scholarly journals HPLC Method for Separation of Cannabidiol Hemp Seed Oil with Skin Lipids and Tandem HRMS Technology for Characterization of a Chemical Marker

Cosmetics ◽  
2021 ◽  
Vol 8 (4) ◽  
pp. 108
Author(s):  
Yuxin Liu ◽  
Yu Wang ◽  
Zhigang Hao ◽  
Long Pan
Keyword(s):  
Mass Spectrometry ◽  
Seed Oil ◽  
High Resolution Mass Spectrometry ◽  
Structural Difference ◽  
Skin Surface ◽  
Raw Material ◽  
Chemical Marker ◽  
Hemp Seed ◽  
Mass Spectrometry Technology ◽  
Ammonium Adduct

Cannabidiol (CBD) hemp seed oil is a commercial raw material with antioxidant and anti-inflammatory benefits that has been formulated into body wash and skin care products. The biggest analytical challenge is how to simultaneously quantify CBD and hemp seed oil as they deposited on the skin surface. CBD is easily separated and quantified from skin surface extracts via a HPLC-mass spectrometry methodology. However, the structural skeleton of triacylglycerides (TAGs) in hemp seed oil is same as those from the skin surface sebum. The strong hydrophobicity with subtle structural difference challenges their separation. In this project, a new reverse phase HPLC-high resolution mass spectrometry methodology was developed with a strong mobile phase normal propanol. The separated hemp seed oil TAGs in the chromatogram were identified and characterized using data-dependent acquisition (DDA) technology. Based on the daughter ion characterization, the separated peak with an ammonium adduct at 890.7226 [M + NH4]+ was confirmed as the parent ion of glycerol with three omega-3 fatty acid chains. This is the first time TAG structure with direct HPLC-tandem mass spectrometry technology has been elucidated without a hydrolysis reaction. The confirmed TAG structure with an ammonium adduct at 890.7226 ± 0.0020 can be used as a representative chemical marker for the hemp seed oil quantification.

Study of High-Resolution Mass Spectrometry Technology as a Replacement for Tandem Mass Spectrometry in the Field of Quantitative Pesticide Residue Analysis

2012 ◽  
Vol 95 (2) ◽  
pp. 528-548 ◽  
Author(s):  
Anton Kaufmann ◽  
Veronika Dvorak ◽  
Claudio Crüzer ◽  
Patrick Butcher ◽  
Kathryn Maden ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
High Resolution ◽  
High Resolution Mass Spectrometry ◽  
Residue Analysis ◽  
Tandem Mass ◽  
Pesticide Residue Analysis ◽  
Accuracy And Precision ◽  
Mass Spectrometry Technology ◽  
Quantitative Performance ◽  
A Current

Abstract A validated LC/MS/MS-based multiresidue pesticide method was converted to an LC high-resolution MS single-stage Orbitrap platform. No changes regarding the cleanup and LC were made. Optimization of high-resolution MS-specific parameters and interface settings was kept at a minimum. The aim was to explore the capability of current Orbitrap technology to substitute for LC/MS/MS technology. The test included the quantitative performance (sensitivity, selectivity, linearity, accuracy, and precision) of some 240 analytes in three different matrixes. The LC/MS/MS instrumentation was operated at the edge of its technical limitations. A further extension of the number of analytes for LC/MS/MS would require the use of even narrower dwell times, significantly reducing sensitivity and reproducibility of measurement. No such limitations exist for the high-resolution technology. Similar performance was observed for both technologies. A current drawback of the high-resolution technology is the speed of data processing, which took significantly longer than for LC/MS/MS data due to the limited capabilities of the software.

Analysis of B-type natriuretic peptide impurities using label-free data-independent acquisition mass spectrometry technology

2021 ◽  
Vol 59 (1) ◽  
pp. 217-226
Author(s):  
Peng Xiao ◽  
Fan Zhang ◽  
Xinxue Wang ◽  
Dewei Song ◽  
Hongmei Li
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Natriuretic Peptide ◽  
Measurement Errors ◽  
Internal Standard ◽  
Raw Material ◽  
Label Free ◽  
Data Independent Acquisition ◽  
Free Data ◽  
Mass Spectrometry Technology

AbstractObjectivesSynthetic B-type natriuretic peptide (BNP) is employed in most clinical testing platforms as a raw material of calibrator. Characterization of impurities with structures similar (BNPstrimp compounds) to that of BNP is a reasonable way to decrease clinical measurement errors and improve drug safety.MethodsA novel quantitative method targeted towards BNPstrimp compounds was developed. First, the peptide samples were separated and identified using ultra-performance liquid chromatography, coupled with high-resolution mass spectrometry (MS). To evaluate biological activity further, BNPstrimp immunoaffinity was investigated using western blot (WB) assays. Second, a quantitative label-free data-independent acquisition (DIA) MS approach was developed, and the internal standard peptide (ISP) was hydrolyzed. Absolute quantification was performed using an isotope dilution MS (ID-MS) approach. Third, method precision was investigated using the C-peptide reference material.ResultsSeventeen BNPstrimp compounds were identified in synthetic BNP, and 10 of them were successfully sequenced. The immunoassay results indicated that deaminated, oxidized, and isomerized BNPstrimp compounds exhibited weaker immunoaffinity than intact BNP1-32. The mass fraction of the synthetic solid ISP1-16, quantified by ID-MS, was 853.5 (±17.8) mg/g. Validation results indicated that the developed method was effective and accurate for the quantitation of the well-separated BNP impurities.ConclusionsThe developed approach was easy to perform, and it was suitable for the parallel quantification of low-abundance BNPstrimp compounds when they performed a good separation in liquid chromatography. The quantitative results were comparable and traceable. This approach is a promising tool for BNP product quality and safety assessment.

Observed adducts on positive mode direct analysis in real time mass spectrometry – Proton/ammonium adduct selectivities of 600-sample in-house chemical library

2017 ◽  
Vol 23 (1) ◽  
pp. 4-10 ◽  
Author(s):  
Natsuhiko Sugimura ◽  
Asami Furuya ◽  
Takahiro Yatsu ◽  
Yoko Igarashi ◽  
Reiko Aoyama ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Nitrogen Atom ◽  
Oxygen Atom ◽  
Real Time ◽  
Density Functional ◽  
High Resolution Mass Spectrometry ◽  
Direct Analysis ◽  
Molecular Ions ◽  
Elemental Compositions ◽  
Ammonium Adduct

In this study, direct analysis in real time adduct selectivities of a 558 in-house high-resolution mass spectrometry sample library was evaluated. The protonated molecular ion ([M + H]+) was detected in 462 samples. The ammonium adduct ion ([M + NH4]+) was also detected in 262 samples. [M + H]+ and [M + NH4]+ molecular ions were observed simultaneously in 166 samples. These adduct selectivities were related to the elemental compositions of the sample compounds. [M + NH4]+ selectivity correlated with the number of oxygen atom(s), whereas [M + H]+ selectivity correlated with the number of nitrogen atom(s) in the elemental compositions. For compounds including a nitrogen atom and an oxygen atom [M + H]+ was detected; [M + NH4]+ was detected for compounds including an oxygen atom only. Density functional theory calculations were performed for selected library samples and model compounds. Energy differences were observed between compounds detected as [M + H]+ and [M + NH4]+, and between compounds including a nitrogen atom and an oxygen atom in their elemental compositions. The results suggested that the presence of oxygen atoms stabilizes [M + NH4]+, but not every oxygen atom has enough energy for detection of [M + NH4]+. It was concluded that the nitrogen atom(s) and oxygen atom(s) in the elemental compositions play important roles in the adduct formation in direct analysis in real time mass spectrometry.

scholarly journals How wort boiling process affects flavonoid polyphenols in beer

2019 ◽  
Vol 65 (6) ◽  
Author(s):  
Alexandr Mikyška ◽  
Martin Dušek
Keyword(s):  
Mass Spectrometry ◽  
Main Part ◽  
High Resolution Mass Spectrometry ◽  
Raw Materials ◽  
Biological Effects ◽  
Raw Material ◽  
Quechers Method ◽  
Boiling Process ◽  
Health Promoting ◽  
Resolution Mass

Beer and brewing raw materials are a source of number of polyphenol substances with potential or proven beneficial biological effects. In pilot brews of Czech pale lager (200 l) the behavior of hop-derived polyphenol substances during wort boiling process in various hopping regimes was studied. Prenylflavonoids, flavonoids and their O-glycosides were determined by liquid chromatography coupled to high resolution mass spectrometry (LC-HR / MS) with sample preparation by the QuEChERS method. The concentration of flavanols (catechin, epicatechin) in hopped wort and beer is dominated by hop raw material, when hopping with aromatic hops rich in polyphenols, 2/3 of the amount in beer is affected by hops. In contrast, the concentration of their mono-O-glucosides in beer does not depend on hopping. Flavonols quercetin, kaempferol and multifidol are found in wort and beer mainly in glycosidic form. The source of all these substances in beer is exclusively hops. Conversely, malt is the only source of myricetin and myricetin-O-glucoside in beer. Main part of hop-derived flavonoids is released during wort boiling into wort within 15-30 minutes. Splitting the hop dose or low pressure boiling technology had no significant effect on health-promoting polyphenols. Beer hopped with hops rich in flavonoids contains a relatively high amount of health-promoting polyphenols, while beer hopped with hop extract is very poor in these antioxidants.

Exploring the Active Compounds of Traditional Mongolian Medicine Agsirga in Intervention of Novel Coronavirus (2019-nCoV) Based on HPLC-Q-Exactive-MS/MS and Molecular Docking Method

2020 ◽  
Author(s):  
Jie Cheng ◽  
Yuchen Tang ◽  
Baoquan Bao ◽  
Ping Zhang
Keyword(s):  
Mass Spectrometry ◽  
Molecular Docking ◽  
High Resolution ◽  
Mass Spectra ◽  
High Resolution Mass Spectrometry ◽  
Structural Formula ◽  
Active Compounds ◽  
High Resolution Mass ◽  
Q Exactive ◽  
Resolution Mass

<p><a></a><a></a><a></a><a><b>Objective</b></a>: To screen all compounds of Agsirga based on the HPLC-Q-Exactive high-resolution mass spectrometry and find potential inhibitors that can respond to 2019-nCoV from active compounds of Agsirga by molecular docking technology.</p> <p><b>Methods</b>: HPLC-Q-Exactive high-resolution mass spectrometry was adopted to identify the complex components of Mongolian medicine Agsirga, and separated by the high-resolution mass spectrometry Q-Exactive detector. Then the Orbitrap detector was used in tandem high-resolution mass spectrometry, and the related molecular and structural formula were found by using the chemsipider database and related literature, combined with precise molecular formulas (errors ≤ 5 × 10<sup>−6</sup>) , retention time, primary mass spectra, and secondary mass spectra information, The fragmentation regularities of mass spectra of these compounds were deduced. Taking ACE2 as the receptor and deduced compounds as the ligand, all of them were pretreated by discover studio, autodock and Chem3D. The molecular docking between the active ingredients and the target protein was studied by using AutoDock molecular docking software. The interaction between ligand and receptor is applied to provide a choice for screening anti-2019-nCoV drugs.</p> <p><b>Result</b>: Based on the fragmentation patterns of the reference compounds and consulting literature, a total of 96 major alkaloids and stilbenes were screened and identified in Agsirga by the HPLC-Q-Exactive-MS/MS method. Combining with molecular docking, a conclusion was got that there are potential active substances in Mongolian medicine Agsirga which can block the binding of ACE2 and 2019-nCoV at the molecular level.</p>

A Mucin-Specific Protease Enables Molecular and Functional Analysis of Human Cancer-Associated Mucins

2018 ◽  
Author(s):  
Stacy A. Malaker ◽  
Kayvon Pedram ◽  
Michael J. Ferracane ◽  
Elliot C. Woods ◽  
Jessica Kramer ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Molecular Mechanisms ◽  
Cultured Cells ◽  
High Resolution Mass Spectrometry ◽  
Human Cancer ◽  
Glycosylation Sites ◽  
Bacterial Protease ◽  
Specific Protease ◽  
To Come ◽  
And Function

<div> <div> <div> <p>Mucins are a class of highly O-glycosylated proteins that are ubiquitously expressed on cellular surfaces and are important for human health, especially in the context of carcinomas. However, the molecular mechanisms by which aberrant mucin structures lead to tumor progression and immune evasion have been slow to come to light, in part because methods for selective mucin degradation are lacking. Here we employ high resolution mass spectrometry, polymer synthesis, and computational peptide docking to demonstrate that a bacterial protease, called StcE, cleaves mucin domains by recognizing a discrete peptide-, glycan-, and secondary structure- based motif. We exploited StcE’s unique properties to map glycosylation sites and structures of purified and recombinant human mucins by mass spectrometry. As well, we found that StcE will digest cancer-associated mucins from cultured cells and from ovarian cancer patient-derived ascites fluid. Finally, using StcE we discovered that Siglec-7, a glyco-immune checkpoint receptor, specifically binds sialomucins as biological ligands, whereas the related Siglec-9 receptor does not. Mucin-specific proteolysis, as exemplified by StcE, is therefore a powerful tool for the study of glycoprotein structure and function and for deorphanizing mucin-binding receptors. </p> </div> </div> </div>

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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