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JOURNAL ARTICLE
VALIDATION STUDIES
Development and Validation of an HPLC Method for Determination of Thiamethoxam and Its Metabolites in Cotton Leaves and Soil.
Journal of AOAC International 2017 May 2
An easy and simple analytical method was standardized and validated for the estimation of residues of thiamethoxam and its metabolites in cotton. The samples were extracted with acetonitrile, water, and methanol; diluted with brine solution; partitioned into dichloromethane and ethyl acetate; dried over anhydrous sodium sulfate; and cleaned up by glass column chromatography. Final clear extracts were concentrated under vacuum and reconstituted into HPLC grade acetonitrile, and residues were estimated using an HPLC instrument equipped with a C18 column and photodiode array detector system. Acetonitrile-1% formic acid in HPLC grade water (30 + 70) was used as mobile phase at 0.2 mL/min. Consistent recoveries ranging from 82 to 97% for thiamethoxam and its metabolites were observed when samples were spiked at 0.05-1.0 mg/kg levels. The LOQ of the method was determined to be 0.05 mg/kg. The analytical method was validated in terms of the selectivity, linearity, precision, and accuracy of the detection system.
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