• Title/Summary/Keyword: MS analysis

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Analysis of Polymer Characteristics Using Matrix-assisted Laser Desorption/Ionization Time-of-flight Mass Spectrometry (말디토프 질량분석을 이용한 고분자의 특성분석)

  • Kang, Min-Jung;Seong, Yunseo;Kim, Moon-Ju;Kim, Myung Soo;Pyun, Jae-Chul
    • Applied Chemistry for Engineering
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    • v.28 no.3
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    • pp.263-271
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    • 2017
  • The application of mass spectrometry to polymer science has rapidly increased since the development of MALDI-TOF MS. This review summarizes current polymer analysis methods using MALDI-TOF MS, which has been extensively applied to analyze the average molecular weight of biopolymers and synthetic polymers. Polymer sequences have also been analyzed to reveal the structures and composition of monomers. In addition, the analysis of unknown end-groups and the determination of polymer concentrations are very important applications. Hyphenated techniques using MALDI-tandem MS have been used for the analysis of fragmentation patterns and end-groups, and also the combination of SEC and MALDI-TOF MS techniques is recommended for the analysis of complex polymers. Moreover, MALDI-TOF MS has been utilized for the observation of polymer degradation. Ion mobility MS, TOF-SIMS, and MALDI-TOF-imaging are also emerging technologies for polymer characterization because of their ability to automatically fractionate and localize polymer samples. The determination of polymer characteristics and their relation to the material properties is one of the most important demands for polymer scientists; the development of software and instrument for higher molecular mass range (> 100 kD) will increase the applications of MALDI-TOF MS for polymer scientists.

Identification of Novel Metabolic Proteins Released by Insulin Signaling of the Rat Hypothalmus Using Liquid Chromatography-Mass Spectrometry (LC-MS)

  • Chin, Chur
    • Journal of Korean Neurosurgical Society
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    • v.42 no.6
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    • pp.470-474
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    • 2007
  • Objective : The brain is dependent on glucose as an energy source. Intricate homeostatic mechanisms have been implicated in maintaining the blood glucose concentration in the brain. The aim of this study is to find the way to identify the metabolic proteins regulating the glucose in rat hypothalamus. Methods : In this study, we analysed the secretome from rat hypothalamus in vivo. We introduced 500 nM of insulin into the rat hypothalamus. The chromatographic patterns of the secretome were identified, after which Mass Spectrometry-Mass Spectrometry (MS-MS) analysis was performed. Results : In Liquid Chromatography-Mass Spectrometry (LC-MS) analysis, 60 proteins were identified in the secretome. Among them, 8 novel proteins were unveiled and were associated with the energy metabolism of insulin signaling in mitochondria of rat hypothalamic neuron. Nineteen other proteins have unknown functions. These ligands were confirmed to be secreting from the rat hypothalmus on insulin signaling by western blotting. Conclusion : The hypothalamus is the master endocrine gland responsible for the regulation of various physiological and metabolic processes. Proteomics using LC-MS analysis offer a efficient means for generating a comprehensive analysis of hypothalamic protein expression by insulin signaling.

A case study of MS Excel's powerful functions for statistical data analysis. (Focused on an Analysis of Variance menu) (자료 통계 분석을 위한 MS 엑셀의 유용한 기능들에 관한 사례연구 (지하철 이용객 자료 분석))

  • Kim, Sook-Young
    • Journal of the Korea Computer Industry Society
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    • v.9 no.5
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    • pp.223-228
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    • 2008
  • A case study to show MS Excel's convenient and powerful functions was conducted to test hypotheses with subway data. Quantitative variables were described using descriptive menu, and qualitative variables were described using histogram menu of a MS Excel software. Relationships were tested using regression menu, differences were tested using t-test menu, and factors were tested using variance-layout menu of a Excel software. Data input, management, and statistical analysis were done successfully with only a MS Excel software.

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Simultaneous Determination of Preservatives in Food by GC/MS (Gas Chromatography/Mass Spectrometry를 이용한 식품보존료의 동시분석방법 연구)

  • 김승기;노동석
    • Journal of Food Hygiene and Safety
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    • v.14 no.2
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    • pp.140-145
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    • 1999
  • Analytical method for preservatives in food was developed using gas chromatography/mass spectrometry (GC/MS). Propionic acid, sorbic acid, benzoic acid, ethyl salicylate, ethyl p-hydroxy benzoate, iso-propyl p-hydroxy benzoate, n-propyl p-hydroxy benzoate, iso-butyl p-hydroxy benzoate, n-butyl p-hydroxy benzoate, p-hydroxy benzoic acid and dehydro acetic acid were extracted from cooling beverage with diethyl ether. The polar hydroxyl and carboxyl groups of food preservatives were derivatized with N-methyl-N-tert-butyldimethylisilyl-trifluoroscetamide (MTBSTFA) to form the corresponding tert-bytyldimethyl-silylated derivatives, and submitted to GC/MS analysis. The mass spectra of the derivatives were investigated for the selection of monitoring ions for multi-residue analysis of 11 preservatives by GC/MS. The macro program was also developed for the qualitative analysis of these preservatives in food.

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Method for Simultaneous Determination of Cyanotoxins in Water by LC-MS/MS (액체크로마토그래프/질량분석기를 이용한 수중 남조독소물질 동시분석법)

  • Kim, Jeong-Hee;Yun, Mi-Ae;Kim, Hak-Chul
    • Journal of Korean Society on Water Environment
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    • v.25 no.4
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    • pp.597-605
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    • 2009
  • Algae bloom occurred in reservoir in summer can cause taste and odor in water and disturb the flocculation and sedimentation processes in water treatment plant and cause sand filter plugging. It was also reported that microcystins, anatoxin and saxitoxin released from cyanobacteria had acute toxic effects on liver and nervous system. For these reasons, many advanced countries inclusive of WHO set the guideline for these toxins and cyanotoxins have been managed with regular monitoring in Korea as well. However, complex sample preparation steps such as a solid phase extraction (SPE) and derivatization are required with an existing analysis method with HPLC. We needed to improve an analysis method for low extraction efficiency and long sample preparation time. In this study, we have established a new LC/MS/MS method which can simultaneously determine 6 cyanotoxins (Microcystins-LR, Microcystins-RR, Microcystins-YR, Anatoxin-a, Saxitoxin, Neosaxitoxin) with only simple filtration step. When $75{\mu}L$ filterated sample was injected onto the LC-MS/MS, the recovery ranged from 86% to 112% and the MDL was $0.025{\sim}0.581{\mu}g/L$. We can make the MDL be lower than the guideline ($1{\sim}3{\mu}g/L$) of advanced countries with simple preparation.

MALDI-MS: A Powerful but Underutilized Mass Spectrometric Technique for Exosome Research

  • Jalaludin, Iqbal;Lubman, David M.;Kim, Jeongkwon
    • Mass Spectrometry Letters
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    • v.12 no.3
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    • pp.93-105
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    • 2021
  • Exosomes have gained the attention of the scientific community because of their role in facilitating intercellular communication, which is critical in disease monitoring and drug delivery research. Exosome research has grown significantly in recent decades, with a focus on the development of various technologies for isolating and characterizing exosomes. Among these efforts is the use of matrix-assisted laser desorption ionization (MALDI) mass spectrometry (MS), which offers high-throughput direct analysis while also being cost and time effective. MALDI is used less frequently in exosome research than electrospray ionization due to the diverse population of extracellular vesicles and the impurity of isolated products, both of which necessitate chromatographic separation prior to MS analysis. However, MALDI-MS is a more appropriate instrument for the analytical approach to patient therapy, given it allows for fast and label-free analysis. There is a huge drive to explore MALDI-MS in exosome research because the technology holds great potential, most notably in biomarker discovery. With methods such as fingerprint analysis, OMICs profiling, and statistical analysis, the search for biomarkers could be much more efficient. In this review, we highlight the potential of MALDI-MS as a tool for investigating exosomes and some of the possible strategies that can be implemented based on prior research.

Sample Preparation for Matrix-Assisted Laser Desorption/Ionization Mass Spectrometry

  • Kim, Jeongkwon
    • Mass Spectrometry Letters
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    • v.6 no.2
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    • pp.27-30
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    • 2015
  • This article reviews the fundamentals of sample preparation used in matrix-assisted laser desorption/ionization-mass spectrometry (MALDI-MS). MALDI is a soft ionization method used to generate analyte ions in their intact forms, which are then detected in MS analysis. MALDI-MS boasts fast analysis times and easy-to-use operation. The disadvantages of MALDI-MS include the occurrence of matrix-associated peaks and inhomogeneous distribution of analyte within the matrix. To overcome the disadvantages of MALDI-MS, various efforts have been directed such as using different matrices, novel matrix systems, various additives, and different sample preparation methods. These various efforts will be discussed in detail. This article will benefit those who would like to obtain basic knowledge of MALDI sample preparation and those who would like to use MALDI-MS in their chemical analyses.

Quantitative Analysis of amphetamines in hair by EI-GC-MS using SIM mode with uncertainty estimation

  • Yang, Won-Kyung;Han, Eun-Young;Lee, Jae-Sin;Park, Yong-Hoon;Kim, Eun-Mi;Lim, Mi-Ae;Chung, Hee-Sun
    • Proceedings of the PSK Conference
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    • 2003.04a
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    • pp.169.2-169.2
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    • 2003
  • A method using EI-GC-MS is described for the determination of amphetamines in hair. The method is applied to simultaneous quantify amphetamines (methamphetamine, amphetamine, MDMA and MDA). Drugs were extracted in 1 % HCl in methanol from hair. After derivertization with TFAA, the resulting drugs were separated on HP-5MS column during a 16 min program and identified by mass spectrometry with the SIM mode(EI-GC-MS). (omitted)

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Quality Characteristics of Sulgidduk Added with Makgeolli (막걸리 첨가 설기떡의 품질 특성)

  • Shim, Eun Kyoung;Kim, Hyun Jeong;Lee, Su Jin;Kim, Mee Ree
    • Journal of the Korean Society of Food Culture
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    • v.29 no.6
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    • pp.605-614
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    • 2014
  • The objective of this study was to investigate the quality characteristics of Baeksulgi (BS) and Sulgidduk added with Makgeolli (MS, BS+ Makgeolli) during storage at $20{\pm}2$ for 3 days. Moisture contents of MS were significantly higher than those of BS during storage. Reducing sugar contents (%) were higher in MS. The pH values were 6.23 and 5.93, for BS and MS, respectively. The pH of MS was lower and thus indicated higher in acidity. The Hunter color L (lightness) and a (redness) values were higher for BS, whereas b (yellowness) value of MS was lower. In the texture analysis, hardness and chewiness of MS were found to be lower, whereas springiness, gumminess, and resilience were higher than those of MS. According to DSC (Differential scanning calorimeter) analysis, enthalpy of MS appeared to be lower than that of BS during storage, which suggests retrogradation of MS was delayed. The total phenol content was higher in MS. The $IC_{50}$ value of DPPH and hydroxyl radical scavenging activity was lower in MS, which means antioxidant activity increased in MS. Results of the preference test showed that appearance, flavor, taste, and overall acceptability of MS scored higher than those of BS. From these results, high quality of MS was derived from Makgeolli addition.

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.