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| Development of a multiresidue method for determination of 110 pesticide residues in soil using QuEChERS-HPLC-MS/MS and QuEChERS-GC-MS |
| Received:December 26, 2016 |
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| KeyWord:QuEChERS;high performance liquid chromatography tandem mass spectrometry;gas chromatography tandem mass spectrometry;pesticide residues;soil |
| Author Name | Affiliation | E-mail | | CAI Lin | Key Laboratory of Industrial Ecology and Environmental Engineering(Ministry of Education), School of Environmental Science and Technology, Dalian University of Technology, Dalian 116024, China | | | XI Pu-yu | Key Laboratory of Industrial Ecology and Environmental Engineering(Ministry of Education), School of Environmental Science and Technology, Dalian University of Technology, Dalian 116024, China | | | XIE Qing | Key Laboratory of Industrial Ecology and Environmental Engineering(Ministry of Education), School of Environmental Science and Technology, Dalian University of Technology, Dalian 116024, China | | | LI Xue-hua | Key Laboratory of Industrial Ecology and Environmental Engineering(Ministry of Education), School of Environmental Science and Technology, Dalian University of Technology, Dalian 116024, China | | | QIAO Xian-liang | Key Laboratory of Industrial Ecology and Environmental Engineering(Ministry of Education), School of Environmental Science and Technology, Dalian University of Technology, Dalian 116024, China | | | XIE Hong-bin | Key Laboratory of Industrial Ecology and Environmental Engineering(Ministry of Education), School of Environmental Science and Technology, Dalian University of Technology, Dalian 116024, China | | | CHEN Jing-wen | Key Laboratory of Industrial Ecology and Environmental Engineering(Ministry of Education), School of Environmental Science and Technology, Dalian University of Technology, Dalian 116024, China | | | CAI Xi-yun | Key Laboratory of Industrial Ecology and Environmental Engineering(Ministry of Education), School of Environmental Science and Technology, Dalian University of Technology, Dalian 116024, China | xiyuncai@dlut.edu.cn |
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| Abstract: |
| A method was established for the determination of 110 pesticides in soil using high performance liquid chromatography tandem mass spectrometry(HPLC-MS/MS) and gas chromatography tandem mass spectrometry(GC-MS) with modified QuEChERS(Quick, Easy, Cheap, Effective, Rugged, and Safe). Levels of acetic acid used in the QuEChERS procedure were optimized, and results indicated that higher recoveries were obtained when 1% acetic acid was added. Based on differences in polarity, thermostability, volatility, and other characteristics of pesticides, analysis of 43 pesticides was conducted via HPLC-MS/MS and the other 67 pesticides were analyzed using GC-MS. Five internal standards(atrazine-d5, sulfosulfuron, 1,3-dimethyl-2-nitrobenzene, triphenyl phosphate, and perylene-d12) were used for the method validation. The average recoveries of the 43 pesticides analyzed via HPLC-MS/MS at three spike levels(10, 20, and 50 μg·kg-1) ranged from 59.1% to 129.4% with relative standard deviations(RSDs) between 0.3% and 15%; whereas the average recoveries of the 67 compounds analyzed using GC-MS ranged from 44.9% to 168.1% with RSDs of 0.5%~20%. The detection limits of the method ranged from 0.01 to 5.00 μg·kg-1. The established method was used to determine pesticide resides in a soil sample, in which 68 pesticides were found, including nicosulfuron, propyzamide, oxyfluorfen, folpet, dimethomorph, lambda-cyhalothrin, some organophosphorus pesticides, and some organochlorine pesticides. Overall, the method is simple, efficient, and sensitive, and thus can be used for the simultaneous determination of pesticide residues in soil. |
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