International Journal of Farming and Allied Sciences
Available online at www.ijfas.com
©2014 IJFAS Journal-2014-3-11/1201-1205/ 30 November, 2014
ISSN 2322-4134 ©2014 IJFAS
High Performance Liquid Chromatographic
Determination of an Asymmetrical Triazine
Herbicide from Soil
Mohammad Mehdizadeh*
PhD student in Weed Science, Department of Agronomy and Plant Breeding, Mohaghegh Ardabili University of
Ardabil, Iran
Corresponding author: Mohammad Mehdizadeh
ABSTRACT: A rapid method for determining residues of the herbicide metribuzin in soil by laboratory
experiment under controlled conditions is described. Field soil fortified with herbicide at concentration of 5
mg kg
-1
soil, and maintained at field capacity moisture regime and kept at ambient temperature 25 ± 5°C.
The soil samples were extracted with different ratio of methanol/water solution and the residue was
estimated by HPLC with UV detection at 290 nm and a flow rate of 0.5 ml/ min. The detection limits were
0.05 mg/kg in soil. The results indicate 52.55% degradation of metribuzin in soil samples on 120-days of
experiment. The methanol/water (4:1 v/v) was found to be most effective in metribuzin degradation
recovery and enhances the recovery as compared to the other. The proposed method has been
satisfactorily applied in soil samples showing recoveries ranging from 85% to 98% and represents a
valuable procedure for analysis of metribuzin by high performance liquid chromatography (HPLC).
Keywords: Degradation, Extraction, Metribuzin, Recovery, Retention Time, UV Detector
INTRODUCTION
Metribuzin [4-amino-6-(1-1-dimethylethyl)-3-(methylthio)-1,2,4-triazin-5(4H)-one] is a selective systemic
herbicide used for pre and post-emergence control of many grasses and broad-leaved weeds in soya beans,
potatoes, tomatoes, sugar cane, and cereals at 0.07–1.05 kg a.i./ha (Tomlin, 2002). It is considered a mobile
pesticide with estimated sorption coefficients in soil (Kd) generally well below 1.0 (Shaato, 2002). Metribuzin belongs
to the group of triazinone herbicides, that highly water soluble (1.05 g.L
−1
) and adsorption in low-organic sandy soils
is rather weak, sorption coefficients vary from 0.56 in a very sandy loam to 31.7 in a soil containing 60% organic
matter (Henriksen, 2002). Metribuzin is moderately water soluble and interacts with some polar as well as nonpolar
soil constituents. The solubility of metribuzin in methanol is several hundred times greater than in water (WSSA,
1983). In aqueous solution, metribuzin ionizes at very low pH (3 or less, pK/a) (Weber, 1980), resulting from
protonation of the amine group. Hydrophilic binding at pH levels < 7 occurs due to hydrogen bonding rather than
from ionization of the metribuzin molecule. Therefore, inclusion of water with a moderately nonpolar organic solvent
improves the extraction efficiency of metribuzin from hydrophilic sites. This herbicide is considered to be of short to
moderate persistence in soils. Metribuzin have received a great deal of attention because of its extensive use and
potential for widespread contamination of ecosystems. For detecting low level of metribuzin which may persist in soil
and groundwater, sensitive and accurate methods of analysis are desired. The primary criteria for choosing extraction
solvent is based on several factors related to extraction efficiency and residue recovery. Various studies on
metribuzin have been investigated by using the electro analytical method (Skopalova, 2001), chromatographic
methods such as liquid chromatography (Erenchun, 1977; Lawrence, 1996; Papadakis and Mourkidos, 2002; Shah,
2011), gas chromatography (Beltran, 1997), micellar electro kinetic chromatography (Huertas-Peres, 2006; Martinez,