Determination of Imazaquin Residues in Soil by Solid-Phase Extraction and High-Performance Liquid Chromatography

An effective method based on a modified quick, easy, cheap, effective, rugged, and safe sample preparation step and determination by LC with MS/MS has been developed and validated for the simultaneous determination of pesticides with different characteristics in soil samples. Several parameters that affect the extraction and analysis were studied and the proposed method was validated using spiked blank soil samples. Recoveries for the herbicides clomazone, imazapic and imazethapyr, the insecticides fipronil and thiamethoxam, and the fungicides propiconazole and trifloxystrobin from blank samples spiked at levels between 2 and 100 µg kg−1 were in the acceptable range of 72.5–119.3% with relative standard deviation below 18.2%. Method limit of detection ranged between 0.12 and 0.6 µg kg−1. The method was successfully applied to the analysis of soil samples from rice paddies were thiamethoxam (103.4–770.8 µg kg−1), imazethapyr (2.4–293.5 µg kg−1), and fipronil (2.1–170.0 µg kg−1) were found in all samples. Imazapic, clomazone, trifloxystrobin presented low concentrations and propiconazole was not detected. The main advantages of the method lie in the fact that is simple and quick to perform, demand small amount of solvent and permit the analysis of multiclass pesticides at trace levels in soil samples with good trueness and precision.

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Simultaneous LC–MS/MS Determination of Imidazolinone Herbicides Together with Other Multiclass Pesticide Residues in Soil

Martins

Friggi

Prestes

et al. 2014

CLEAN Soil Air Water

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Analysis of Imazaquin in Soybeans by Solid-phase Extraction and High-performance Liquid Chromatography

Guo

Chen

et al. 2008

Bull Environ Contam Toxicol

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An analytical method for the determination imazaquin residues in soybeans was developed. The developed liquid/liquid partition and strong anion exchange solid-phase extraction procedures provide the effective cleanup, removing the greatest number of sample matrix interferences. By optimizing mobile-phase pH water/acetonitrile conditions with phosphoric acid, using a C-18 reverse-phase chromatographic column and employing ultraviolet detection, excellent peak resolution was achieved. The combined cleanup and chromatographic method steps reported herein were sensitive and reliable for determining the imazaquin residues in soybean samples. This method is characterized by recovery [88.4%, precision \6.7% CV, and sensitivity of 0.005 ppm, in agreement with directives for method validation in residue analysis. Imazaquin residues in soybeans were further confirmed by high performance liquid chromatographymass spectrometry (LC-MS). The proposed method was successfully applied to the analysis of imazaquin residues in soybean samples grown in an experimental field after treatments of imazaquin formulation.

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Determination of Imazaquin and its Metabolite by Liquid Chromatography-Quadrupole-Time of Flight Tandem Mass

Yao

Han

Liu

et al. 2010

Bull Environ Contam Toxicol

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A method consisting of solvent extraction followed by liquid chromatography-quadrupole-time of flight- tandem mass spectrometry analysis was developed for the identification of Imazaquin and its metabolite. The relationships between detector response and sample concentrations showed a high degree of linearity (r > 0.998) over the range 0.03-10 microg/g. The recoveries obtained were in the acceptable range of 86%-104% between spiked. The relative standard deviation of this method was 6.4%-17.1%. A 35-day study of Imazaquin degradation was taken in agricultural soil from Binzhou, China. The degradation followed first order kinetics (C = 0.7672e(-0.0774t)), with half-life of less than 8.5 days. Investigation of the by-products from liquid chromatography-quadrupole-time of flight- tandem mass spectrometry has shown that there were four important metabolites 4-methylene-2-(quinolin-2-yl)-1H-imidazol-5(4H)-one, quinoline-3-carbaldehyde, 1-amino-2,3-dimethyl-1-oxobutan-2-ylium and 1H-[1,2]oxazino[4,5-b]quinolin-1-one in the degradation process. The accurate mass measurements error was 5 ppm in this study. The method was successfully applied to the analysis of imazaquin and its metabolite residues in soil.

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Determination of Imazaquin Residues in Soil by Solid-Phase Extraction and High-Performance Liquid Chromatography

Cited by 5 publications

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Simultaneous LC–MS/MS Determination of Imidazolinone Herbicides Together with Other Multiclass Pesticide Residues in Soil

Simultaneous LC–MS/MS Determination of Imidazolinone Herbicides Together with Other Multiclass Pesticide Residues in Soil

Analysis of Imazaquin in Soybeans by Solid-phase Extraction and High-performance Liquid Chromatography

Determination of Imazaquin and its Metabolite by Liquid Chromatography-Quadrupole-Time of Flight Tandem Mass

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