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Analysis of pesticide residues in irrigated rice grains is important for food security. In this study, we analyzed accelerated solvent extraction (ASE) conditions for the extraction of thiamethoxam and chlorantraniliprole insecticides from rice hulls, rice bran, and polished rice grains. Several variables, including extraction solvent, extraction temperature, extraction pressure, cell size, static extraction time, and sample concentration, were investigated. The average recoveries of the three matrixes were between 89.7 and 109.7% at the fortification level of 0.75 mg/kg. The optimum ASE operating conditions were acetonitrile (100%) as extraction solvent, extraction temperature of 75°C for rice hulls and 100°C for rice bran and polished rice grains, extraction cell pressure of 10.3 MPa, 22 mL cell size, and two extraction cycles. The total extraction time was approximately 25 min. The extracted volume was evaporated to dryness and the residues were redissolved in 2 mL acetonitrile after 1 min of vortex-shaking. Thiamethoxam and chlorantraniliprole were analyzed by ultra-HPLC with tandem MS. In conclusion, ASE in rice hulls, rice bran, and polished rice grains offers the possibility of a fast and simple method for obtaining a quantitative extraction of the studied pesticides.

Thiamethoxam and chlorantraniliprole insecticides have been important tools for controlling pests in rice. However, food safety issues related to pesticide residues are important to consider with a food crop such as rice. Therefore, the objective of this study was to analyze thiamethoxam and chlorantraniliprole residues in rice hull, bran, and polished rice grains. The study was conducted during the 2012 cropping season at the Texas A&M Agrilife Research, David R. Wintermann Rice Research Station, near Eagle Lake, TX, USA. Rice was planted on May 5, 2012, using the cultivar 'Presidio'. Pesticide applications were performed at 5, 15, 25, and 35 days after flowering (DAF) using 1 and 2 times the recommended rate of 30 g active ingredient (ai) ha(-1) for thiamethoxam and 30 g ai ha(-1) for chlorantraniliprole. Sequentially, two treatments using the insecticides at recommended rate were applied at 5 and 25 DAF and at 5, 25, and 35 DAF. Insecticide residues were analyzed in different sample fractions: rice hull, bran, and polished rice grains. The samples were subjected to extraction using an accelerated solvent extraction (ASE) technique. Sample aliquots were analyzed using ultrahigh-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS), with a limit of quantification (LOQ) of 5 × 10(-5) mg kg(-1). Residues of thiamethoxam and chlorantraniliprole were detected in rice hull, bran, and polished rice grains, and the quantified values were greater in hull and in rice bran.