endogenous NPY‐COOH was about 0.05% of the matured NPY‐amide amount in adult mouse brain. [ABSTRACT FROM AUTHOR]

Mahonia leschenaultia (ML) and Mahonia napaulensis (MN) are less known and unexplored medicinal plants of the family Berberidaceae. They are used by the Todas of Nilgiris in their religious and medical practices but chemically less identified. Hence, we decided to do extensive phytochemical analysis to explore the potential of these plant extracts. An ultrahigh performance electrospray tandem mass spectrometry (UHPLC-ESI-MS/MS) method was successfully developed for qualitative analysis of the bioactive components in Mahonia species using Orbitrap Velos Pro mass spectrometer. Sixteen compounds were identified by comparison of their retention times and mass spectra (MS) with authentic standards and reported literature. Multi-stage mass spectra (MS2–8) for the identification of protoberberine and aporphine alkaloids showed the sequential expulsion of all the substituents attached with their basic skeleton followed by CO loss. Eight of the identified compounds (berberine, jatrorrhizine, palmatine, magnoflorine, isocorydine, glaucine, tetrahydropalmatine and tetrahydroberberine) were simultaneously determined by another UHPLC-ESI-MS/MS method under the multiple reactions monitoring (MRM) mode quantitatively using triple quadrupole linear ion trap mass spectrometer. The analytical method was validated for 8 bioactive compounds with overall recovery in the range 98.5%–103.6% (RSD≤2.2%), precise (RSD≤2.07%) and linear (r≥0.9995) over the concentration range of 0.5–1000 ng/mL and successfully applied in ML and MN roots, which suggests the suitability of the proposed approach for the routine analysis of Mahonia species and their quality control.

Zolpidem, N,N-dimethyl-2-[6-methyl-2-(4-methylphenyl)imidazo[1,2-a]pyridin-3-yl]acetamide, is a hypnotic agent widely used in clinical practice but is detected in many clinical cases of fatal intoxication and suicide. In forensic toxicology, the precise determination of zolpidem concentration in blood is a must to provide concrete evidence of death by zolpidem poisoning. However, the concentrations of zolpidem in blood at autopsy often differ from those at the estimated time of death. In the present study, we found that zolpidem was degraded by hemoglobin (Hb) via the Fenton reaction at various temperatures. The mechanism underlying zolpidem degradation involved the oxidation of its linker moiety. The MS and MS/MS spectra obtained by liquid chromatography quadrupole-Orbitrap mass spectrometry (LC-Q-Orbitrap-MS) showed the formation of 2-hydroxy-N,N-dimethyl-2-(6-methyl-2-(p-tolyl)imidazo[1,2-a]pyridin-3-yl)acetamide (2-OH ZOL) in Hb/H 2 O 2 solution incubated with zolpidem and in the blood of several individuals who died from ingestion of zolpidem. These results suggest that 2-OH ZOL is the post-mortem product of zolpidem degradation by Hb via the Fenton reaction.

Marine organic aerosols play crucial roles in global climatic systems. However, their chemical properties and relationships with various potential organic sources still need clarification. This study employed high-resolution mass spectrometry to investigate the identity, origin, and transportation of organic aerosols in pristine Antarctic environments (King Sejong Station; 62.2°S, 58.8°W), where complex ocean-cryosphere-atmosphere interactions occur. First, we classified the aerosol samples into three clusters based on their air mass transport history. Next, we investigated the relationship between organic aerosols and their potential sources, including organic matter dissolved in the open ocean, coastal waters, and runoff waters. Cluster 1 (C1), in which the aerosols mainly originated from the open ocean area (i.e., pelagic zone-influenced), exhibited a higher abundance of lipid-like and protein-like organic aerosols than cluster 3 (C3), with ratios 1.8- and 1.6-times higher, respectively. In contrast, C3, characterized by longer air mass retention over sea ice and land areas (i.e., inshore-influenced), had higher lignin- and condensed aromatic structures (CAS)-like organic aerosols by 2.2- and 3.4-times compared to C1. Cluster 2 (C2) has intermediate characteristics between C1 and C3 concerning the chemical properties of the aerosols and air mass travel history. Notably, the chemical properties of the aerosols assigned to C1 are closely related to those of phytoplankton-derived organics enriched in the open ocean. In contrast, those of C3 are comparable to those of terrestrial plant-derived organics enriched in coastal and runoff waters. These findings help evaluate the source-dependent properties of organic aerosols in changing Antarctic environment. • Back-trajectory cluster analysis reveals varied aerosol sources and characteristics. • Open ocean aerosols have more lipid and protein; possibly derived from phytoplankton. • Inshore aerosols contain higher lignin and condensed aromatic structures (CAS). • Organics of inshore aerosols likely originate from coastal and runoff waters. [ABSTRACT FROM AUTHOR]

Persimmon leaves have played an important role in Chinese medicine. Persimmon extracts and formulations have been shown to possess a wide range of pharmacological activities, including antioxidant, hypolipidaemic and antidiabetic, and they have been used to treat cardiovascular disease, improve homeostasis, as antibacterial and anti-inflammatory agents, and as a beauty treatment. In this work, liquid chromatography coupled to hybrid linear ion trap quadrupole Orbitrap mass spectrometry was used to accurately identify persimmon leaf polyphenols. Forty-one phenolic compounds, including simple phenolic acids, hydroxybenzoic acids, hydroxycinnamic acids, flavanols, flavonols, flavanones, flavone-chalcones, tyrosols and their conjugated derivatives, were identified and quantified using high mass accuracy data and confirmed by MS2 experiments. To the best of our knowledge, this is the most extensive study of persimmon leaf polyphenols performed so far, since 33 phenolic compounds are reported for the first time.

Homeopathic products are still a controversial issue in modern medicine, understood as complementary or alternative medicine (CAM). In this particular case, homeopathic products prepared from Atropa belladonna extracts may present specific problems due to the effects derived from its components. This article applies a simple, rapid, reliable method to the analysis of different homeopathic products obtained from Atropa belladonna; drugs containing high concentration of plant extracts; and Atropa belladonna seeds. The method was based on a simple solid‐phase preconcentration method followed by ultra‐high pressure liquid chromatography (UHPLC) coupled to high resolution mass spectrometry using Exactive‐Orbitrap as an analyser. An in‐house database was set and atropine and scopolamine were the compounds detected at highest concentrations in homeopathic products from Atropa belladonna extracts (4.57 and 2.56 μg/kg, respectively), in Belladonna ointment (4007 and 1139 μg/kg, respectively) and Belladonna seeds (338 and 32.1 mg/kg, respectively). Other tropane alkaloids such as tropine, apoatropine, aposcopolamine, tropinone, homatropine, and anisodamine were detected at lower concentrations (0.04–1.36 μg/kg). When untargeted analysis was performed, other tropane alkaloids were identified in the tested samples, such as ecgonine (0.003 μg/kg), benzoylecgonine (0.56 μg/kg), calystegines A (19.6 μg/kg), B (33.1 μg/kg), and C (1.01 μg/kg). Finally other compounds present in the homeopathic products, such as sugars (fructose, glucose, and lactose) or amino acids (valine, ornithine, leucine, and phenylalanine), were identified. Targeted and untargeted analysis have been performed for the determination of tropane alkaloids and related compounds in homeopathic products, drugs and seeds from Atropa belladonna, using liquid chromatography‐high mass spectrometry (Orbitrap). [ABSTRACT FROM AUTHOR]

Large volumes of oil sands process-affected water (OSPW) are generated during the extraction of bitumen from oil sands in the Athabasca region of northeastern Alberta, Canada. As part of the development of treatment technologies, molecular characterization of naphthenic acids (NAs) and naphthenic acid fraction compounds (NAFC) in wetlands is a topic of research to better understand their fate and behavior in aquatic environments. Reported here is the application of high-resolution negative-ion electrospray Orbitrap-mass spectrometry for molecular characterization of NAs and NAFCs in a non-aerated constructed treatment wetland. The effectiveness of the wetlands to remove OSPW-NAs and NAFCs was evaluated by monitoring the changes in distributions of NAFC compounds in the untreated sample and non-aerated treatment system. After correction for measured evapotranspiration, the removal rate of the classical NAs followed approximately first-order kinetics, with higher rates observed for structures with relatively higher number of carbon atoms. These findings indicate that constructed wetland treatment is a viable method for removal of classical NAs in OSPW. Work is underway to evaluate the effects of wetland design on water quality improvement, preferential removal of different NAFC species, and reduction in toxicity. [ABSTRACT FROM AUTHOR]

Mahonia leschenaultia ( ML ) and Mahonia napaulensis ( MN ) are less known and unexplored medicinal plants of the family Berberidaceae. They are used by the Todas of Nilgiris in their religious and medical practices but chemically less identified. Hence, we decided to do extensive phytochemical analysis to explore the potential of these plant extracts. An ultrahigh performance electrospray tandem mass spectrometry (UHPLC-ESI-MS/MS) method was successfully developed for qualitative analysis of the bioactive components in Mahonia species using Orbitrap Velos Pro mass spectrometer. Sixteen compounds were identified by comparison of their retention times and mass spectra (MS) with authentic standards and reported literature. Multi-stage mass spectra (MS 2–8 ) for the identification of protoberberine and aporphine alkaloids showed the sequential expulsion of all the substituents attached with their basic skeleton followed by CO loss. Eight of the identified compounds (berberine, jatrorrhizine, palmatine, magnoflorine, isocorydine, glaucine, tetrahydropalmatine and tetrahydroberberine) were simultaneously determined by another UHPLC-ESI-MS/MS method under the multiple reactions monitoring (MRM) mode quantitatively using triple quadrupole linear ion trap mass spectrometer. The analytical method was validated for 8 bioactive compounds with overall recovery in the range 98.5%–103.6% (RSD≤2.2%), precise (RSD≤2.07%) and linear ( r ≥0.9995) over the concentration range of 0.5–1000 ng/mL and successfully applied in ML and MN roots, which suggests the suitability of the proposed approach for the routine analysis of Mahonia species and their quality control. [ABSTRACT FROM AUTHOR]

Metabolomics, along with other "omics" approaches, is rapidly becoming one of the major approaches aimed at understanding the organization and dynamics of metabolic networks. Mass spectrometry is often a technique of choice for metabolomics studies due to its high sensitivity, reproducibility and wide dynamic range. High resolution mass spectrometry (HRMS) is a widely practiced technique in analytical and bioanalytical sciences. It offers exceptionally high resolution and the highest degree of structural confirmation. Many metabolomics studies have been conducted using HRMS over the past decade. In this review, we will explore the latest developments in Fourier transform mass spectrometry (FTMS) and Orbitrap based metabolomics technology, its advantages and drawbacks for using in metabolomics and lipidomics studies, and development of novel approaches for processing HRMS data. [ABSTRACT FROM AUTHOR]

Persimmon leaves have played an important role in Chinese medicine. Persimmon extracts and formulations have been shown to possess a wide range of pharmacological activities, including antioxidant, hypolipidaemic and antidiabetic, and they have been used to treat cardiovascular disease, improve homeostasis, as antibacterial and anti-inflammatory agents, and as a beauty treatment. In this work, liquid chromatography coupled to hybrid linear ion trap quadrupole Orbitrap mass spectrometry was used to accurately identify persimmon leaf polyphenols. Forty-one phenolic compounds, including simple phenolic acids, hydroxybenzoic acids, hydroxycinnamic acids, flavanols, flavonols, flavanones, flavone-chalcones, tyrosols and their conjugated derivatives, were identified and quantified using high mass accuracy data and confirmed by MS 2 experiments. To the best of our knowledge, this is the most extensive study of persimmon leaf polyphenols performed so far, since 33 phenolic compounds are reported for the first time. [ABSTRACT FROM AUTHOR]

The zebrafish embryo is a highly interesting biological model with applications in different scientific fields, such as biomedicine, pharmacology and toxicology. In this study, we used liquid chromatography/electrospray ionisation-linear ion trap quadrupole-Orbitrap-mass spectrometry (HPLC/ESI-LTQ-Orbitrap-MS) to identify the polyphenol compounds in a red wine extract and zebrafish embryos. Phenolic compounds and anthocyanin metabolites were determined in zebrafish embryos previously exposed to the red wine extract. Compounds were identified by injection in a high-resolution system (LTQ-Orbitrap) using accurate mass measurements in MS, MS 2 and MS 3 modes. To our knowledge, this research constitutes the first comprehensive identification of phenolic compounds in zebrafish by HPLC coupled to high-resolution mass spectrometry. [ABSTRACT FROM AUTHOR]

Color Index Disperse Yellow 42 (DY42), a high-volume disperse dye for polyester, was used to compare the capabilities of the LTQ-Orbitrap XL and the LTQ-FT-ICR with respect to mass measurement accuracy (MMA), spectral accuracy, and sulfur counting. The results of this research will be used in the construction of a dye database for forensic purposes; the additional spectral information will increase the confidence in the identification of unknown dyes found in fibers at crime scenes. Initial LTQ-Orbitrap XL data showed MMAs greater than 3 ppm and poor spectral accuracy. Modification of several Orbitrap installation parameters (e.g., deflector voltage) resulted in a significant improvement of the data. The LTQ-FT-ICR and LTQ-Orbitrap XL (after installation parameters were modified) exhibited MMA ≤ 3 ppm, good spectral accuracy (χ values for the isotopic distribution ≤ 2), and were correctly able to ascertain the number of sulfur atoms in the compound at all resolving powers investigated for AGC targets of 5.00 × 10 and 1.00 × 10. [ABSTRACT FROM AUTHOR]

• Molecular characterization of a M/LTCT using three mass spectrometers. • A large number of aromatic hydrocarbons have been detected by the GC×GC/TOF-MS. • The condensation aromatic compounds were analysed with ESI Orbitrap-MS. A middle/low-temperature coal tar from Northern Shaanxi Province (M/LTCT NSP) was extracted with petroleum ether, and the resulting extract was analyzed by three mass spectrometers. The main group components detected by gas chromatograph/mass spectrometer (GC/MS) are aliphatics, arenes, oxygen-containing organic compounds (OCOCs), and nitrogen-containing organic compounds (NCOCs). In total, nearly 1000 aliphatics, arenes, OCOCs (mainly O 1 and O 2), NCOCs and sulfur-containing organnic compouds (SCOCs) were detected by the two-dimensional gas chromatography/time-of-flight mass spectrometer (GC×GC/TOF-MS). The relative abundances (RAs) of NCOCs, OCOCs, and SCOCs detected by ESI Orbitrap-mass spectrometry in the positive ion mode are 80.8%, 16.1%, and 3.1%, While in the negative ion mode, the RAs of OCOCs and NCOCs are 85.6%, and 14.4%, respectively. The condensation degree of aromatics and existing forms of heteroatoms were also examined. [ABSTRACT FROM AUTHOR]

The complex natural organic matter of the Suwannee River fulvic acid (SRFA) standard was analyzed by online reversed-phase chromatography with Orbitrap MS/MS using collision-induced dissociation (CID). The number of isobars per nominal mass could be reduced to a single dominantly abundant species in a chromatographic run, sharing some ions with signals having the identical molecular formula in adjacent chromatographic segments and later serving as a precursor ion for fragmentation. A very large proportion of the same fragment ions existed in adjacent chromatographic fractions. The difference in the fragment ions in adjacent chromatographic fractions could be attributed to a gradual change in the formula composition of precursor ions in a chromatographic run. It could be concluded that dissolved organic matter (DOM) molecules with the same elemental composition in different chromatographic fractions may have very similar molecular structures. In addition, we propose a possible DOM model that might greatly deepen our understanding of the behavior of DOM in aquatic matrices. [Display omitted] • A novel approach was developed to explore the molecular structure complexity of SRFA by using UPLC-Orbitrap MSMS. • DOM molecules with the same elemental composition in different fractions may have very similar molecular structures. • The possible DOM model could greatly deepen our understanding of the behavior of DOM in aquatic matrices. [ABSTRACT FROM AUTHOR]

Drugs of abuse are psychoactive substances illicitly distributed and used worldwide. In Rio de Janeiro, Brazil, they represent a public health issue and are directly related to several social problems. The recent increase in appearances of new psychoactive substances (NPS), derived from structural modifications of existing psychoactive substances, poses a threat to public health and forensic laboratories worldwide, as little is known about these substances. This study aimed to chemically and geographically map drugs of abuse from blotter papers seized by the Civil Police of Rio de Janeiro State (PCERJ) between 2006 and 2019. High-performance analytical techniques, such as gas chromatography-mass spectrometry (GC-MS) and Orbitrap mass spectrometry (Orbitrap-MS), combined with statistical analyses, were employed to characterize the seized samples. The most common chemical compounds in NPS found in this study were synthetic phenethylamines, i.e., molecules from the 25I-NBOH (2-(((4-iodo-2,5-dimethoxyphenethyl)amino)methyl)phenol) and 25I-NBOMe (2-(4-iodo-2,5-dimethoxyphenyl)-N-(2-methoxybenzyl)ethanamine) families. Prior to 2014, the majority of seized blotter papers contained lysergic acid diethylamide (LSD) and were concentrated in the Metropolitan region. An upsurge in blotter paper seizures was observed from 2014 to 2017; the most common substances during this time were from the NBOMe family. NBOH compounds emerged in 2016 in coastal regions with high tourism, reaching over 1300 items only in 2017. Only one synthetic cannabinoid was found among the blotter papers seized in Rio de Janeiro between 2006 and 2019. The assembled chemical data and statistical analyses allowed the mapping and monitoring of the chemical profiles of the seized blotter papers, providing a strong foundation for the understanding of the origins and movement of these drugs around the RJ State. [ABSTRACT FROM AUTHOR]

• MS application using two different high-resolution mass analyzers: ICR and Orbitrap. • FT-ICR MS and Orbitrap-MS used on 30 Brazilian crude oils with a wide range of oAPI. • Greater abundance of assigned species by FT-ICR MS due to higher resolving power. • Notable distribution and distinction of the heteroatom classes using FT-ICR MS. • FT-ICR MS detected substances with higher molecular weight. • A prevalence of O 2 class in major crude oils using Orbitrap-MS. • Orbitrap-MS is a useful technique in petroleomics despite lower resolution power. • Orbitrap-MS exhibited O2 and N1 heteroatomic species predominance pattern in petroleum. Among the different types of available high-resolution mass spectrometers, Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR MS) and Orbitrap-MS are important tools for the study of nonvolatile crude oil fraction composition. No in deep comparison between each analyzer was still performed, mostly with a wide broad of real crude oil samples. Therefore, in this study a representative set of 30 Brazilian crude oils with a wide range of American Petroleum Institute (API) gravity (13.1–53.7) were considered. The ICR and Orbitrap analyzers allowed the elemental composition to be obtained by accurate mass measurements, and the most abundant species were mainly N, N 2 , O 3 , O 1 , O 2 , NO 2 , NS, NOS, and OS classes. In general, FT-ICR MS favored the detection of higher molecular weight analytes in relation to Orbitrap-MS. The notable distribution of the heteroatom classes showed that crude oils with intermediate API gravity presented a higher relative abundance of nitrogenous compounds (N x), while lighter oils presented a higher abundance of oxygenated compounds (O 1). The heavier ones had a higher abundance of O 2 class, which was not verified by Orbitrap-MS, where a prevalence of O 2 class was detected in major crude oils. An increase in average molar weight values was observed when we changed technique (Orbitrap-MS → FT-ICR MS) and ionization mode (negative → positive), since FT-ICR MS detected substances with higher m / z. In this way, this work examines the application of two different high-resolution mass analyzers, and shows the versatility and analytical response of each one within petroleomics. [ABSTRACT FROM AUTHOR]

Mahonia leschenaultia ( ML ) and Mahonia napaulensis ( MN ) are less known and unexplored medicinal plants of the family Berberidaceae. They are used by the Todas of Nilgiris in their religious and medical practices but chemically less identified. Hence, we decided to do extensive phytochemical analysis to explore the potential of these plant extracts. An ultrahigh performance electrospray tandem mass spectrometry (UHPLC-ESI-MS/MS) method was successfully developed for qualitative analysis of the bioactive components in Mahonia species using Orbitrap Velos Pro mass spectrometer. Sixteen compounds were identified by comparison of their retention times and mass spectra (MS) with authentic standards and reported literature. Multi-stage mass spectra (MS 2-8 ) for the identification of protoberberine and aporphine alkaloids showed the sequential expulsion of all the substituents attached with their basic skeleton followed by CO loss. Eight of the identified compounds (berberine, jatrorrhizine, palmatine, magnoflorine, isocorydine, glaucine, tetrahydropalmatine and tetrahydroberberine) were simultaneously determined by another UHPLC-ESI-MS/MS method under the multiple reactions monitoring (MRM) mode quantitatively using triple quadrupole linear ion trap mass spectrometer. The analytical method was validated for 8 bioactive compounds with overall recovery in the range 98.5%-103.6% (RSD≤2.2%), precise (RSD≤2.07%) and linear ( r ≥0.9995) over the concentration range of 0.5-1000 ng/mL and successfully applied in ML and MN roots, which suggests the suitability of the proposed approach for the routine analysis of Mahonia species and their quality control.