• Title/Summary/Keyword: Liquid Chromatography-mass Spectroscopy

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Identification of New Urinary Metabolites of Byakangelicin, a Component of Angelicae dahuricae Radix, in Rats

  • Kwon, Oh-Seung;Song, Yun-Seon;Shin, Kuk-Hyun;Ryu, Jae-Chun
    • Archives of Pharmacal Research
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    • v.26 no.8
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    • pp.606-611
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    • 2003
  • Byakangelicin, 9-(2,3-dihydroxy-2-methylbutoxy)-4-methoxy-7H- furo[3,2-g][l]benzopyran-7-one (BKG), a component of Angelicae dahuricae Radix, is considered to be an inhibitor of aldose reductase for the treatment of diabetic cataract. An analytical method for the isolation of BKG developed by high-performance liquid chromatography has been reported. No literature on the metabolism of BKG, however, has been found. With the purpose of identifying new metabolites of BKG, BKG (100 mg/kg) was orally administered to Sprague-Dawley rats via a gavage. Using a metabolic cage, urine was collected for 24 h, and the urine samples were extracted by liquid-liquid extraction. For structural identification of new urinary metabolites of BKG, various instrumental analyses were conducted by gas-chromatography/mass spectrometry, high-performance liquid chromatography/diode array detector, liquid chromatography/mass spectroscopy with thermospray interface and $^1H$ nuclear magnetic resonance spectroscopy. Two metabolites produced from the Ο-demethylation or Ο-dealkylation of BKG were newly identified, and another new but unknown metabolite was assumed to be the hydroxylated form of BKG. These results indicate that the major metabolic products of BKG are formed by Ο-demethylation or Ο-dealkylation of BKG side chains.

Improved Calibration for the Analysis of Emerging Contaminants in Wastewater Using Ultra High Performance Liquid Chromatography and Time-of-Flight Mass Spectrometry

  • Pellinen, Jukka;Lepisto, Riikka-Juulia;Savolainen, Santeri
    • Mass Spectrometry Letters
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    • v.9 no.3
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    • pp.77-80
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    • 2018
  • The focus of this paper is to present techniques to overcome certain difficulties in quantitative analysis with a time-of-flight mass spectrometer (TOF-MS). The method is based on conventional solid-phase extraction, followed by reversed-phase ultra high performance liquid chromatography of the extract, and mass spectrometric analysis. The target compounds included atenolol, atrazine, caffeine, carbamazepine, diclofenac, estrone, ibuprofen, naproxen, simazine, sucralose, sulfamethoxazole, and triclosan. The matrix effects caused by high concentrations of organic compounds in wastewater are especially significant in electrospray ionization mass spectroscopy. Internal-standard calibration with isotopically labeled standards corrects the results for many matrix effects, but some peculiarities were observed. The problems encountered in quantitation of carbamazepine and triclosan, due to nonlinear calibration were solved by changing the internal standard and using a narrower mass window. With simazine, the use of a quadratic calibration curve was the best solution.

Utilization of Liquid Chromatography Mass Spectroscopy for Screening Analysis of Acetogenins in Extracts of Asimina triloba Leaves (포포나무 잎 추출물에 존재하는 Acetogenin 확인을 위한 액체크로마토그래피 질량분석기의 활용)

  • Im, Do-Youn;Lee, Kyoung-In
    • Korean Journal of Pharmacognosy
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    • v.49 no.3
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    • pp.278-284
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    • 2018
  • Asimina triloba contains many kinds of annonaceous acetogenins known to have toxicity and/or activity. In this study, analysis of acetogenins was carried out on the extract and its solvent fractions of A. triloba leaves using a liquid chromatography mass spectroscopy(LC-MS). In the extract, the ethanolic extract was significantly higher acetogenin contents than hot water extract. In the analysis of solvent fraction from the ethanolic extract, n-hexane, ethylacetate, and aqueous fraction were contained 85.17~90.92%, 8.96~14.52% and 0.12~0.35% of total acetogenin in the extract. Based on these results, the analytical method is useful for comparing annonaceous acetogenins contents in plant samples. Moreover, when research or product development aiming at the physiological activity of acetogenin such as anticancer activity using A. triloba leaves is performed, a fractionation using a nonpolar organic solvents and alcohol extract may be useful methods. This method can also be used for the purpose of eliminating toxicity as well.

NEAR INFRARED TRANSFLECTANCE SPECTROSCOPY (NIRS) IN PHYTOCHEMISTRY

  • Huck, C.W.;W.Guggenbichler;Bonn, G.K.
    • Proceedings of the Korean Society of Near Infrared Spectroscopy Conference
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    • 2001.06a
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    • pp.3114-3114
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    • 2001
  • During the last years phytochemistry and phytopharmaceutical applications have developed rapidly and so there exists a high demand for faster and more efficient analysis techniques. Therefore we have established a near infrared transflectance spectroscopy (NIRS) method that allows a qualitative and quantitative determination of new polyphenolic pharmacological active leading compounds within a few seconds. As the NIR spectrometer has to be calibrated the compound of interest has at first to be characterized by using one or other a combination of chromatographic or electrophoretic separation techniques such as thin layer chromatography (TLC), high performance liquid chromatography (HPLC), capillary electrophoresis (CE), gas chromatography (GC) and capillary electrochromatography (CEC). Both structural elucidation and quantitative analysis of the phenolic compound is possible by direct coupling of the mentioned separation methods with a mass spectrometer (GC-MS, LC-MS/MS, CE-MS, CEC-MS) and a NMR spectrometer (LC-NMR). Furthermore the compound has to be isolated (NPLC, MPLC, prep. TLC, prep. HPLC) and its structure elucidated by spectroscopic techniques (UV, IR, HR-MS, NMR) and chemical synthesis. After that HPLC can be used to provide the reference data for the calibration step of the near infrared spectrometer. The NIRS calibration step is time consuming, which is compensated by short analysis times. After validation of the established NIRS method it is possible to determine the polyphenolic compound within seconds which allows to raise the efficiency in quality control and to reduce costs especially in the phytopharmaceutical industry.

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MEASUREMENT OF PESTICIDES RESIDUES USING SPECTROSCOPY ON AGRICULTURAL PRODUCTS

  • Kim, Y. W.;S. H. Noh
    • Proceedings of the Korean Society for Agricultural Machinery Conference
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    • 2000.11c
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    • pp.525-532
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    • 2000
  • A new spectroscopic method for pesticide residues detection on agricultural products was developed. The general determination methods are high performance liquid chromatography (HPLC), gas chromatography (GC) or GC-mass spectrometry. They have provided relatively good detection limit and accuracy with complicated and time-consuming (5hrs above) procedures. In addition freshness is very important for evaluating qualities of agricultural products. This requires a simple and fast method for detection of pesticides. Reflectance, transmittance and fluorescence spectrometry of pesticides were tested using UV range because most of pesticides contain conjugation band in the molecular structures. Fluorescence spectrometry showed better sensitive to detect pesticide residues than did reflectance and transmittance spectrometry. Intensity and shape of fluorescence spectra showed different patterns with different structures of pesticides. Detection limit for fluorescence spectrometry was 0.1 ppm to 10 ppm depending on the structures of pesticides. Application of fluorescence spectrometry appears to be an easy method for detection of pesticide residues on agricultural products.

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Phytochemical analysis of Panax species: a review

  • Yang, Yuangui;Ju, Zhengcai;Yang, Yingbo;Zhang, Yanhai;Yang, Li;Wang, Zhengtao
    • Journal of Ginseng Research
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    • v.45 no.1
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    • pp.1-21
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    • 2021
  • Panax species have gained numerous attentions because of their various biological effects on cardiovascular, kidney, reproductive diseases known for a long time. Recently, advanced analytical methods including thin layer chromatography, high-performance thin layer chromatography, gas chromatography, high-performance liquid chromatography, ultra-high performance liquid chromatography with tandem ultraviolet, diode array detector, evaporative light scattering detector, and mass detector, two-dimensional high-performance liquid chromatography, high speed counter-current chromatography, high speed centrifugal partition chromatography, micellar electrokinetic chromatography, high-performance anion-exchange chromatography, ambient ionization mass spectrometry, molecularly imprinted polymer, enzyme immunoassay, 1H-NMR, and infrared spectroscopy have been used to identify and evaluate chemical constituents in Panax species. Moreover, Soxhlet extraction, heat reflux extraction, ultrasonic extraction, solid phase extraction, microwave-assisted extraction, pressurized liquid extraction, enzyme-assisted extraction, acceleration solvent extraction, matrix solid phase dispersion extraction, and pulsed electric field are discussed. In this review, a total of 219 articles published from 1980 to 2018 are investigated. Panax species including P. notoginseng, P. quinquefolius, sand P. ginseng in the raw and processed forms from different parts, geographical origins, and growing times are studied. Furthermore, the potential biomarkers are screened through the previous articles. It is expected that the review can provide a fundamental for further studies.

Characterization of Triterpenoids, Flavonoids and Phenolic Acids in Eclipta prostrata by High-performance Liquid Chromatography/diode-array Detector/electrospray Ionization with Multi-stage Tandem Mass Spectroscopy

  • Lee, Ki-Yong;Ha, Na-Ry;Kim, Tae-Bum;Kim, Young-Choong;Sung, Sang-Hyun
    • Natural Product Sciences
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    • v.16 no.3
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    • pp.164-168
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    • 2010
  • High-performance liquid chromatographic method with diode-array detector and electrospray ionization with multi-stage tandem mass spectroscopy (HPLC/DAD/ESI-$MS^n$) was used to identify the major constituents in a methanolic extract of Eclipta prostrata. The chromatographic separation was performed on a C18 column. Acetonitrile-water was used as a mobile phase. HPLC/DAD/ESI-$MS^n$ allowed the characterization of constituents of E. prostrata, mainly triterpenoids (eclalbasaponin I, II, III, IV, VI), flavonoids (luteolin 7-O-glucoside, demethylwedelolactone, wedelolactone, luteolin, demetylwedelolactone sulfate, luteolin sulfate, apigenin sulfate) and phenolic acids (5-O-caffeoylquinic acid, 3, 4-O-dicaffeoylquinic acid, 3, 5-O-dicaffeoylquinic acid, 4, 5-Odicaffeoylquinic acid).

Separation of Lipid-Soluble Component to Decrease Thermal Oxidation of Lard from Spinach (Spinacia oleracea)

  • Hwang, A-Reum;Kim, Moon-Jung;Choe, Eun-Ok
    • Food Science and Biotechnology
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    • v.15 no.2
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    • pp.220-226
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    • 2006
  • Component having antioxidant activity on lard during heating was separated from hexane extract of spinach, and its characteristic chemical structure was speculated through nuclear magnetic resonance spectroscopy, liquid chromatography-mass spectrometry, and Fourier transform infrared spectrophotometry. Lard was heated with hexane-, ethyl ether-, ethyl acetate-, or ethanol extract of spinach at $180^{\circ}C$ for 20 hr. Hexane extract of spinach, having highest antioxidant activity on lard during heating, was fractionated by silicic acid column chromatography (SACC), and SACC fractions having higher antioxidant activity on lard during heating were further separated by thin layer chromatography (TLC). Isolated compound from SACC fractions of hexane extract of spinach by TLC had sugar moieties and benzene ring along with hydroxy, carbonyl, and alkyl groups in the structure.

Isolation and Identification of Free Phenolic Acids in Korean Ginseng (인삼의 유리 페놀성 분획중 phenolic acid의 순수분리 동정)

  • Kim, Man-Wook;Wee, Jae-Joon;Park, Jong-Dae
    • Korean Journal of Food Science and Technology
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    • v.19 no.5
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    • pp.392-396
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    • 1987
  • A method for isolation of some phenolic acids from Korean ginseng(Panax ginseng C.A.Meyer)was studied using silicic acid column chromatography. preparative thin layer chromatography and high performance liquid chromatography. Two phenolic compounds were isolated and identified as ferulic acid, mp $156-157^{\circ}C$ and vanillic acid. mp $154-156^{\circ}C$ by spectral data of Mass and NMR spectroscopy.

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In situ isolation and characterization of the biosurfactants of B. Subtilis

  • Akthar, Wasim S.;Aadham, Mohamed Sheik;Nisha, Arif S.
    • Advances in environmental research
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    • v.9 no.3
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    • pp.215-232
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    • 2020
  • Crude oils are essential source of energy. It is majorly found in geographical locations beneath the earth's surface and crude oil is the main factor for the economic developments in the world. Natural crude oil contains unrefined petroleum composed of hydrocarbons of various molecular weights and it contains other organic materials like aromatic compounds, sulphur compounds, and many other organic compounds. These hydrocarbons are rapidly getting degraded by biosurfactant producing microorganisms. The present study deals with the isolation, purification, and characterization of biosurfactant producing microorganism from oil-contaminated soil. The ability of the microorganism producing biosurfactant was investigated by well diffusion method, drop collapse test, emulsification test, oil displacement activity, and blue agar plate method. The isolate obtained from the oil contaminated soil was identified as Bacillus subtilis. The identification was done by microscopic examinations and further characterization was done by Biochemical tests and 16SrRNA gene sequencing. Purification of the biosurfactant was performed by simple liquid-liquid extraction, and characterization of extracted biosurfactants was done using Fourier transform infrared spectroscopy (FTIR). The degradation of crude oil upon treatment with the partially purified biosurfactant was analyzed by FTIR spectroscopy and Gas-chromatography mass spectroscopy (GC-MS).