| Agriculture is the key industry of our country and even the world. In recent years,with the rapid development of new science and technology,the industrial structure of agriculture and cropping patterns change,climate anomalies,sharply increased resistance of crop diseases and insect pests and other reasons, harm is serious day by day,food security and ecological security issues outstanding, agriculture ecological situation is grim. To deal with the current pest took mainly chemical control measures, but in the long run,caused by the improper use of environmental pollution, ecological damage and harm of pesticide residues on issues such as human health,has already caused the extensive concern,become solve agricultural science and technology development needs the important technology and realistic subject. Therefore,to establish a method for determination of soil and water fast,efficient,low cost of pesticide has already become the priority among priorities.This study selected56kinds of pesticide organophosphorus,organochlorine,car bamate and its derivatives,by liquid liquid extraction (LLE) and oscillatory extraction methods such as extraction,solid phase extraction (SPE) was purified,using liquid chromatography tandem mass spectrometry (LC-MS-MS) and gas chromatography ta ndem mass spectrometry (GC-MS-MS) were detected,built the residue analysis of56pesticides in soil and water environment, and apply these methods to the investigation of non-point source pollution in parts of the territory of Shandong province. This pap-er is divided into4parts:1.This study reviewed the kinds and properties of pesticides,pesticide residues in soil water environment and the basic situation, multi residue detection technology,s-ummarized the detection technology commonly used pesticide residues in soil and water environment.2. Residue method for56kinds of pesticides in water environment analyses. Purification technology and liquid liquid extraction technology of comprehensive application of solid-phase extraction,using liquid chromatography tandem mass spe-ctrometry and gas chromatography tandem mass spectrometry method for the linear and the recovery of56kinds of pesticide rate was determined;extraction process of LC-MS-MS method and GC-MS-MS method of selection of flow gas phase mass spe-ctrometry instrument conditions part of the tandem chromat ography part and and pre-treatment method and the purification process was optimized. Based on water blank sample addition recovery experiments,different methods of most pesticides stable recovery ratio is between60%-120%, the relative standard deviation is less than20%. This method is simple,rapid pretreatment process,saving time and labor,the detection of short time needed,can give the experimental results very quickly,precision and accuracy are better,can meet the need of common daily detection of pesticides in the water environment..3. Residue method for56kinds of pesticides in soil analyses. Application of oscillation extraction and liquid chromatography tandem mass spectrometry and gas chromatography tandem mass spectrometry method combined with linear and recovery of the56kinds of pesticides in soil rate was determined,the pretreatment method of extraction solvent and extraction method were optimized. The soil blank sample addition recovery experiments, different methods of most pesticides stable recovery ratio is between60%-120%,the relative standard deviation is less than20%, with good accuracy and sensitivity. Qualitative detection limit of this method (LOD) between0.011-0.99g/L,quantitative detection limit (LOQ) between1-5g/L,is a multi residue detection method for pesticide in water environment and soil better,can be widely used for agricultural non-point source pollution investigation and injury accident treatment etc..4. This thesis takes Shandong Province as the pilot,at the same time acquisition and detection of typical agricultural region of surface water, soil and other environm-ental samples,to the current situation and the non-point source pollution in Shandong province has made the understanding of pesticide. |
