• Mass Spectrometry Letters
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• v.12 no.4
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• pp.179-185
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• 2021

Collision-induced dissociation (CID) combined with electrospray ionization mass spectrometry (ESI-MS) was used to obtain structural information on rat islet amyloid polypeptide (rIAPP) monomers (M) and dimers (D) observed in the multiply charged state in the MS spectrum. MS/MS analysis indicated that the rIAPP monomers adopt distinct structures depending on the molecular ion charge state. Peptide bond dissociation between L₂₇ and P₂₈ was observed in the MS/MS spectra of rIAPP monomers, regardless of the monomer molecular ion charge state. MS/MS analysis of the dimers indicated that D⁵⁺ comprised M²⁺ and M³⁺ subunits, and that the peptide bond dissociation process between the L₂₇ and P₂₈ residues of the monomer subunit was also maintained. The observation of (M+ b₂₇)⁴⁺ and (M+ y₁₀)³⁺ fragment ions were deduced to originate from the two different D⁵⁺ complex geometries, the N-terminal and C-terminal interaction geometries, respectively. The fragmentation pattern of the [M_rIAPP + M_hIAPP]⁵⁺ MS/MS spectrum showed that the interaction occurred between the two N-terminal regions of M_rIAPP and M_hIAPP in the heterogeneous dimer (hetero-dimer) D⁵⁺ structure.

• Archives of Pharmacal Research
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• v.28 no.5
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• pp.592-597
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• 2005

An HPLC/Esl/MS method has been developed to identify and quantify the spirostanol glycosides in the rhizomes of five Polygonatum species. The relative distribution of two steroidal saponins in each extract was established using the selective ion monitoring (SIM) mode via an electrospray ionization (ESI) source. It was found that there were significant differences in the amount of spirostanol glycosides among the Polygonatum Species. The results showed that this method could be used to identify the steroidal saponins in the extracts and differentiate Polygonatum species with high sensitivity and reproducibility in a short time. Fragmentation patterns of the two reference compounds were also discussed with the electrospray ionization multi-stage tandem mass spectroscopy (ESI-MS$^n$).

• Mass Spectrometry Letters
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• v.15 no.3
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• pp.121-140
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• 2024

Proteoform diversity is greatly increased by glycosylation, the primary post-translational modification of proteins. Glycans, also known as oligosaccharides, are molecules that are essential to almost all living things. They can affect protein folding and functionality, modulate cell-cell interactions, and support the proliferation of numerous diseases when they are found on cell surfaces or bound to proteins. A thorough understanding of their fundamental structure is necessary to gain insight into their characteristics and functions. But a major obstacle is the structural intricacy of glycans by design. The stereochemistry and regiochemistry of carbohydrates vary and are frequently branched. Because of its superior sensitivity and the abundance of fragmentation information it can provide, mass spectrometry is now the method of choice for glycan and glycopeptide analysis. Differentiating between the structures of isomeric and isobaric glycopeptides, however, presents a difficulty for MS-based characterization. Ion mobility plus mass spectrometry (IM-MS) has become a very promising new method for glycan research in recent years. Recent developments in the growing discipline of glycosylation analysis utilizing IM-MS are outlined in this review, with a focus on the MS methodology and its ability to resolve isomeric glycans.

• Food Science of Animal Resources
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• v.41 no.1
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• pp.59-70
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• 2021

A method for simultaneous detection of fipronil (F) and its metabolites fipronil desulfinyl (FD), fipronil sulfide (FS), fipronil sulfone (FSO) in chicken eggs was applied and validated. It includes single-step, cheap, effective, rugged, safe-based method (SinChERS) for sample preparation and ultra high performance liquid chromatography coupled with mass spectrometry (UHPLC-MS/MS) for chemical analysis. Results suggested that formic acid enhanced the recovery of 4 target residues and 1% supplementation to acetonitrile gained higher recoveries than that of 5%. SinChERS integrated extraction and clean-up steps into one, with shorter time (1.5 h) to operate and higher recoveries (97%-100%) than HLB, Envi-Carb-NH2 and quik-easy-cheap-effective-rugged-safe method (QuEChERS), and it consumed the smallest volume of extracting solvent (10 mL) as QuEChERS. Quantitative analyses using external standard method suggested the linear ranges of 4 target compounds were 1-20 ㎍/L with R2 >0.9947. The limit of detection (S/N>3) and quantification (S/N>10) were 0.3 ㎍/kg and 1 ㎍/kg. Recoveries ranged from 89.0% to 104.4%, and the relative standard deviations (n=6) at 1, 10, and 20 ㎍/kg were lower than 6.03%. Thirty batches of domestic eggs (500 g each) were detected by the established SinChERS-based UHPLC-MS/MS and no target residues were detected in all samples. The method developed in this study is a rapid, sensitive, accurate and economic way for multi-residue analysis of fipronil and its metabolites in eggs.

• Analytical Science and Technology
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• v.25 no.5
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• pp.292-299
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• 2012

GC/MS has been utilized for many applications due to great resolution and reproducibility, which made it possible to build up the database of mass spectrum, while HS-SPME has the advantage of solventfree extraction of volatile compounds. The combination of these two methods, HS-SPME GC/MS, enabled many scientific applications with various possibilities. In this study, the analysis of trail pheromone excreted from live Camponotus japonicus with the feature of solvent-free extraction was carried out and the optimization for this analysis was performed. The major compounds detected were n-decane, n-undecane, and n-tridecane. Optimization for the best detection of these hydrocarbons was processed in the point of SPME parameter (selection of fiber, extraction temperature, extraction time, etc.). The advantage of the analysis of live sample is to analyze phenomenon right after it is excreted by ants. But the experimental process has restriction of extraction temperature and time because of the analysis of live ants. Establishing the process of HS-SPME GC/MS applied to live samples shown in this study can be a breakthrough for the ecofriendly and ethical research of live things.

• Mass Spectrometry Letters
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• v.3 no.1
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• pp.15-17
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• 2012

Eighteen of the PDE-5 inhibitors and their analogues were analyzed using GC-EI-MS. Fourteen of them could be identified by simple GC-MS method without derivatization, but hydroxyhongdenafil, hydroxyvardenafil, xanthoanthrafil and mirodenafil could not be identified without derivatization for the high polarity due to the presence of hydroxyl groups. N,O-bis(trimethylsilyl) trifluoroacetamide (BSTFA) and N-methyl-N-(tert-butyldimethylsilyl)trifluoroacetamide (MTBSTFA), widely used trimethylsilyl (TMS) derivatizing reagents, were used to improve the sensitivity of the hydroxylated analogues. And the analytes could be identified by GC-MS after the derivatization.

• Analytical Science and Technology
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• v.15 no.5
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• pp.410-416
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• 2002

In this study, a new quantitative analytical method has been developed for the rapid determination of vancomycin in human plasma and urine using liquid chromatography/tandem mass spectrometry (LC - MS/MS). Chromatography was carried out on a $C_{18}$ XTerra MS column ($2.1{\times}30mm$) with a particle size of $3.5{\mu}m$. The mobile phase was 0.25% formic acid in 10% acetonitrile and the flow rate was $250{\mu}L/min$. Vancomycin and caffeine (internal standard) were detected by MS/MS using multiple reaction monitoring (MRM). Vancomycin gives a predominant doubly protonated precursor molecule ($[M+2H]^{2+}$) at m/z 725.0 and a corresponding product ion of m/z 100.0. Detection of vancomycin was good, accurate and precise, with a limit of detection of 1 nM in plasma. The calibration curves for vancomycin in human plasma was linear in a concentration range of $0.01{\mu}M$ - $100{\mu}M$ for plasma. This method has been successfully applied to determine the concentration of vancomycin in human plasma and urine from pharmacokinetic study and relative studies.

• Journal of Nutrition and Health
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• v.41 no.4
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• pp.327-340
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• 2008

This study was designed to investigate the correlation between nutrition status and cardiovascular disease in type 2 diabetes patients with metabolic syndrome. The subjects were 66 patients and divided into Non MS (a group without metabolic syndrome, n = 37) and MS (a group with metabolic syndrome, n = 29). The percentage of patients accompanying metabolic syndrome was 43.9% and family history such as DM, skipping meal and eating speed were higher in MS (P < 0.05) The average values of BMI, body fat (%), waist circumference were significantly higher in patients of MS than that of Non MS. For hamatological values, MS showed higher FRS, HOMA-IR, LDL-Cholesterol, CRP. Percentage of FRS was 21.63% in MS that is relatively higher in comparison with 16.81% in Non MS. Moreover, the incidence of cardiovascular disease appeared 13.8% in MS that is higher than 2.7% in Non MS. The intake of sodium and vitamin E were higher, but the intake of fat, vitamin A and zinc were lower in MS than in Non MS. Close correlations were elucidated among FRS, occurrence of cardiovascular disease, weight, waist circumference, Total-Cholesterol, LDLCholesterol, sodium in both groups. In conclusion, cardiovascular disease risk factors would be higher in type 2 diabetes patients with metabolic syndrome and there were distinctive patterns that were associated with hamatological values, nutrition intake risk factors. This result should be considered when designing nutrition study and intervetion programs.

• Asian-Australasian Journal of Animal Sciences
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• v.13 no.12
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• pp.1674-1680
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• 2000

A study was conducted to compare the feeding value of urea treated and untreated mustard straw (MS) for sheep. Treated MS was prepared by adding urea-N at 1.84% and followed by packing in a pit silo for 21 days. Two groups of six empty Avikaline ewes were fed untreated (UTMS) and treated (TMS) mustard straw along with 200 g concentrate per head daily for 90 days. Untreated MS had 0.41% N and the urea treatment increased its N value to 1.58 %. The cell wall constituents were decreased in the TMS except for cellulose which remained unaffected. Dry matter intake of TMS was consistently higher than that of UTMS. Digestibility of DM, OM and fibre fractions of MS improved by the urea treatment. Ewes in both groups were in positive N balance while % N retention was lower in UTMS (26.30%) than in TMS (52.14%). The TMS fed group on average consumed 30.2 g DM, 2.9 g digestible crude protein and $0.2MJ\;DE\;per\;kg\;BW\;day^{-1}$ and maintained their weight whereas, the UTMS fed ewes lost weight. The VFA concentration in rumen liquor was higher in TMS than in UTMS. Total-N, ammonia-N and TCA-precipitable-N were also higher in TMS fed ewes. Blood glucose concentrations in the two groups were similar at initiation of the study. However the glucose concentration of UTMS fed group was significantly (p<0.01) lower than those fed UTMS at the termination of the study. Urea-N concentration was also higher in TMS fed group after 90 days of feeding period. It is concluded that urea treatment of MS improved N value of MS from 0.41% to 1.58% along with sizable improvement in nutritive value and in conjunction with 200 g concentrate, TMS can serve as maintenance ration for sheep. ($ME_{lakt}/ME_{m}=1.46$).

• Bulletin of the Korean Chemical Society
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• v.34 no.5
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• pp.1487-1493
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• 2013

Based on the finding that the 2-aminobenzamido group of MS-275 plays a crucial role in inhibiting HDACs through chelation of zinc existing at the active site of HDAC enzymes, novel N-(2-hydroxyphenyl)arylsulfonamide derivatives were synthesized for their potential ability to inhibit HDACs and evaluated for anticancer activity against human breast cancer cell line (MCF-7). Although the synthesized arylsulfonamides have failed to significantly inhibit total HDACs activity, phenyl carbamate-linked arylsulfonamide 10 and benzyl thiocarbamate-linked arylsulfonamide 15 exhibited good anticancer activities, which were only 4.3- and 3.6-fold lower anticancer activities, respectively, than MS-275 that is undergoing phase II clinical trials. These results suggest that these compounds may act as a selective HDAC inhibitor and probably N-(2-hydroxyphenyl) sulfamoyl group may play an important role in interacting with HDAC enzymes through chelation of zinc ion.