高效液相色谱法同时测定生活饮用水中七种有机磷农药残留研究
发布时间:2019-04-01 12:04
【摘要】:大多数的农药残留(简称农残)物质都属于有毒有害物质,它们以各种危害形式持续存在于水体、土壤、大气等各种日常生活环境当中,能够通过不同的途径进入人体,对人的身体健康产生极大的危害。有机磷农药(OrganophosphorousPesticides,OPPs)是用于防治植物病、虫、害的含有机磷的有机化合物。这一类农药品种多,药效高,用途广,易分解,在人、畜体内一般不积累,在农药中是极为重要的一类化合物。但有不少品种对人、畜的急性毒性很强。水体中OPPs的存在主要是来自于农业及工业废水的排放。有大量报告研究表明,微量的有机磷农残对水的生态系统已经产生一定的危害,因此水域生态环境系统中有机磷农残污染问题也随之成为水环境研究的热点问题。因此,研究出能快速、灵敏、准确的检测环境中有机磷农残的方法,对于评价其生态风险等问题具有十分重要的意义。然而,对于环境中的微量有机磷农残的检测技术方法仍然存在准确性和灵敏度较差等诸多的难题,而且通常情况下水体中OPPs的量很低(μg/L级),一般方法难于对其进行直接测定。 本文对兰州市安宁区不同地点的生活饮用水中有机磷农药残留检测研究为基础,分别对有机磷农药的性质、结构特征及高效液相色谱法的的原理、特点进行研究;建立一种以高效液相色谱法为基础的同时检测多种有机磷农药残留的方法;确定了采用高效液相色谱法(HPLC)时的最佳条件。结果表明,以甲醇:水(68.5:31.5,V/V)作为流动相、流动相pH为6、流速为1.0mL/min、进样量为20μL的条件下,,HPLC完全可以分离七种有机磷农药(乐果、敌敌畏、毒死蜱、内吸磷、甲基对硫磷、马拉硫磷、对硫磷)。该方法的最低检出限在1.1μg/L~1.7μg/L之间;回收率在83%~96%,相对标准偏差3.6%~6.5%之间,精密度高。通过试验证明该方法分离效果好,选择性高,检测灵敏度高。
[Abstract]:Most pesticide residues (referred to as agricultural residues) are toxic and harmful substances, which persist in water, soil, atmosphere and other daily living environments in various hazardous forms, and can enter the human body through different ways. It does great harm to people's health. Organophosphorus pesticides (OrganophosphorousPesticides,OPPs) are organic compounds that contain organic phosphorus, which are used to control plant diseases, insects and pests. This kind of pesticide has many varieties, high efficacy, wide use, easy to decompose, does not accumulate in human and animal body, and is a very important kind of compound in pesticide. But there are many species to human, animal acute toxicity is very strong. The existence of OPPs in water is mainly from the discharge of agricultural and industrial wastewater. A large number of reports have shown that a small amount of organophosphorus agricultural residues has caused certain harm to the water ecosystem, so the pollution of organophosphorus agricultural residues in the aquatic ecosystem has become a hot issue in the water environment research. Therefore, it is of great significance to study a rapid, sensitive and accurate method for the detection of organophosphorus agricultural residues in the environment. However, there are still many difficulties in the detection of trace organophosphorus agricultural residues in the environment, such as poor accuracy and sensitivity, and the amount of OPPs in water is usually very low (渭 g / L). It is difficult to determine it directly by general method. Based on the study on determination of organophosphorus pesticide residues in drinking water at different locations in Anning District of Lanzhou City, the properties, structural characteristics, principle and characteristics of high performance liquid chromatography (HPLC) of organophosphorus pesticides were studied. To establish a method for simultaneous determination of organophosphorus pesticide residues based on high performance liquid chromatography (HPLC). The optimum conditions were determined when (HPLC) was used by high performance liquid chromatography (HPLC). The results showed that seven organophosphorus pesticides (dimethoate, dichlorvos, dimeth Chlorpyrifos, internal absorption phosphorus, methyl parathion, malathion, parathion). The detection limit of this method is between 1.1 渭 g / L and 1.7 渭 g / L, the recovery is 83% ~ 96%, the relative standard deviation is 3.6% ~ 6.5%, and the precision is high. The experimental results show that the method has good separation effect, high selectivity and high detection sensitivity.
【学位授予单位】:西北师范大学
【学位级别】:硕士
【学位授予年份】:2013
【分类号】:O657.72;R123.1
[Abstract]:Most pesticide residues (referred to as agricultural residues) are toxic and harmful substances, which persist in water, soil, atmosphere and other daily living environments in various hazardous forms, and can enter the human body through different ways. It does great harm to people's health. Organophosphorus pesticides (OrganophosphorousPesticides,OPPs) are organic compounds that contain organic phosphorus, which are used to control plant diseases, insects and pests. This kind of pesticide has many varieties, high efficacy, wide use, easy to decompose, does not accumulate in human and animal body, and is a very important kind of compound in pesticide. But there are many species to human, animal acute toxicity is very strong. The existence of OPPs in water is mainly from the discharge of agricultural and industrial wastewater. A large number of reports have shown that a small amount of organophosphorus agricultural residues has caused certain harm to the water ecosystem, so the pollution of organophosphorus agricultural residues in the aquatic ecosystem has become a hot issue in the water environment research. Therefore, it is of great significance to study a rapid, sensitive and accurate method for the detection of organophosphorus agricultural residues in the environment. However, there are still many difficulties in the detection of trace organophosphorus agricultural residues in the environment, such as poor accuracy and sensitivity, and the amount of OPPs in water is usually very low (渭 g / L). It is difficult to determine it directly by general method. Based on the study on determination of organophosphorus pesticide residues in drinking water at different locations in Anning District of Lanzhou City, the properties, structural characteristics, principle and characteristics of high performance liquid chromatography (HPLC) of organophosphorus pesticides were studied. To establish a method for simultaneous determination of organophosphorus pesticide residues based on high performance liquid chromatography (HPLC). The optimum conditions were determined when (HPLC) was used by high performance liquid chromatography (HPLC). The results showed that seven organophosphorus pesticides (dimethoate, dichlorvos, dimeth Chlorpyrifos, internal absorption phosphorus, methyl parathion, malathion, parathion). The detection limit of this method is between 1.1 渭 g / L and 1.7 渭 g / L, the recovery is 83% ~ 96%, the relative standard deviation is 3.6% ~ 6.5%, and the precision is high. The experimental results show that the method has good separation effect, high selectivity and high detection sensitivity.
【学位授予单位】:西北师范大学
【学位级别】:硕士
【学位授予年份】:2013
【分类号】:O657.72;R123.1
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