• Title/Summary/Keyword: LC-MS-MS

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Analysis of Photodegradation Products of Organic Photochromes by LC/MS

  • Lim, Young-Hee;Youn, Yeu Young;Kim, Kyung Hoon;Cho, Hye-Sung
    • Mass Spectrometry Letters
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    • v.3 no.4
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    • pp.101-103
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    • 2012
  • The ultraviolet (UV) degradation products of photochromic naphthoxazine and naphthopyran derivatives in acetonitrile were separated and identified using liquid chromatography-mass spectrometry (LC-MS). Photodegradation resulted in oxidation of products.

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.

Sensitive Determination of Felodipine in Human Plasma by LC-MS/MS

  • Kim, Ho-Hyun;Roh, Hyeon-Jin;Lee, He-Joo;Han, Sang-Beom
    • Proceedings of the PSK Conference
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    • 2003.04a
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    • pp.283.2-283.2
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    • 2003
  • This study established a highly sensitive novel quantification method for detecting felodipine in human plasma using LC-MS/MS. The mobile phase used after degassing was composed of 1 mM ammonium acetate and acetonitrile (20:80, pH 6.0), with flow rate of 200 uL/min. One mL plasma were pipetted into glass tubes and spiked with 0.1 mL of internal standard solution. (omitted)

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Determination of Glimepiride in Human Plasma by LC-MS/MS

  • Kim, Ho-Hyun;Roh, Hyeong-Jin;Lee, Hee-Joo;Han, Sang-Beom
    • Proceedings of the PSK Conference
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    • 2003.04a
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    • pp.282.1-282.1
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    • 2003
  • This study established a sensitive novel Quantification method for detecting glimepiride in human plasma using LC-MS/MS for pharmacokinetic studies. The mobile phase used after degassing was composed of 10 mM ammonium acetate and acetonitrile (20:80, pH 3.0), with flow rate of 200uL/min. One mL plasma were pipetted into glass tubes and spiked with 0.1 mL of internal standard solution. (omitted)

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Establishment of the Analytical Method for Residual Pharmaceuticals in Raw Water Using Online Sample Preparation and High Resolution Orbitrap LC/ESI-MS (온라인 자동화 시료 전처리 및 HR Orbitrap LC/ESI-MS를 이용한 환경시료 중 잔류 의약물질 분석방법 확립)

  • Hwang, Yoonjung;Sin, Sanghee;Park, Jongsuk
    • Journal of Korean Society on Water Environment
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    • v.29 no.3
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    • pp.409-419
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    • 2013
  • In this study, the analytical method for 27 residual pharmaceuticals in raw water was developed. Online sample preconcentration/extraction and analysis with high resolution Orbitrap mass spectrometry (LC-ESI/Orbitrap MS) were performed. The calibration curves showed good linearities (above $r^2$ = 0.998) in the range of 5 ~ 1,000 ng/L. The method detection limit and the limit of quantification were 1.1 ~ 10.0 ng/L and 3.4 ~ 31.7 ng/L, respectively. Recoveries of the target compounds were between 70.1% and 115.8% (except cefadroxil, cefradine, vancomycin, and iopromide (50.2 ~ 67.0%)). The optimized analytical method can be useful to determine the residual pharmaceuticals in raw water.

Development of an Isotope Dilution Mass Spectrometry (IDMS)-Based Method for the Analysis of Ibuprofen

  • Lee, Joonhee;Kim, Byungjoo
    • Mass Spectrometry Letters
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    • v.8 no.3
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    • pp.49-52
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    • 2017
  • Ibuprofen is one of the most popular analgesic and antipyretic drugs. An isotope dilution mass spectrometry method based on LC/MS was developed as a candidate reference method for the accurate determination of ibuprofen in pharmaceutical tablets. Isotope labelled ibuprofen, $ibuprofen-d_3$, was added as an internal standard into sample extracts. Ibuprofen and $ibuprofen-d_3$, was analysed by LC/MS in a selected ion monitoring (SIM) mode to detect ions at m/z 205 and 208, respectively. The repeatability and reproducibility of the developed ID-LC/MS method were tested for the validation and assessment of metrological quality of the method.

An Evaluation of Liquid Chromatography/Mass Specrometry with Atmospheric Pressure Chemical Ionizarion for the Rapid and Simultaneous Measurement of Carbamate Pesticides and Organophosphorus Pesticides

  • Kim, Byeong Ju;So, Hyeon Yeong
    • Bulletin of the Korean Chemical Society
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    • v.21 no.5
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    • pp.471-476
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    • 2000
  • Liquid chromatography/mass spectrometry with an atmospheric pressure chemical ionization interface (LC/APCI/MS) is evaluated for the simultaneous determination of carbamate pesticides and organophosphorus pesticides in a single chromatographic analysis. APCI mass spectra of those compounds were obtrained to study their ionization characteristics. APCI provided abundant ions such as protonated molecules and characteristic fragment ions for carbamate pesticides and organophosphorus pesticides. To evaluate the feasibility of the LC/APCI/MS for a routine quantitative analysis, the linearity and repeatability of LC/APCI/MS were examined by measuring standard solution mixtures of five carbamate pesticides and four organophosphorus pesticides over the range of 1 to 100 ㎍/mL. Teh peak areas in chromatograms of characteristic ions for those compounds showed less than 3% of variation from run to run. The standard calibration curves for the nine pesticides show good linearity in the concentration range. The detection limits of the LC/APCI/MS system for those compounds range from 0.006 to 0.2 ng.

Effects of Column Length and Particle Diameter on Phospholipid Analysis by Nanoflow Liquid Chromatography-Electrospray Ionization-Mass Spectrometry

  • Lee, Ju-Yong;Lim, Sang-Soo;Moon, Myeong-Hee
    • Mass Spectrometry Letters
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    • v.2 no.3
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    • pp.65-68
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    • 2011
  • The effects of column length and particle size on the efficiency of separation and characterization of phospholipids (PLs) are investigated using nanoflow liquid chromatography-electrospray ionization-tandem mass spectrometry (nLC-ESI-MS-MS). Since PLs are associated with cell proliferation, apoptosis, and signal transduction, it is of increasing interests in lipidomics to establish reliable analytical methods for the qualitative and quantitative profiling of PLs related to biomarker development in adult diseases. Due to the complexity of PLs, the preliminary separation of PLs is necessary prior to MS analysis. In this study, length of capillary column and the particle size of reversed phase ($C_{18}$) packing materials are varied to find a reliable condition for the high speed and high resolution separation using 8 PL standard mixtures. From experiments, it was found that a capillary column of nLC-ESI-MS-MS analysis for PL mixtures can be minimized to a 5 cm long pulled tip column packed with 3 ${\mu}m$ $C_{18}$ particles without losing resolution.

Comparison of Liquid Chromatography-Mass/Mass Spectrometry (MS) and Gas Chromatography-MS for Quantitative Analysis of Indole-3-acetic acid and Indole-3-butyric acid from the Concentrated Liquid Fertilizer (Liquid Chromatography-Mass/Mass Spectrometry (MS)와 Gas Chromatography-MS를 이용한 농축 액상 비료제품 중 Indole-3-acetic acid 및 Indole-3-butyric acid 정량분석능 비교)

  • Kim, Jin Hyo;Park, Jong Min;Choi, Geun-Hyoung;Park, Yun-Ki;Im, Geon-Jae;Kim, Doo-Ho;Kwon, Oh-Kyung
    • Journal of Applied Biological Chemistry
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    • v.56 no.1
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    • pp.53-57
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    • 2013
  • In here, we investigated the quantitative analysis method of indole-3-acetic acid (IAA) and indole-3-butyric acid (IBA) with liquid chromatography-mass/mass spectrometry (LC-MS/MS) or gas chromatography-MS. Two ways of clean-up process were investigated for LC-MS/MS instrumental analysis of IAA, but both a simple dilution and hydrophile-lipophile balance (HLB) solid phase extraction (SPE) were not met the optimal recovery rates for quantitative analysis. On the other hand, the clean-up method for GC-MS was finally optimized through HLB-SPE from 250-folds diluted sample and methylation with trimethylsilyl chloride in methanol for 4 h. The limit of detection for methyl ester of IAA and IBA were both 1.4 mg/L, and recovery rates showed 93-107% from the concentrated liquid fertilizer.