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

An 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 and 0.005 to 0.15 mg kg and the limit of quantification was in the range of 0.024-0.028 mg kg and 0.016-0.051 mg kg 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).