Determination of 3-nitrobenzanthrone in surface soil by normal-phase high-performance liquid chromatography with fluorescence detection

J Chromatogr A. 2003 Apr 11;992(1-2):101-7. doi: 10.1016/s0021-9673(03)00279-6.

Abstract

A sensitive method for determining 3-nitrobenzanthrone in surface soil was developed. 3-Nitrobenzanthrone was reduced to 3-aminobenzanthrone by refluxing at 60 degrees C with hydrazine and Raney nickel for 20 min, and 3-aminobenzanthrone was determined by normal-phase high-performance liquid chromatography (HPLC) with fluorescence detection. We used a cyanopropyl stationary phase and an n-hexane-ethyl acetate (3:1, v/v) mobile phase, since 3-aminobenzanthrone exhibits fluorescence in a low-polarity solvent such as n-hexane or ethyl acetate, but not in a polar solvent such as water or methanol. The calibration graph showed good linearity (r2>0.9999) in the range of 0.002-2 ng, and the detection limit was 0.002 ng (S/N=3). 3-Nitrobenzanthrone in extracts from surface soil collected in the Chubu area (central area) of Japan was determined after clean-up using silica gel chromatography and high-performance liquid chromatography on a pyrenylethyl stationary phase. The concentration of 3-nitrobenzanthrone in surface soil was determined in the range of 1.2-1020 pg/g soil.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Benz(a)Anthracenes / analysis*
  • Calibration
  • Chromatography, High Pressure Liquid / methods*
  • Sensitivity and Specificity
  • Soil Pollutants / analysis*
  • Spectrometry, Fluorescence / methods*

Substances

  • Benz(a)Anthracenes
  • Soil Pollutants
  • 3-nitrobenzanthrone