【作者】 赵春杰；

【导师】 罗旭； 陈英杰；

【作者基本信息】 沈阳药科大学 ， 药物分析学， 2006， 博士

【摘要】 人们长期、广泛、大量地使用农药，以消灭病虫害，促进农作物生长。但早期对农药只重视其急性毒性，而忽视了其慢性毒性，致使一些性质稳定、具慢性毒性的有机氯农药如滴滴涕、六六六和含汞、铅等重金属的农药不仅污染了环境，而且在人和动物体内蓄积，遂成为今日的农药公害。 作为农作物，中药材中残留农药和重金属超标所造成的中毒和国际贸易退货事件时有发生，已严重危害了中药材声誉，妨碍了其贸易。对中药材中残留农药和重金属含量控制的问题，是急待解决的。 从根本上讲，解决上述问题，应采用防治病虫害的生物和物理技术，栽培出无污染的绿色中药材。目前，国内外已开展了这样的研究工作，但这不是一蹴而就的。本研究从实际情况出发，把CO₂超临界萃取技术应用于中药材党参、当归、淫羊藿、黄芪和熟地中残留农药和重金属的脱除，采用3个水平、4因素（压力、温度、时间、流速）的L₉（3⁴）正交阵列确定优化条件。在选定的最优条件下，农药和重金属的净化率在85％以上，指定有效成分的损失率在5％以下，从而使各该中药材质量达到安全、有效的标准。在应用于重金属的脱除时，4因素中的流速为会属配位剂二乙基二硫代氨基甲酸酯的浓度所代替。 除上述两项工作外，必须建立农药、重金属和中药材指定有效成分的测定方法，才能评价净化前后中药材残留农药、重金属和指定有效成分含量的变化。需要进行以下3项工作： 1、建立中药材中12种有机氯类农药残留量的测定方法。采用有关机构（FDA）的方法提取，以磺化后不分流进样方式，采用弹性石英毛细管柱程序升温技术分离，电子捕获检测器检测，按外标法计算含量。进行了党参、当归、淫羊藿、黄芪和熟地中12种有机氯农药的含量测定。 2、建立了7种重金属的原子吸收光谱（AAS）测定法，用空气-乙炔火焰法测定铅、镉、铜、铁、锌，用氢化物发生法测定砷、汞。 3、以C₁₈反相色谱柱测定中药材中指定有效成分的含量测定方法，采用的流动相和检测波长各不相同。更多还原

【Abstract】 Virtually all of the Chinese Herbal Medicine （CHM） nowadays have been cultivated with the application of pesticides to reduce pest damage and promote the production.The application of pesticides not only pollutes the cultivating soil and ground water, i.e. the environment, but leads to the accumulation of them in plants, animals and human beings eating them. The risk of the consumers’ health due to incidental intake of the remaining contaminants in CHM thus cultivated is highly possible. The organochlorine pesticides （OCPs） and heavy metals are the first ones to be considered, because they possess the characteristics of harmful biological effects and high accumulation.The cultivation of Green CHM has been promoted to reduce the pollution of OCPs and heavy metals. However, as many kinds of pesticides and fertilizers, which usually contain heavy metals, have been used for a long time, to say nothing of the soil and ground water, the proposal can hardly be put into practice. The need for an efficient method of reducing OCPs and heavy-metals in the cultivated CHMs is obvious. In the study, a method of CO₂ supercritical fluid extraction（SFE） has been developed for the removal of pesticide and heavy metal residues from CHMs, such as Radix Codoposis, Angelicae Sinenisis, Herba Epimedii, Radix Astragali and Radix Rehmanniae Preparata.1. An efficient and rapid method of CO₂ supercritical fluid extraction has been designed successfully for the removal of 12 remaining OCPs from the five CHMs mentioned above. In the study, L₉（3⁴）, an orthogonal array of 3 levels, 4 factors and 9 trials, was used to optimize the conditions with the result of more than 85% removal of the pesticide and less更多还原