Determination of 3-nitrobenzanthrone in surface soil by normal-phase high-performance liquid chromatography with fluorescence detection.
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.
Kyoto Pharmaceutical University, 5 Nakauchi-cho Misasagi Yamashina-ku, 607-8414 Kyoto, Japan. tmu@mb.kyoto-phu.ac.jp
Tsuyoshi
T
Murahashi
Tetsushi
T
Watanabe
Shuhei
S
Otake
Yoshimasa
Y
Hattori
Takeji
T
Takamura
Keiji
K
Wakabayashi
Teruhisa
T
Hirayama
D001551:Benz(a)Anthracenes / Q000032:analysis*; D002138:Calibration; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D012680:Sensitivity and Specificity; D012989:Soil Pollutants / Q000032:analysis*; D013050:Spectrometry, Fluorescence / Q000379:methods*
D001551:Benz(a)Anthracenes; D012989:Soil Pollutants; C117220:3-nitrobenzanthrone