Bulletin of the Korean Chemical Society

Korean Chemical Society (대한화학회)
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Development of an Isotope-Dilution Flow-Injection Electrospray/ Mass Spectrometric Method for the Accurate Determination of Glucosamine in Pharmaceutical Formulation

  • Kim, Gui-Nam (Department of Chemistry, Kyungnam University) ;
  • Kim, Byung-Joo (Division of Metrology for Quality Life, Korea Research Institute of Standards and Science) ;
  • Ahn, Seong-Hee (Division of Metrology for Quality Life, Korea Research Institute of Standards and Science) ;
  • Hwang, Eui-Jin (Division of Metrology for Quality Life, Korea Research Institute of Standards and Science) ;
  • Kim, Yong-Seong (Department of Chemistry, Kyungnam University)
  • Published : 2009.02.20
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Abstract

An isotope-dilution flow-injection electrospray/mass spectrometric method was developed for the accurate determination of glucosamine contents in pharmaceutical formulations. Samples were extracted by methanol. After spiking glucosamine-1-$^{13}C_1$ as an internal standard, the extracts were then analyzed by flow-injection ESI/MS in a selected ion monitoring (SIM) mode to detect [M+H]$^+$ ions of the analyte and its isotope analogue at m/z 180 and m/z 181, respectively. Confirmatory measurements were made by selectively monitoring the collisionally induced dissociation channels of m/z 180 $\rightarrow$ m/z 72 and m/z 181 $\rightarrow$73, respectively, to test the possibility of bias in the SIM method due to matrix interferences, but any significant bias in the SIM mode was not observed. Repeatability and reproducibility studies showed that the flow-injection ESI/MS method is a reliable and reproducible method which can provide a typical method precision of 1.0 %. Other results for the method validation are reported.

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