• 제목/요약/키워드: ESI-MS response

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The Influence of Mixed Solvents Volatility on Charge State Distribution of Peptides During Positive Electrospray Ionization Mass Spectrometry

  • Nielsen, Birthe V.;Abaye, Daniel A.;Nguyen, Minh T.L.
    • Mass Spectrometry Letters
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    • v.8 no.2
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    • pp.29-33
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    • 2017
  • Understanding the mechanisms that control and concentrate the observed electrospray ionisation (ESI) response from peptides is important. Controlling these mechanisms can improve signal-to-noise ratio in the mass spectrum, and enhances the generation of intact ions, and thus, improves the detection of peptides when analysing mixtures. The effects of different mixtures of aqueous: organic solvents (25, 50, 75%; v/v): formic acid solution (at pH 3.26) compositions on the ESI response and charge-state distribution (CSD) during mass spectrometry (MS) were determined in a group of biologically active peptides (molecular wt range 1.3 - 3.3 kDa). The ESI response is dependent on type of organic solvent in the mobile phase mixture and therefore, solvent choice affects optimal ion intensities. As expected, intact peptide ions gave a more intense ESI signal in polar protic solvent mixtures than in the low polarity solvent. However, for four out of the five analysed peptides, neither the ESI response nor the CSD were affected by the volatility of the solvent mixture. Therefore, in solvent mixtures, as the composition changes during the evaporation processes, the $pK_b$ of the amino acid composition is a better predictor of multiple charging of the peptides.

Development and Validation of an Analytical Method for Glucuronolactone in Energy Drinks by Hydrophilic Interaction Liquid Chromatography-electrospray Tandem Mass Spectrometry

  • Oh, Mi Hyune;Lim, Moo Song;Chai, Jeung Young;Kim, Eun Jung;Cho, Joong Hoon;Lim, Chul Joo;Choi, Sun Ok
    • Journal of Food Hygiene and Safety
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    • v.32 no.2
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    • pp.89-95
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    • 2017
  • A rapid, sensitive analytical method for glucuronolactone in beverages was developed and validated using hydrophilic interaction liquid chromatography coupled to electrospray ionization tandem mass spectrometry (HILIC-ESI-MS/MS). To determine the optimum analytical conditions for glucuronolactone, three different kinds of HILIC columns and two mobile phases with different pH values were examined. An amide-bonded stationary phase with a pH 9 acetonitrile-rich mobile phase was the best condition in terms of column retention, ESI-MS/MS response area, and signal-to-noise ratio. After extraction, glucuronolactone was separated through the HILIC amide column and detected by negative ESI-MS/MS in selected reaction monitoring (SRM) mode. Nine energy drinks sold in Korea were spiked with glucuronolactone at a concentration of 5 ng/mL; the Monster $Energy^{TM}$ sample showed the smallest peak area and its signal-to-noise ratio was used for method validation. Good linearity was obtained in the concentration range from 20 to 1500 ng/mL with a correlation coefficient > 0.998. The developed method had a limit of detection (LOD) of 6 ng/mL and a limit of quantitation (LOQ) of 20 ng/mL. The recovery of this method at concentration of 20, 100, 500, and 1000 ng/mL was 96.3%-99.2% with relative standard deviations (RSD) of 1.6%-14.0%. A reproducibility precision assessment at concentration of 100 and 500 ng/mL was carried out among three laboratories. The recovery of that evaluation was 95.1%-102.3% with RSD of 2.7%-7.0%. An analysis of variance indicated that there was no difference between the recovery results of the three laboratories at the 5% significance level. The validated method is applicable to inspecting beverages adulterated with glucuronolactone in Korea.

Hydrolysis of Penicillin G and Carbenicillin in Pure Water - As Studied by HPLC/ESI-MS

  • Kolek, Marta;Franski, Rafal;Franska, Magdalena
    • Mass Spectrometry Letters
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    • v.10 no.4
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    • pp.108-111
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    • 2019
  • The hydrolysis of penicillin G, carbenicillin and ampicillin in pure water at room temperature was studied by high pressure liquid chromatography electrospray ionization mass spectrometry. Hydrolysis of ampicillin did not occur under these conditions; however, penicillin G and carbenicillin were completely hydrolyzed after seven days. A short interpretation of this difference is proposed. The mass spectrometric behaviour, namely ESI response and fragmentation pathway, of hydrolyzed penicillin G and hydrolyzed carbenicillin have been also discussed.

Effects of Qi Gong Exercise on the Immune Response, Pulse Wave Parameter and Heart Rate Variability(HRV) for Post Mastectomy Women (기공(氣功) 운동이 유방암 절제술 여성의 면역, 맥상파 및 심박변이에 미치는 영향)

  • Kim, Yi Soon;Lee, Jeong Won;Kim, Yun Hee;Oh, Mi Jung;Kim, Gyeong Cheol
    • The Journal of the Society of Korean Medicine Diagnostics
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    • v.19 no.2
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    • pp.75-90
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    • 2015
  • Objectives The purposes of this study was to develope a Qi gong exercise that suits characteristics of post mastectomy women, and to evaluate the effect of Qi gong exercise on immune response, blood circulation index, pulse wave parameter and heart rate variability. Methods This study was applied to total 35 post mastectomy women, including 17 for experiment group and 18 for control group. The Qi gong exercise was composed of total 24 times of 90 minutes per each time, twice a week, and 12 weeks and it was conducted by the oriental medicine professor who was an expert of Qi gong exercise. Results 1. Two group comparison revealed that the experimental group had significantly improved immune response(p<.021), HR(beats/min)(p<.001), ESV(ml/beat)(p=.038), ESI($ml/beat/m^2$)(p=.040), ECO (L/min)(p=.019), ECI($L/min/m^2$)(p=.023), ECRI($dyne^*sec/cm$)(p=.015), Left Kwan($div^3$)(p=.021), Right Kwan($div^3$)(p=.038), Mean HRV(cycle/min)(p<.001), SDNN(ms)(p=.043), RMSSD(ms)(p=.040), and TP(log $ms^2$)(p=.039). 2. Two group comparison revealed that the experimental group had significantly decreased ECR ($dyne^*sec^*cm^{-5}$) (p=.034), Left RAI(p=.044), Right RAI(p=.042), and pNN50(%)(p=.038). Conclusions These results from Qi gong exercise program can be used as basic data for development of health promotion program for Post Mastectomy Women.

Genistein alleviates pulmonary fibrosis by inactivating lung fibroblasts

  • Seung-hyun Kwon;Hyunju Chung;Jung-Woo Seo;Hak Su Kim
    • BMB Reports
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    • v.57 no.3
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    • pp.143-148
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    • 2024
  • Pulmonary fibrosis is a serious lung disease that occurs predominantly in men. Genistein is an important natural soybean-derived phytoestrogen that affects various biological functions, such as cell migration and fibrosis. However, the antifibrotic effects of genistein on pulmonary fibrosis are largely unknown. The antifibrotic effects of genistein were evaluated using in vitro and in vivo models of lung fibrosis. Proteomic data were analyzed using nano-LC-ESI-MS/MS. Genistein significantly reduced transforming growth factor (TGF)-β1-induced expression of collagen type I and α-smooth muscle actin (SMA) in MRC-5 cells and primary fibroblasts from patients with idiopathic pulmonary fibrosis (IPF). Genistein also reduced TGF-β1-induced expression of p-Smad2/3 and p-p38 MAPK in fibroblast models. Comprehensive protein analysis confirmed that genistein exerted an anti-fibrotic effect by regulating various molecular mechanisms, such as unfolded protein response, epithelial mesenchymal transition (EMT), mammalian target of rapamycin complex 1 (mTORC1) signaling, cell death, and several metabolic pathways. Genistein was also found to decrease hydroxyproline levels in the lungs of BLM-treated mice. Genistein exerted an anti-fibrotic effect by preventing fibroblast activation, suggesting that genistein could be developed as a pharmacological agent for the prevention and treatment of pulmonary fibrosis.

Proteomic Analysis of Protein Expression in Streptococcus pneumoniae in Response to Temperature Shift

  • Lee Myoung-Ro;Bae Song-Mee;Kim Tong-Soo;Lee Kwang-Jun
    • Journal of Microbiology
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    • v.44 no.4
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    • pp.375-382
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    • 2006
  • From its initial colonization to causation of disease, Streptococcus pneumoniae has evolved strategies to cope with a number of stressful in vivo environmental conditions. In order to analyze a global view of this organism's response to heat shock, we established a 2-D electrophoresis proteome map of the S. pneumoniae D39 soluble proteins under in vitro culture conditions and performed the comparative proteome analysis to a 37 to $42^{\circ}C$ temperature up-shift in S. pneumoniae. When the temperature of an exponentially growing S. pneumoniae D39 culture was raised to $42^{\circ}C$, the expression level of 25 proteins showed changes when compared to the control. Among these 25 proteins, 12 were identified by MALDI-TOF and LC-coupled ESI MS/MS. The identified proteins were shown to be involved in the general stress response, energy metabolism, nucleotide biosynthesis pathways, and purine metabolism. These results provide clues for understanding the mechanism of adaptation to heat shock by S. pneumoniae and may facilitate the assessment of a possible role for these proteins in the physiology and pathogenesis of this pathogen.

Mass Spectrometric Determination of Zn2+ Binding/Dissociation Constant for Zinc Finger Peptides

  • Lee, Choong Sik;Park, Soo Jin;Lee, Jae Young;Park, Sungsu;Jo, Kyubong;Oh, Han Bin
    • Mass Spectrometry Letters
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    • v.6 no.1
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    • pp.7-12
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    • 2015
  • In the present study, we proposed a simple ESI-MS model for determining $Zn^{2+}$ binding (or dissociation) constants for zinc finger peptides (ZFPs) with a unique ${\beta}{\beta}{\alpha}$ fold consensus. The ionization efficiency (response) factors for this model, i.e., ${\alpha}$ and ${\beta}$, could be determined for ZiCo ZFP with a known $Zn^{2+}$ binding constant. We could determine the binding constants for other ZFPs assuming those with a ${\beta}{\beta}{\alpha}$ consensus conformation have the same ${\alpha}/{\beta}$ response ratio. In general, the ZPF dissociation constants exhibited $K_d$ values of $10^{-7}{\sim}10^{-9}M$, while $K_d$ values for a negative control non-specific $Zn^{2+}$ peptides were high, e.g., $5.5{\times}10^{-6}M$ and $4.3{\times}10^{-4}M$ for BBA1 and melittin, respectively.

Botrytis cinerea hypovirulent strain △BcSpd1 induced Panax ginseng defense

  • Shuhan Zhang;Junyou Han;Ning Liu;Jingyuan Sun;Huchen Chen;Jinglin Xia;Huiyan Ju;Shouan Liu
    • Journal of Ginseng Research
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    • v.47 no.6
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    • pp.773-783
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    • 2023
  • Background: Gray mold, caused by Botrytis cinerea, is one of the major fungal diseases in agriculture. Biological methods are preferred over chemical fungicides to control gray mold since they are less toxic to the environment and could induce the resistance to pathogens in plants. In this work, we try to understand if ginseng defense to B. cinerea could be induced by fungal hypovirulent strain △BcSpd1. BcSpd1 encodes Zn(II)2Cys6 transcription factor which regulates fungal pathogenicity and we recently reported △BcSpd1 mutants reduced fungal virulence. Methods: We performed transcriptomic analysis of the host to investigate the induced defense response of ginseng treated by B. cinerea △BcSpd1. The metabolites in ginseng flavonoids pathway were determined by UPLC-ESI-MS/MS and the antifungal activates were then performed. Results: We found that △BcSpd1 enhanced the ginseng defense response when applied to healthy ginseng leaves and further changed the metabolism of flavonoids. Compared with untreated plants, the application of △BcSpd1 on ginseng leaves significantly increased the accumulation of p-coumaric acid and myricetin, which could inhibit the fungal growth. Conclusion: B. cinerea △BcSpd1 could effectively induce the medicinal plant defense and is referred to as the biological control agent in ginseng disease management.

Degradation of oxytetracycline by nano zero valent iron under UV-A irradiation: Chemical mechanism and kinetic

  • Hassanzadeh, Parisa;Ganjidoust, Hossein;Ayati, Bita
    • Advances in environmental research
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    • v.3 no.1
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    • pp.29-43
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    • 2014
  • Pharmaceutical wastewater effluents are well known for their difficult elimination by traditional biotreatment methods and their important contribution to environmental pollution due to its fluctuating and recalcitrant nature. OTC is one of the nonbiodegradable antibiotics that makes antibiotic-resistant, so it can make be high risk for environment. NZVI can be a good choice for removal of OTC in aqueous solution. Response surface methodology (RSM) was used to optimize the amounts of NZVI and OTC to be used at pH 3 and under 200 W, UV-A irradiation. The responses were removal percent of absorption at 290 and 348 nm, TOC and COD of OTC. In the optimum condition, Linear model was performed 155 ppm of OTC were removed by 1000 ppm NZVI after 6.5 hours and the removal efficiency of absorption at 290 and 348 nm, TOC and COD were 87, 95, 85 and 89 percent, respectively. In the similar process, there is no organic compound after 14 hours. The parameters ORP, DO and pH were investigated for 6:30 hours to study the type of NZVI reaction in process. In the beginning of reaction, oxidation was the dominant reaction after 3 hours, photocatalytic reaction was remarkable. The mechanism of OTC degradation is proposed by HPLC/ESI-MS and four by products were found. Also the rate constants (first order kinetic chain reaction model) were 0.0099, 0.0021, 0.0010, 0.0049 and $0.0074min^{-1}$, respectively.

A Quinoline carboxamide based Fluorescent Probe's Efficient Recognition of Aluminium Ion and its Application for Real Time Monitoring

  • Manivannan, Ramalingam;Ryu, Jiwon;Son, Young-A
    • Textile Coloration and Finishing
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    • v.32 no.4
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    • pp.185-192
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    • 2020
  • A novel binding site for metal ion made by designing molecule with tetrazolo quinoline with hydrazine carboxamide (TQC) and the designed molecule successfully synthesized. The probe works by selectively detecting Al3+ ion via both fluorimetric and colorimetric approach. The probe's effectiveness towards aluminium ion detection is highly sensitive and selective with no substantial interference with other competing ions. The added Al3+ ion to TQC fetched a rapid change of visual color to yellow from colorless, also the response of fluorescence turn-on. The fluorescence turn-on and color change visibly by the probe TQC with Al3+ ion credited to the ICT phenomenon (intramolecular charge-transfer transition). The likely interaction of the probe with aluminium ion has also been there predicted from ESI-MS spectral analysis results. The usefulness of the probe confirmed by practical utility by making a test kit to monitor Al3+ ion in water which showed a naked eye detection by notable color change.