Validation and quantification of neonicotinoid insecticide residues in rice whole grain and rice straw using LC-MS/MS

Abstract

ABSTRACTAn efficient analytical method was developed and validated using a modified QuEChERS method and LC-MS/MS for the detection and quantification of neonicotinoid insecticide residues in rice whole grain and rice straw. The samples were extracted using acetonitrile and cleaned up by dispersive solid-phase extraction. Validation based on five fortification levels showed good recoveries of neonicotinoids ranging from 75% to 116 % and 60% to 105 % for rice whole grain and straw, respectively. The precision ranged between 3% and 17 %, and 2% and 10 % for grain and straw, respectively. The limit of detection was from 0.007 to 0.0084 mg kg−1 and 0.005 to 0.15 mg kg−1 and the limit of quantification was in the range of 0.024–0.028 mg kg−1 and 0.016–0.051 mg kg−1 for rice whole grain and rice straw, respectively. Monitoring of farm gate samples indicated that, out of 24 samples, 1 rice whole grain sample was contaminated with thiamethoxam residues (0.07 mg kg−1).