Chromatographia

, 70:1055 | Cite as

Determination and Identification of Primary Aliphatic Amines Using 4-(1H-Phenanthro[9,10-d]Imidazol-2-yl)Benzoic Acid as Novel Pre-Column Labeling Reagent by LC with Fluorescence Detection and Atmospheric Pressure Chemical Ionization Mass Spectroscopy

Original

Abstract

4-(1H-Phenanthro[9,10-d]imidazol-2-yl)benzoic acid (PIBA), a new amine-reactive fluorescent probe was synthesized and used as a pre-column derivatizing reagent for the determination of aliphatic amines from environmetal water samples. Derivatization was successfully carried out by a condensation reaction using 1-ethyl-3-(3-dimethylaminopropyl)-carbodiimide hydrochloride as the dehydrant. Studies on derivatization conditions indicated that the condensation reaction proceeded rapidly and smoothly in the presence of pyridine. Amines were labeled with PIBA to give the corresponding sensitively fluorescent derivatives with an excitation maximum at λ ex 260 nm and an emission maximum at λ em 445 nm. Identification of derivatives was carried out by online APCI–MS–MS and showed an intense protonated molecular ion corresponding m/z [M + H]+ in the positive ion mode. Excellent linear responses were observed with coefficients of >0.9996. Detection limits were 6.7–27 fmol (at a signal-to-noise ratio of 3). The mean intra- and inter-assay precision for all amine levels were <2.79 and 3.85%, respectively. The established method for the determination of aliphatic amines from real water was satisfactory.

Keywords

Column liquid chromatographia Mass spectrometry Pre-column derivatization Fluorescence detection Aliphatic amines 

Notes

Acknowledgment

This work was supported by the National Science Foundation under Grant # 20075016, and the Programs of “Hundreds Talent” of the Chinese Academy of Sciences (328).

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Copyright information

© Vieweg+Teubner | GWV Fachverlage GmbH 2009

Authors and Affiliations

  • Zhiwei Sun
    • 1
    • 3
  • Jinmao You
    • 1
    • 2
  • Lian Xia
    • 1
    • 3
  • Yourui Suo
    • 1
  1. 1.Northwest Plateau Institute of BiologyChinese Academy of SciencesXiningPeople’s Republic of China
  2. 2.College of Chemistry ScienceQufu Normal UniversityQufu ShandongPeople’s Republic of China
  3. 3.Graduate University of the Chinese Academy of ScienceBeijingPeople’s Republic of China

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