• Title/Summary/Keyword: LC-SPE-NMR

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Liquid Chromatography-Solid Phase Extraction-NMR (LC-SPE-NMR) Analysis of Liquid Crystalline Mixtures

  • Park, Gregory Hyung-Jin;Park, Ae-Na;Rho, Kyung-Rae;Shin, Jong-Ho;Kim, Yeong-Jeon;Jo, Sung-Chan;Oh, Weon-Sik
    • Journal of the Korean Magnetic Resonance Society
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    • v.15 no.1
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    • pp.14-24
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    • 2011
  • We have performed Liquid Chromatography-Solid Phase Extraction-NMR (LC-SPE-NMR) analysis for liquid crystalline mixture and elucidated the structures of selected components by NMR spectra. Combining the results of one-dimensional 1H experiments as well as homonuclear and heteronuclear two-dimensional experiments, we could analyze the molecular structure of the liquid crystal singles whose structure had not been interpretable by mass spectrometry alone.

Identification of Xanthium Sibiricum Components using LC-SPE-NMR-MS Hyphenated System

  • Sohn, Ji Soo;Jung, Youngae;Han, Ji Soo;Hwang, Geum-Sook
    • Journal of the Korean Magnetic Resonance Society
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    • v.22 no.2
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    • pp.26-33
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    • 2018
  • Xanthium sibiricum is used as a traditional folk medicine for the treatment of cancer, fever, headache, nasal sinusitis, and skin pruritus. This study aimed to identify components from Xanthium sibiricum extracts using an SPE-800MHz NMR-MS hyphenated system. The simultaneous acquisition of MS and NMR spectra from the same chromatographic peaks significantly increases the depth of information acquired for the compound and allows the elucidation of structures that would not be possible using MS or NMR data alone. LC -NMR analysis was conducted using a HPLC separation system coupled to 800 MHz spectrometer equipped with a cryoprobe, and a SPE unit was used to automatically trap chromatographic peaks using a HPLC pump. LC-MS analysis was conducted with a Q-TOF MS instrument using ESI ionization in the negative ion mode. Using the hyphenated analysis, several secondary metabolites were identified, such as 3',5'-O-dicaffeoylquinic acid, 1',5'-O-dicaffeoyl- quinic acid, and ethyl caffeate. These results demonstrate that the SPE-800MHz NMR-MS hyphenated system can be used to identify metabolites within natural products that have complex mixtures.