• Title/Summary/Keyword: electrospray ionization (ESI)

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Profiling of the leaves and stems of Curcuma longa using LC-ESI-MS and HPLC analysis

  • Gia Han Tran;Hak-Dong Lee;Sun-Hyung Kim;Seok Lee;Sanghyun Lee
    • Journal of Applied Biological Chemistry
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    • v.66
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    • pp.338-344
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    • 2023
  • Curcuma longa is a plant belonging to the genus Curcuma and is distributed across various Asian regions. This plant is widely known for its rhizomes, which possess a variety of pharmacological properties. However, although the leaves and stems of this plant also contain several health-promoting secondary metabolites, very few studies have characterized these compounds. Therefore, our study sought to quantify the secondary metabolites from the leaves and stems of Curcuma longa L. (LSCL) using liquid chromatography-electrospray ionization-mass spectrometry (LC-ESI-MS) and high-performance liquid chromatography (HPLC). Our LC-ESI-MS analyses detected twenty-one phenolic compounds in the LSCL, among which fifteen compounds were detected via HPLC analysis. Four compounds, namely vanillic acid (0.129 mg/g), p-coumaric acid (0.431 mg/g), 4-methylcatechol (0.199 mg/g), and afzelin (0.074 mg/g) were then quantified. These findings suggest that LSCL is rich in secondary metabolites and holds potential as a valuable resource for the development of functional and nutritional supplements in the future.

A Simple and Sensitive High Performance Liquid Chromatography-Electrospray Ionization/Mass Spectrometry Method for the Quantification of Ethyl Pyruvate in Rat Plasma

  • Kim, Hyun-Ji;Kim, Seung-Woo;Lee, Ja-Kyeong;Yoon, Sung-Hwa
    • Bulletin of the Korean Chemical Society
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    • v.32 no.4
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    • pp.1221-1227
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    • 2011
  • Ethyl pyruvate (EP) is known as a scavenger of reactive oxygen species (ROS) in the body through its role in the donation of diketone groups to metals to form an EP-metal complex. In order to develop a method for the quantification of EP in biological media, a sensitive and specific, high-performance liquid chromatographyelectrospray ionization-mass spectrometry (HPLC-ESI/MS) method is used to determine the EP-alkali metal ion binding species. The analyte was separated on a ZORBOX SB-C8 ($3.5{\mu}m$, $30mm{\times}2.1mm$ I.D.) column and analyzed in selected ion monitoring (SIM) mode with a positive ESI interface using the m/z 255 $[2M + Na]^+$ ion. The method was validated over the concentration range of $0.5-60.0\;{\mu}g$/mL under 1/9 (v/v) of acetonitrile/methanol solvent system with flow rate 0.05 mL/min. The limit of quantification (LOQ) was $0.5{\mu}g$/mL.

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.

Determination of thyroid hormones in plasma samples by high performance liquid chromatograph/diode array detector/electrospray ionization mass spectrometer (HPLC/DAD/ESI-MS를 이용한 혈장시료 중 갑상선 호르몬 분석)

  • Kwak, Sun Young;Moon, Myeong Hee;Pyo, Heesoo
    • Analytical Science and Technology
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    • v.20 no.5
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    • pp.424-433
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    • 2007
  • An analytical method for the determination of thyroid hormones in plasma samples has been studied by solid-phase extraction and high-performance liquid chromatography/diode array detector (DAD)/electrospray ionization (ESI)-mass spectrometer. Seven thyroid hormones were successfully separated by gradient elution on the reverse phase Hypersil ODS column (4.6 mm I.D., 250 mm length, particle size $5{\mu}m$) with ammonium formate buffer and acetonitrile. In addition, these compounds were confirmed by UV spectra and ESI-mass Spectra. The extraction recoveries of thyroid hormones in the plasma sample (at pH 3) were in the range of 74.5-115.7 % with solid-phase extraction by C18, followed by elution with 4 mL of methanol. The calibration curves showed good linearity with the correlation coefficients ($r^2$) varying from 0.9939 to 0.9978 and the detection limits of all analytes were obtained in the range of 20-50 ng/mL (38.1-162.8 pmol/mL). As a result, thyroxine was found in the range of 50.98-112.97 ng/mL in normal plasma samples.

Phospholipid Analysis by Nanoflow Liquid Chromatography-Tandem Mass Spectrometry

  • Moon, Myeong Hee
    • Mass Spectrometry Letters
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    • v.5 no.1
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    • pp.1-11
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    • 2014
  • Lipids play important roles in biological systems; they store energy, play a structural role in the cell membrane, and are involved in cell growth, signal transduction, and apoptosis. Phospholipids (PLs) in particular have received attention in the medical and lipidomics research fields because of their involvement in human diseases such as diabetes, obesity, atherosclerosis, and many cancers associated with lipid metabolic disorders. Here I review experimental strategies for PL analysis based on nanoflow liquid chromatography-electrospray ionization-tandem mass spectrometry (nLC-ESI-MSn). In particular, discussed are lipid extraction methods, nanoflow LC separation of PLs, effect of ionization modifiers on the ESI of PLs, influence of chain lengths and unsaturation degree of acyl chains of PLs on MS intensity, structural determination of the molecular structure of PLs and their oxidized products, and quantitative profiling of PLs from biological samples such as tissue, urine, and plasma in relation to cancer and coronary artery disease.

Sheathless electrospray ionization with integrated metal emitter on microfluidic device (전기 분무 이온화를 이용한 단백질 질량분석용 마이크로 유체 소자의 제작 및 실험)

  • Kim, Min-Su;Joo, Hwang-Soo;Lee, Kook-Nyung;Kim, Byung-Gee;Kim, Yong-Kweon
    • Proceedings of the KIEE Conference
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    • 2004.07c
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    • pp.2102-2104
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    • 2004
  • In this study, sheathless electrospray from PDMS/glass microchips with conducting metal emitter tip is described. A chip-based capillary electrophoresis/mass spectrometry (CE/MS) system has advantages of the CE separation and on-line electrospray detection of peptide solution. We have fabricated a new electrospray ionization(ESI) device composed of the metal emitter tip and CE separation channel monolithically in a glass microchip. The separation channel and metal emitter tip are fabricated using a glass wet etching and gold electro plating process, respectively. The fabricated micro electrospray chip was tested by spraying peptide sample for mass spectrometric analysis. Singlely-charged peak and doublely-charged peak of peptide were detected and further MS/MS fragmentation was performed in each peak. Direct comparisons with conventional glass or fused silica emitters showed very similar performance with respect to signal strength and stability.

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Determination of nucleosides in human urine by high-performance liquid chromatography with electrospray ionization mass spectrometry(LC/ESI-MS)

  • Lee, Sang-Hee;Jung, Byung-Hwa;Kim, Sun-Yeou;Kim, Ho-Cheol;Chung, Bong-Chul
    • Proceedings of the PSK Conference
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    • 2003.04a
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    • pp.290.1-290.1
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    • 2003
  • Oxidative DNA damage has been associated with many disease. Quantation of DNA adducts is considered to be a useful biomarker of oxidative DNA damage because its formation can also be induced by oxidative stress. Extensive efforts have been taken to identify the analytical methods for minimizing the artifactual formation of oxidative DNA damage. We have done direct analysis of DNA adducts using LC/ESI-MS without urine sample extraction. (omitted)

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Examination of Various Metal Ion Sources for Reducing Nonspecific Zinc finger-Zn2+ Complex Formation in ESI Mass Spectrometry

  • Park, Soo-Jin;Park, Sun-Hee;Oh, Joo-Yeon;Han, Sang-Yun;Jo, Kyu-Bong;Oh, Han-Bin
    • Mass Spectrometry Letters
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    • v.3 no.3
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    • pp.82-85
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    • 2012
  • The formation of zinc finger peptide-$Zn^{2+}$ complexes in electrospray ionization mass spectrometry (ESI-MS) was examined using three different metal ion sources: $ZnCl_2$, $Zn(CH_3COO)_2$, and $Zn(OOC(CHOH)_2COO)$. For the four zinc finger peptides (Sp1-1, Sp1-3, CF2II-4, and CF2II-6) that bind only a single $Zn^{2+}$ in the native condition, electrospray of apo-zinc finger in solution containing $ZnCl_2$ or $Zn(CH_3COO)_2$ resulted in the formation of zinc finger-$Zn^{2+}$ complexes with multiple zinc ions. This result suggests the formation of nonspecific zinc finger-$Zn^{2+}$ complexes. Zn(tartrate), $Zn(OOC(CHOH)_2COO)$, mainly produced specific zinc finger-$Zn^{2+}$ complexes with a single zinc ion. This study clearly indicates that tartrate is an excellent counter ion in ESI-MS studies of zinc finger-$Zn^{2+}$ complexes, which prevents the formation of nonspecific zinc finger-$Zn^{2+}$ complexes.

Characterization of Basic Nitrogen-Containing Compounds in the Products of Lube Base Oil Processing by Electrospray Ionization Fourier Transform Ion Cyclotron Resonance Mass Spectrometry

  • Li, Xiaohui;Zhu, Jianhua;Wu, Bencheng
    • Bulletin of the Korean Chemical Society
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    • v.35 no.1
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    • pp.165-172
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    • 2014
  • The distribution of basic nitrogen-containing compounds in three vacuum gas oils (VGOs) with different boiling ranges and their dewaxed oils from the lube base oil refining unit of a refinery were characterized by positive-ion electrospray ionization (ESI) Fourier transform-ion cyclotron resonance mass spectrometry (FT-ICR MS). It turned out that the composition of basic nitrogen compounds in the samples varied significantly in DBE and carbon number, and the dominant basic N-containing compounds in these oil samples were N1 class species. $N_1O_1$, $N_1O_2$, and $N_2$ class species with much lower relative abundance were also identified. The composition of basic nitrogen compounds in VGOs and dewaxed VGOs were correlated with increased boiling point and varied in DBE and carbon numbers. The comparison of the analytical results between VGOs and dewaxed VGOs indicated that more basic N-containing compounds in VGO with low carbon number and small molecular weight tend to be removed by solvent refining in lube base oil processing.

Development of a Four-way Interface for Online Capillary Isoelectric Focusing-Electrospray-Mass Spectrometry (CIEF-ESI-MS)

  • Yu, Hai Dong;Kim, Byungjoo;Shin, Dae-Ho;Ahn, Seonghee
    • Mass Spectrometry Letters
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    • v.4 no.4
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    • pp.83-86
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    • 2013
  • A new interface for coupling CIEF and MS using a four-way cross has been developed in a single mechanical system. This new interface could be operated without the electric discontinuity and reinstallation of lines. Additionally, a bare fused silica capillary was facilitated as a spray needle to produce electrospray and to guide catholyte or sheath liquid. Focusing for CIEF was completed in a hanging droplet at the end of spray needle. This capillary spray needle also provided stable spray, enhanced the ionization efficiency and increased sensitivity. Results with carbonic anhydrase I showed that focusing and spraying were well completed with the new interface and the new spray needle.