An effective method for the trace analysis of indoxacarb residue in foodstuffs of plant and animal origin [grapefruit, ginger, fresh soybean, bamboo shoot, qing-gen-cai （cruciferous vegetable）, chicken, fish, and po...An effective method for the trace analysis of indoxacarb residue in foodstuffs of plant and animal origin [grapefruit, ginger, fresh soybean, bamboo shoot, qing-gen-cai （cruciferous vegetable）, chicken, fish, and pork] was developed using gas chromatography （GC-ECD） and liquid chromatography tandem mass spectrometry （LC-MS/MS）. Samples were extracted using acetone and n-hexane mixed solvent （1：2, v/v） and then purified using solid-phase extraction （SPE） columns. The extracts were analyzed using GC-ECD and LC-MS/MS. The multiple reaction monitoring （MRM） scheme used involved transitions of the precursor ions to selected two product ions in which one pair for identification was m/z 529 → 293 and another pair for quantification was m/z 529 → 249. The detection limits （LODs） of the method were 0.0015 and 0.0006 mg kg^-1, and the quantification limits （LOQs） were 0.005 and 0.002 mg kg^-1 for GC-ECD and LC-MS/MS, respectively. The relative standard deviations （RSDs） of recovery for indoxacarb were lower than 15% in 10 types of agro-products. Ten repetitive determinations of recovery achieved good reproducibility for indoxacarb and the recovery ranged from 72.08 to 113.74%. The proposed procedure was applied to the analysis of several real samples of different origin from Fujian Province, China, and 299 samples were screened for indoxacarb residue, of which 5 positive samples were found.展开更多
基金grants from Fujian Pro- vincial Department of Science and Technology (2006F3002)Xiamen Science and Technology Bureau (3502Z20072003)China Postdoctoral Programme (20060390291)
文摘An effective method for the trace analysis of indoxacarb residue in foodstuffs of plant and animal origin [grapefruit, ginger, fresh soybean, bamboo shoot, qing-gen-cai （cruciferous vegetable）, chicken, fish, and pork] was developed using gas chromatography （GC-ECD） and liquid chromatography tandem mass spectrometry （LC-MS/MS）. Samples were extracted using acetone and n-hexane mixed solvent （1：2, v/v） and then purified using solid-phase extraction （SPE） columns. The extracts were analyzed using GC-ECD and LC-MS/MS. The multiple reaction monitoring （MRM） scheme used involved transitions of the precursor ions to selected two product ions in which one pair for identification was m/z 529 → 293 and another pair for quantification was m/z 529 → 249. The detection limits （LODs） of the method were 0.0015 and 0.0006 mg kg^-1, and the quantification limits （LOQs） were 0.005 and 0.002 mg kg^-1 for GC-ECD and LC-MS/MS, respectively. The relative standard deviations （RSDs） of recovery for indoxacarb were lower than 15% in 10 types of agro-products. Ten repetitive determinations of recovery achieved good reproducibility for indoxacarb and the recovery ranged from 72.08 to 113.74%. The proposed procedure was applied to the analysis of several real samples of different origin from Fujian Province, China, and 299 samples were screened for indoxacarb residue, of which 5 positive samples were found.
