Time-of-flight Mass Spectrometry Research Articles

Components research on Tetrastigma hemsleyanum Diels et Gilg: Identification and effect of drying methods on the content of ten main constituents by targeting metabolomics method

Tetrastigma hemsleyanum Diels et Gilg (TH) is one of the new eight Genuine Medicinal Materials of Zhejiang. It has extensive biological activities, such as anti-inflammatory, anti-tumor and analgesic activities, etc. In this study, the chemical components of TH were systematically investigated by ultra high-performance liquid chromatography-tandem quadrupole time of flight mass spectrometry (UPLC/Q-TOF-MS). Based on the MS spectrum, 39 compounds in TH extracts including 14 flavonoids, 10 fatty acids, 5 polyphenols and phenolic acids, 4 terpenes and other compounds were detected and tentatively identified. TH samples were treated under different drying methods (vacuum freeze drying, hot air drying, natural drying, light drying and vacuum drying). Besides, the effect of different drying methods on the content of 10 main chemical constituents in TH extracts including catechin, rutin, kaempferol-3-O-rutinoside and so on was also investigated by targeting metabolomics method with ultra high-performance liquid chromatography-tandem triple quadrupole mass spectrometry (UPLC-MS/MS) assisted by multivariate statistical analysis. Large differences were observed between vacuum drying and vacuum freeze drying with remarkable content changes. The contents of rutin, proanthocyanidin B1 and catechin were the most different among the various drying methods. The systematic identification of chemical constituents is helpful for the further medicinal development and application of TH. The effects of drying methods on the content of TH components were studied, which provided experimental data for the processing, storage and quality control of TH.

Perspectives of species identification by MALDI-TOF MS in monitoring-Stability of proteomic fingerprints in marine epipelagic copepods.

We analysed the robustness of species identification based on proteomic composition to data processing and intraspecific variability, specificity and sensitivity of species-markers as well as discriminatory power of proteomic fingerprinting and its sensitivity to phylogenetic distance. Our analysis is based on MALDI-TOF MS (matrix-assisted laser desorption ionization time of flight mass spectrometry) data from 32 marine copepod species coming from 13 regions (North and Central Atlantic and adjacent seas). A random forest (RF) model correctly classified all specimens to the species level with only small sensitivity to data processing, demonstrating the strong robustness of the method. Compounds with high specificity showed low sensitivity, that is identification was based on complex pattern-differences rather than on presence of single markers. Proteomic distance was not consistently related to phylogenetic distance. A species-gap in proteome composition appeared at 0.7 Euclidean distance when using only specimens from the same sample. When other regions or seasons were included, intraspecific variability increased, resulting in overlaps of intra and inter-specific distance. Highest intraspecific distances (>0.7) were observed between specimens from brackish and marine habitats (i.e., salinity probably affects proteomic patterns). When testing library sensitivity of the RF model to regionality, strong misidentification was only detected between two congener pairs. Still, the choice of reference library may have an impact on identification of closely related species and should be tested before routine application. We envisage high relevance of this time- and cost-efficient method for future zooplankton monitoring as it provides not only in-depth taxonomic resolution for counted specimens but also add-on information, such as on developmental stage or environmental conditions.

Extraction and identification of steroidal saponins from Polygonatum cyrtonema Hua using natural deep eutectic solvent-synergistic quartz sand-assisted extraction method.

In this study, quartz sand with particularly sharp nanoscale edges acted like a nanoscale knife physically cut cells of Polygonatum cyrtonema Hua into nanosized particles and was synergized with natural deep eutectic solvent to extract steroidal saponins of Polygonatum cyrtonema Hua. The natural deep eutectic solvent (choline chloride-lactic acid)-synergistic quartz sand-assisted extraction was optimized using response surface methodology. The steroidal saponins purified with AB-8 macroporous resin were identified using ultra-high-performance liquid chromatography-triple time of flight mass spectrometry. The results showed that the experimental total saponins content value (36.97±0.12mg dioscin equivalent/g dry weight) at optimal extraction conditions with a temperature of 68°C, a rotational speed of 20 400rpm, shear time of 4.3min, the liquid-solid ratio of 38ml/g, was close to the maximum possible theoretical value (36.64mg dioscin equivalent/g dry weight). A total of 20 steroidal saponins were identified, among which the content of (25R)-Kingianoside E was the highest (102.66±3.47mg/g). Furthermore, a new steroid saponin (3β,25S)-26-(β-D-glucopyranosyloxy)-22-hydroxyfurost-5-en-3-yl 4-O-β-D-glucopyranosyl-β-D-galactopyranoside+Glc was found for the first time. These results revealed that natural deep eutectic solvent-synergistic quartz sand-assisted extraction was an efficient and green method to extract a variety of steroidal saponins.

Rapid identification of bacteria from agricultural environment using MALDI-TOF MS

AbstractIn this study, matrix-assisted laser desorption ionisation time of flight mass spectrometry (MALDI-TOF MS) was used to identify bacteria from environmental matrices. The aim of this work was to determine the efficacy of this rapid technique and the bacterial community of agricultural samples. Environmental samples included the collection of irrigation waters and manures, and bacteria from the surface of vegetables were also investigated. From food safety point of view, the investigation of these microbial communities is inevitable considering their potential hazardous impact on the food production chain. Altogether 235 bacterial isolates were identified with the most frequent genera being Pseudomonas, Bacillus, Acinetobacter and Aeromonas. Our results indicated that MALDI-TOF MS can be used to identify causative agents of foodborne illnesses, food spoilage and common plant pathogens. However, limitations of the rapid identification technique were also encountered as we obtained correct identification at species level for 30.2% and at genus level for 69.8% of the isolates.

In-vitro Activity of Isepamicin against Gram-negative Bacteria in Comparison to Other Aminoglycosides Routinely used at a Teaching Hospital in Northern India.

Background Isepamicin is a 1-N-S-a-hydroxy-b-aminopropionyl derivative of gentamicin B and the spectrum of pathogenic microorganisms covered by it and its effectiveness is similar to that of amikacin except the action of aminoglycoside inhibitor enzymes is ineffectual on it. Material and Methods We performed a prospective study in the Bacteriology section of the Department of Microbiology at a 1,600-bedded hospital in Northern India from Jan 2022 to March 2022. Isepamicin was tested for susceptibility against gram-negative bacteria, identified by routine biochemicals and matrix-assisted-desorption/ionization -time of flight-mass spectrometry (MALDI-TOF-MS) assay. The antibiotic susceptibility testing for each of the isolates was performed by Kirby Bauer's disc diffusion method, according to the CLSI 2019 guidelines. Results The majority of isolates were obtained from blood samples (50, 39.1%). Among the non-inducible Enterobacteriaceae , Escherichia coli was least susceptible to amikacin (8/27, 29.63%) and most susceptible to isepamicin (18/27, 66.67%). Klebsiella pneumoniae followed the same pattern of susceptibility as E. coli and was least susceptible to Amikacin (20/46, 43.48%) and most susceptible to isepamicin (24/46, 52.17%). Enterobacter cloacae (6/7, 85.71%) was most susceptible to both amikacin and isepamicin, followed by 71.43% (5/7, 71.43%) susceptibility to gentamicin and tobramycin each. Enterobacter aerogenes was equally 53.33% (8/15) susceptible to all antibiotics. Pseudomonas aeruginosa was the most susceptible isolate to all antibiotics (18/21, 85.71%). Conclusion Isepamicin is a potential antimicrobial agent for treating an array of gram-negative bacteria-associated infections and shows better in vitro activity than older aminoglycoside agents.

Mass-Dependent Critical Value Expressions for Particle Finding in Single-Particle ICP-TOFMS.

In time-of-flight mass spectrometry (TOFMS), ion detection is often achieved via electron multiplication followed by fast analog-to-digital conversion (ADC). This detection approach is chosen over time-to-digital conversion because it extends the dynamic range of TOFMS measurements, especially for transient analyses. However, fast ADC detection also introduces measurement noise fundamental to the electron multiplication process. In previous research, we demonstrated that TOFMS signals acquired with fast ADC follow a compound Poisson distribution in which the Poisson-distributed arrival of ions at the detector is compounded with the response profile of the electron multiplier. Here, we consider the influence of mass-to-charge (m/z)-dependent detector responses and their impact on particle-finding accuracy in single-particle inductively coupled plasma TOFMS (spICP-TOFMS). In spICP-TOFMS, highly time-resolved ion signals are recorded and particle signals are distinguished from background signals based on thresholding the data at m/z-specific critical values. Through Monte Carlo modeling with measured m/z-dependent detector responses, we generate compound Poisson model distributions and critical values that accurately account for the dispersion of measured signals. We test the accuracy of critical values through the analysis of dissolved element solutions and comparison of measured versus predicted event rates above critical value thresholds. The use of m/z-dependent compound Poisson critical values reduces false-positive particle identifications by one to two orders of magnitude compared to thresholding criteria based on normal or Poisson statistics. The improved accuracy and robustness of compound Poisson critical values enables automated multi-element particle finding in spICP-TOFMS.

In vivo aroma release and perception of composite foods using nose space PTR–ToF–MS analysis with Temporal-Check-All-That-Apply

In vivo aroma release and perception of complex food matrices have been underexplored. The aims of this study were to investigate the effects of (i) fat and sugar content of chocolate-hazelnut spreads on in vivo aroma release and perception and (ii) carrier addition (bread, wafer) on in vivo aroma release and perception of chocolate-hazelnut spread using dynamic nose space analysis (PTR–ToF–MS) and dynamic sensory analysis (TCATA). Carriers were combined with spreads varying in fat and sugar content and were spiked with five volatile organic compounds (benzaldehyde, filbertone, 2-methylpyrazine, delta-dodecalactone, isovaleraldehyde). TCATA profiles from a consumer panel without in vivo nose space analysis (n = 72) and a trained panel performing in vivo nose space analysis (n = 8, triplicate) were compared. TCATA profiles of the spread-carrier combinations obtained by both panels showed similarly that attributes related to the carriers were perceived at the beginning of consumption, whereas attributes related to the spreads were perceived after swallowing. Significant (p < 0.05) and small differences were observed for the attributes cocoa, creamy, milky, sticky and toffee between both panels. In the evaluated reformulation range, fat and sugar content of chocolate-hazelnut spreads had only a limited effect on in vivo aroma release and perception. In contrast, addition of carriers strongly affected in vivo aroma release and perception for all target molecules. The addition of carriers to spreads generally increased aroma release (duration and intensity of aroma release) and decreased aroma perception. The addition of carriers generally reduced the time to reach maximum intensity compared to when spreads were eaten alone for the five volatile organic compounds while perception decreased. We conclude that the strong effect of carrier addition on in vivo aroma release and perception of chocolate-hazelnut spreads highlights the importance of investigating toppings/spreads accompanied with carriers rather than in isolation.

Candida-associated denture stomatitis: clinical, epidemiological, and microbiological features.

The identification of Candida spp. in denture stomatitis, the clinical manifestations, and the antifungal susceptibility profile lead to a correct and individualized therapeutic management of the patients. This study is aimed at investigating the clinical manifestations and epidemiological and microbiological characteristics of Candida-associated denture stomatitis. The samples were obtained by swabbing the oral mucosa of the subjects and then seeded onto Sabouraud Dextrose Agar and onto CHROMagar® Candida plates. The identification at the species level was confirmed byMatrix Assisted Laser Desorption Time of Flight Mass Spectrometry. Clinical classification was performed according to the criteria proposed by Newton (1962): (i) pinpoint hyperemia, (ii) diffuse hyperemia, and (iii) granular hyperemia. For carrying out the antifungal susceptibility testing, we adopted the CLSI M27-S4 protocol. C. albicans was the most prevalent species in our study. Regarding non-albicans Candida species, C. glabrata was the most common species isolated from the oral mucosa (n = 4, 14.8%), while in the prosthesis, it was C. tropicalis (n = 4, 14.8%). The most prevalent clinical manifestation was pinpoint hyperemia and diffuse hyperemia. Candida albicans, C. glabrata, and C. parapsilosis were susceptible to all the tested antifungals. Concerning fluconazole and micafungin, only two strains showed dose-dependent sensitivity (minimum inhibitory concentration (MIC), 1μg/mL) and intermediate sensitivity (MIC, 0.25μg/mL). One C. tropicalis strain was resistant to voriconazole (MIC, 8μg/mL). C. albicans was the most common species found in oral mucosa and prosthesis. The tested antifungal drugs showed great activity against most isolates. The most prevalent clinical manifestations were Newton's type I and type II.

Pulmonary Nocardiosis Caused by &lt;i&gt;Nocardia otitidiscaviarum&lt;/i&gt; and &lt;i&gt;&lt;/i&gt;Successfully Treated with Ciprofloxacin Based on Bacterial Identification and Antimicrobial Susceptibility Testing

We report a case of pulmonary nocardiosis caused by Nocardia otitidiscaviarum in a man diagnosed with idiopathic thrombocytopenia who was on oral prednisolone therapy. A chest PET/CT examination 13 days after the start of prednisolone therapy revealed a nodular shadow, and it progressively worsened and was accompanied by cavity formation over time. N. otitidiscaviarum was identified in bronchoalveolar lavage fluid by matrix assisted laser desorption ionization time of flight mass spectrometry. The isolate was eventually confirmed to be N. otitidiscaviarum by a 16S rRNA analysis. There was no evidence of disseminated disease. Combination therapy consisting of oral sulfamethoxazole-trimethoprim (SMX-TMP) and intravenous amikacin and imipenem was initiated, but the SMX-TMP was discontinued because of adverse effects. Antimicrobial susceptibility testing revealed that the isolate was non-susceptible to ceftriaxone, imipenem, minocycline, and clarithromycin. The patient declined long-term intravenous therapy. Oral ciprofloxacin was administered instead, and the pulmonary nocardiosis improved after 6 months of therapy. Bacterial identification and antimicrobial susceptibility testing influence the choice of treatment regimens for nocardia infections by N. otitidiscaviarum, which may be resistant to multiple antimicrobial agents.

Large-Scale metabolomics: Predicting biological age using 10,133 routine untargeted LC-MS measurements.

Untargeted metabolomics is the study of all detectable small molecules, and in geroscience, metabolomics has shown great potential to describe the biological age-a complex trait impacted by many factors. Unfortunately, the sample sizes are often insufficient to achieve sufficient power and minimize potential biases caused by, for example, demographic factors. In this study, we present the analysis of biological age in ~10,000 toxicologic routine blood measurements. The untargeted screening samples obtained from ultra-high pressure liquid chromatography-quadruple time of flight mass spectrometry (UHPLC- QTOF) cover + 300 batches and + 30 months, lack pooled quality controls, lack controlled sample collection, and has previously only been used in small-scale studies. To overcome experimental effects, we developed and tested a custom neural network model and compared it with existing prediction methods. Overall, the neural network was able to predict the chronological age with an rmse of 5.88 years (r2 =0.63) improving upon the 6.15 years achieved by existing normalization methods. We used the feature importance algorithm, Shapley Additive exPlanations (SHAP), to identify compounds related to the biological age. Most importantly, the model returned known aging markers such as kynurenine, indole-3-aldehyde, and acylcarnitines along with a potential novel aging marker, cyclo (leu-pro). Our results validate the association of tryptophan and acylcarnitine metabolism to aging in a highly uncontrolled large-s cale sample. Also, we have shown that by using robust computational methods it is possible to deploy large LC-MS datasets for metabolomics studies to reduce the risk of bias and empower aging studies.

Phenotypic and Genotypic Correlation of Antimicrobial Susceptibility of Bacteroides fragilis: Lessons Learnt.

Background Bacteroides fragilis is an opportunistic pathogen causing severe infections, including bacteremia. There have been increased reports of antimicrobial resistance in B. fragilis. However, phenotypic testing of susceptibility is time consuming and not cost effective for anaerobes. The present study investigates the correlation of phenotypic susceptibility with genotypic markers; to determine if these could be considered for deciding empirical therapy for B. fragilis. Material and methods Bacteroides fragilis isolates from various clinical samples including exudates, tissue, and body fluids were collected between November 2018 and January 2020 in the Department of Clinical Microbiology, Christian Medical College (CMC) Vellore. Species identification was done by MatrixAssistedLaserDesorptionIonization time of flight mass spectrometry (MALDI TOF) according to the manufacturer's instructions. A total number of 51 B. fragilis isolates were tested against metronidazole, clindamycin, piperacillin/tazobactam, and meropenem phenotypically by agar dilution method using Clinical & Laboratory Standards Institute (CLSI) 2019 guidelines and minimum inhibitory concentrations (MIC) were interpretated. The genotypic markers for antimicrobial resistance genes (nim, emrF, and cfiA) were studied by polymerase chain reaction (PCR) assay as per the standard protocol on all isolates to detect resistance genes. Results B. fragilis isolates in this study expressed 45%, 41%, and 16% phenotypic resistance to clindamycin, metronidazole, and meropenem, respectively, with least resistance topiperacillin/tazobactam (6%). Among the metronidazole resistant isolates, 52% harbored nim gene. Nim gene was also present in 76% (23/30) of the metronidazole susceptible isolates. Similarly, cfiA was present in all eight meropenem resistant isolates in addition to 22% (9/41) of the susceptible isolates. All cfiA negative isolates were phenotypically susceptible. Interestingly, 74% (17/23) of the clindamycin resistant isolates were positive for ermF. Conclusions Detection of a limited set of genes does not always correlate with phenotypic resistance to metronidazole and clindamycindue to the reported influence of insertion sequence (IS) elements, efflux, and other genetic determinants. Certainly, the absence of the cfiA gene can be employed to rule out meropenem resistance. However, redundant use of antibiotics such as meropenem along with metronidazole could be avoided for B. fragilis, which might otherwise elevate meropenem resistance. Recommendation of metronidazole requires prior phenotypic testing due to the reported 41% resistance.

Non-target analysis of organohalogenated contaminants in deep-sea fishes from the Mediterranean Sea by comprehensive two-dimensional gas chromatography–time-of-flight mass spectrometry

The enhanced separation power and identification capabilities make comprehensive two-dimensional gas chromatography–time-of-flight mass spectrometry (GC × GC − ToF MS) a valuable instrumental alternative for non-target analysis (NTA). In the present study, GC × GC − ToF MS has been used for the NTA of chlorine- and bromine-containing compounds in composite livers of two scarcely investigated Mediterranean deep-sea fish species, hollowsnout grenadier (Coelorinchus caelorhincus) and roughsnout grenadier (Trachyrhinchus trachyrhinchus). Attention focused on the identification of organohalogenated compounds with structural characteristics similar to those of persistent organic pollutants (POPs). In total, 116 Cl-, Br- and mixed Cl/Br-compounds were either positively or tentatively identified in the analyzed liver samples. Up to 88 of these compounds were legacy POPs, being polychlorinated biphenyls (PCBs) and organochlorinated pesticides (OCPs) the most abundant and frequently detected families. The other 28 identified POP-like compounds were analytes not considered by current regulation and environmental monitoring programs, including, among others, degradation products of specific OCPs, naturally produced organohalogen compounds and several perchlorinated diethyldiphenylmethane-derivatives whose presence in the investigated species is reported here for the first time. The presence of other naturally occurring brominated and mixed halogenated compounds in these fish species is also described for the first time. Our results also showed differences in the accumulation profile of the identified compounds in both species. Thereby, anthropogenic POPs showed higher relative abundances in the livers of roughsnout grenadiers than those in hollowsnout grenadiers, while for naturally occurring compounds the opposite trend or similar levels were found in both species.

Beta-Lactam Susceptibility Profiles of Bacteria Isolated from the Ozama River in Santo Domingo, Dominican Republic

The spread and contamination of antimicrobial-resistant bacteria in ambient waters is an emerging concern in urban, rural, medical, and industrial settings. A large amount of domestic, hospital, and industrial wastewater discharged directly into the rivers through the different channels can turn them into extensive reservoirs of antibiotic-resistant bacteria. In the present study, surface water samples from three collection sites were analyzed, according to different levels of anthropogenic impacts, along the Ozama River, one of the most important rivers in the Dominican metropolitan area, a source of water and food for human consumption. Seventy-six bacterial isolates were selected based on resistance to beta-lactams, using culture media previously enriched with cefotaxime and imipenem. Matrix-Assisted Laser Desorption/Ionization Time of Flight Mass Spectrometry (MALDI-TOF) subsequently identified them. The isolates covered 12 genera of bacteria; more than 30% were clinically relevant, and 43% had phenotypes classified as multidrug resistance. A total of 10 (44%) presented resistance. However, only seven presented resistance to 3 or more of the 14 groups of antibiotics, considered to be a multiresistant phenotype, which was sequenced using the high-throughput sequencing technique or New Generation (NGS). This study is part of the initiative to understand the profiles of the dangers of multidrug resistance in the metropolitan and rural areas of the Dominican Republic and its possible implications for human health.

Impact of Matrix Species and Mass Spectrometry on Matrix Effects in Multi-Residue Pesticide Analysis Based on QuEChERS-LC-MS.

With the popularity of multi-residue pesticide analysis based on quick, easy, cheap, effective, rugged, and safe (QuEChERS) cleanup and liquid chromatography-mass spectrometry (LC-MS), matching optimal matrix-matched calibration protocols and LC-MS conditions to reduce matrix effects (MEs) has become a crucial task for analysts in their routines. However, dozens to hundreds of pesticide analytes in a single run generate increasingly multi-dimensional ME data, requiring appropriate tools to handle these data sets. Therefore, we established an ME analysis strategy by drawing on analytical thinking and tools from metabolomics analysis. Using this, matrix species-induced and mass spectrometry-induced systematic ME variations were distinguished, and pesticides contributed to the variations were scanned out. A simultaneous weakening of MEs on 24 pesticides in 32 different matrices was achieved using the time-of-flight-mass spectrometry (TOF-MS) scan under the information-dependent acquisition (IDA) mode of high-resolution mass spectrometry (HR-MS), compared to multiple reaction monitoring (MRM) scanning by tandem mass spectrometry (MS/MS). Bay leaf, ginger, rosemary, Amomum tsao-ko, Sichuan pepper, cilantro, Houttuynia cordata, and garlic sprout showed enhanced signal suppression in the MRM scan for 105 differential MRM transitions for 42 pesticides and in IDA mode for 33 pesticides, respectively. This study revealed the interference of matrix species and mass spectrometry on MEs and provided a novel strategy for ME analysis.

Exceptionally Stable Dimers and Trimers of Au25 Clusters Linked with a Bidentate Dithiol: Synthesis, Structure and Chirality Study

AbstractA bidentate chiral dithiol (diBINAS) is utilised to bridge Au25 nanoclusters to form oligomers. Separation by size allows the isolation of fractions that are stable thanks to the bidentate nature of the linker. The structure of the products is elucidated by small‐angle X‐ray scattering and calculated using density functional theory. Additional structural details are studied by diffusion‐ordered nuclear magnetic resonance spectroscopy, transmission electron microscopy and matrix‐assisted laser desorption/ionization time of flight mass spectrometry. Significant changes in the optical properties are analysed by UV/Vis and fluorescence spectroscopies, with the latter demonstrating a strong emission enhancement. Furthermore, the emergent chiral characteristics are studied by circular dichroism. Due to the geometry constraints of the nanocluster assemblies, diBINAS can be regarded as a templating molecule, taking a step towards the directed self‐assembly of metal clusters.

Exceptionally Stable Dimers and Trimers of Au25 Clusters Linked with a Bidentate Dithiol: Synthesis, Structure and Chirality Study.

A bidentate chiral dithiol (diBINAS) is utilised to bridge Au25 nanoclusters to form oligomers. Separation by size allows the isolation of fractions that are stable thanks to the bidentate nature of the linker. The structure of the products is elucidated by small-angle X-ray scattering and calculated using density functional theory. Additional structural details are studied by diffusion-ordered nuclear magnetic resonance spectroscopy, transmission electron microscopy and matrix-assisted laser desorption/ionization time of flight mass spectrometry. Significant changes in the optical properties are analysed by UV/Vis and fluorescence spectroscopies, with the latter demonstrating a strong emission enhancement. Furthermore, the emergent chiral characteristics are studied by circular dichroism. Due to the geometry constraints of the nanocluster assemblies, diBINAS can be regarded as a templating molecule, taking a step towards the directed self-assembly of metal clusters.

Integrated UPLC-Q-TOF-MS and network pharmacology approach-driven quality marker discovery of Danggui Shaoyao San for primary dysmenorrhea.

Danggui Shaoyao San (DSS), a famous prescription, has been clinically proved to be effective in treating primary dysmenorrhea (PD). Currently there is no valid quality control data available for DSS. The main aim of the current research was to explore quality markers (Q-markers) of DSS. The chemical constituents of DSS were qualitatively identified using ultra-performance liquid chromatography tandem quadrupole time of flight mass spectrometry (UPLC-Q-TOF-MS) technology. On this basis, the targets of DSS and PD were predicted and screened using the TCMSP, SwissTargetPrediction, GeneCards, OMIM and TTD databases. Gene Ontology and Kyoto Encyclopedia of Genes and Genomes pathway analysis was performed on the core intersection targets using string and Cytoscape 3.7.1 software. Then molecular docking was conducted to screen the Q-markers of DSS in PD. A total of 126 chemical constituents, including 22 organic acids, 14 phthalides, 24 monoterpenoids, five sesquiterpene lactones, 22 triterpenoids, four phenylpropanoids and 35 other compounds were preliminarily characterized. According to network pharmacology prediction analysis, six compounds containing polyporenic acid C, senkyunolide P, alisol B 23-acetate, naringenin, gallic acid, ferulic acid and albiflorin were regarded as Q-markers of DSS. The present research established an integrative UPLC-Q-TOF-MS and network pharmacology method to discover the latent Q-markers of DSS and provided a theoretical data for the follow-up quality control of DSS.

Salvia sclarea Essential Oil Chemical Composition and Biological Activities.

Salvia sclarea essential oil (SSEO) has a long tradition in the food, cosmetic, and perfume industries. The present study aimed to analyze the chemical composition of SSEO, its antioxidant activity, antimicrobial activity in vitro and in situ, antibiofilm, and insecticidal activity. Besides that, in this study, we have evaluated the antimicrobial activity of SSEO constituent (E)-caryophyllene and standard antibiotic meropenem. Identification of volatile constituents was performed by using gas chromatography (GC) and gas chromatography/mass spectrometry (GC/MS) techniques. Results obtained indicated that the main constituents of SSEO were linalool acetate (49.1%) and linalool (20.6%), followed by (E)-caryophyllene (5.1%), p-cimene (4.9%), a-terpineol (4.9%), and geranyl acetate (4.4%). Antioxidant activity was determined as low by the means of neutralization of the DDPH radical and ABTS radical cation. The SSEO was able to neutralize the DPPH radical to an extent of 11.76 ± 1.34%, while its ability to decolorize the ABTS radical cation was determined at 29.70 ± 1.45%. Preliminary results of antimicrobial activity were obtained with the disc diffusion method, while further results were obtained by broth microdilution and the vapor phase method. Overall, the results of antimicrobial testing of SSEO, (E)-caryophyllene, and meropenem, were moderate. However, the lowest MIC values, determined in the range of 0.22-0.75 µg/mL for MIC50 and 0.39-0.89 µg/mL for MIC90, were observed for (E)-caryophyllene. The antimicrobial activity of the vapor phase of SSEO (towards microorganisms growing on potato) was significantly stronger than that of the contact application. Biofilm analysis using the MALDI TOF MS Biotyper showed changes in the protein profile of Pseudomonas fluorescens that showed the efficiency of SSEO in inhibiting biofilm formation on stainless-steel and plastic surfaces. The insecticidal potential of SSEO against Oxycarenus lavatera was also demonstrated, and results show that the highest concentration was the most effective, showing insecticidal activity of 66.66%. The results obtained in this study indicate the potential application of SSEO as a biofilm control agent, in the shelf-life extension and storage of potatoes, and as an insecticidal agent.

Comparison of APCI orbitrap MS and GCxGC/EI TOF MS for the hydrocarbon analysis of heavy base oils

The performance of positive-ion mode atmospheric pressure chemical ionization linear quadrupole ion trap orbitrap mass spectrometry (APCI LQIT Orbitrap MS) has been compared to that of two-dimensional gas chromatography coupled with positive-ion mode electron ionization time-of-flight mass spectrometry (GCxGC/EI TOF MS) for the analysis of group III heavy base oils. Upon APCI, all compounds were predominantly ionized via protonation. However, protonated alkanes are not stable and predominantly generated [M−H]+ ions via elimination of a hydrogen molecule from the protonated molecule. The high-resolution APCI mass spectra provided elemental composition information for the compounds while low-resolution APCI mass spectra were used for semiquantitative evaluation of the relative amounts of the compounds. Ions corresponding to compounds in seven hydrocarbon classes, i.e., (1) linear and branched alkanes, (2) monocycloalkanes, (3) dicycloalkanes, (4) tricycloalkanes and alkylbenzenes, (5) tetracycloalkanes, (6) pentacycloalkanes, and (7) hexacycloalkanes were identified. On the other hand, the GCxGC/EI TOF MS method enabled the chromatographic separation of most analytes. The measured EI mass spectra were used for the identification of the compounds while the GC peak areas were used for semiquantitative evaluation. The detected compounds were classified into three different hydrocarbon classes, (1) linear and branched alkanes, (2) cycloalkanes, and (3) aromatic hydrocarbons. The (+)APCI LQIT Orbitrap MS method was found to be faster and to provide more information for the larger compounds in the samples. For example, polycycloalkanes were only detected by using (+)APCI MS. However, no aromatic compounds were detected. Data processing was more straightforward than when using the GCxGC/EI TOF MS method. However, the latter method provided more accurate results for aromatic hydrocarbons and small alkanes as the analysis of small alkanes by using (+)APCI MS is limited due to the fact that [M−H]+ ions of small alkanes overlap with alkane fragment ions. Both light and heavy aliphatic and aromatic hydrocarbons were detected by using the GCxGC/EI TOF MS method but not polycycloalkanes. Therefore, these two methods complement each other, and each has different strengths and weaknesses.

In-Depth Analysis of the N-Glycome of Colorectal Cancer Cell Lines.

Colorectal cancer (CRC) is the third most commonly diagnosed cancer and the second leading cause of cancer deaths worldwide. A well-known hallmark of cancer is altered glycosylation. Analyzing the N-glycosylation of CRC cell lines may provide potential therapeutic or diagnostic targets. In this study, an in-depth N-glycomic analysis of 25 CRC cell lines was conducted using porous graphitized carbon nano-liquid chromatography coupled to electrospray ionization mass spectrometry. This method allows for the separation of isomers and performs structural characterization, revealing profound N-glycomic diversity among the studied CRC cell lines with the elucidation of a number of 139 N-glycans. A high degree of similarity between the two N-glycan datasets measured on the two different platforms (porous graphitized carbon nano-liquid chromatography electrospray ionization tandem mass spectrometry (PGC-nano-LC-ESI-MS) and matrix-assisted laser desorption/ionization time of flight-mass spectrometry (MALDI-TOF-MS)) was discovered. Furthermore, we studied the associations between glycosylation features, glycosyltransferases (GTs), and transcription factors (TFs). While no significant correlations between the glycosylation features and GTs were found, the association between TF CDX1 and (s)Le antigen expression and relevant GTs FUT3/6 suggests that CDX1 contributes to the expression of the (s)Le antigen through the regulation of FUT3/6. Our study provides a comprehensive characterization of the N-glycome of CRC cell lines, which may contribute to the future discovery of novel glyco-biomarkers of CRC.