Cloud point extraction with Triton X-114 for separation of metsulfuron-methyl, chlorsulfuron, and bensulfuron-methyl from water, soil, and rice and analysis by high-performance liquid chromatography.

A new and efficient analytic methodology based on cloud point extraction (CPE) was developed for determination of pesticide residues of metsulfuron-methyl (MSM), chlorsulfuron (CS), and bensulfuron-methyl (BSM) in water, soil, and rice grain by high-performance liquid chromatography (HPLC). Multiple experimental conditions that affected CPE efficiency-including surfactant type and concentration, equilibration temperature and duration, ionic strength, and solution pH were identified. CPE conditions were optimized as follows: 1.5% Triton X-114 (w/v), 12% Na(2)SO(4) (w/v) solution (pH 2.0), and heat-assisted at 50 °C for 15 min. The calibration curves for all analytes were linear, ranging from 0.05 to 4.0 mg L(-1), with the correlation coefficients >0.9995 by HPLC-ultraviolet detector and were linear, ranging from 0.004 to 2.0 mg L(-1), with correlation coefficients >0.9983 by CPE-HPLC. The average recoveries at the three spiked levels using CPE ranged from 86.0% to 94.5% for water samples with relative SDs (RSDs) of 0.4% to approximately 7.8%; from 85.6% to 94.8% for soil samples with RSDs of 1.2% to approximately 9.5%; and from 81.9% to 91.3% for rice samples with RSDs of 1.7% to approximately 5.8%. The proposed CPE-HPLC method can be successfully used to analyze MSM, CS, and BSM residues from contaminated water, soil, and rice grain samples.
(© Springer Science+Business Media, LLC 2010)