溴氰菊酯在中药材头花蓼及土壤中的残留消解动态研究

【作者】 王永康；

【导师】 胡德禹； 黄荣茂；

【作者基本信息】 贵州大学 ， 有机化学， 2008， 硕士

【摘要】 溴氰菊酯具有高效、广谱、毒性低等特点,是防治中药材虫害的常用药剂。本文对溴氰菊酯在土壤及中药材中的残留分析方法和残留动态进行了研究,为溴氰菊酯在中药材种植过程中的安全使用提供科学依据。以头花蓼为研究对象,建立了溴氰菊酯残留的分析方法,采用超声波提取、弗罗里硅土柱净化等手段对样品进行处理,利用气相色谱电子捕获检测器对样品中溴氰菊酯残留的含量进行测定;对方法的灵敏度、准确度、精密度进行了分析。比较不同的提取方法、不同淋洗液和层析材料对农药残留检测结果的影响,结果表明,用超声波萃取方式提取中药材中的农药残留可以达到好的提取效果;不同的淋洗液对实验结果影响也很大,采用石油醚/乙酸乙酯（9:1,V/V）做为淋洗液,以弗罗里硅土进行净化,实验效果最好。溴氰菊酯在土壤及植株中的3个浓度添加回收率为80.6～99.3%,相对标准偏差为3.4～13.1%,最低检出浓度为0.01mg/kg,最小检出量为4.7×10^-3ng。以上数据说明方法准确度、精密度和灵敏度均达到了农药残留检测的要求。对头花蓼植株及土壤中溴氰菊酯的残留量分别进行检测,结果表明:溴氰菊酯在头花蓼植株及土壤中的半衰期分别为2.1～2.6d,3.3～3.4d;头花蓼及土壤中的溴氰菊酯最终残留量低于0.01mg/kg。更多还原

【Abstract】 Due to its characters of high effectiveness, low toxicity and broad spectrum, deltamethrin has been widely used in pest insect prevention for Chinese herbal medicine. In this paper, the residue determination and degradation of deltamethrin in soil and Chinese herbal medicine were studied, in order to establish the MRL standard for safe deltamethrin using in Chinese herbal medicine planting. In this article, Polygonum Capitatum Buch was chosen to be our study object. The sample was extracted by ultrasonic wave assisted method and was purified by Florisil. Residue of deltamethrin in Polygonum Capitatum Buch and soil was analyzed and studied by GC-ECD with pre-column. Comparison was made within several different ways of sample extraction、different eluents and different sorbents to find out their influence on the test result respectively. The result is that: ultrasonic wave assisted method is better for the sample extraction and the mixture of petroleum ether-ethylacetate （9:1） and purified by the Florisil is the most satisfactory match of eluent and sorbent. The average recoveries of the three spiked levels of deltamethrin was 80.6-99.3% in Polygonum Capitatum Buch; the Coefficient of Variation （CV） was 3.4-13.1%, the limit of quantification （LOQ） was 0.01 mg/kg; and the limit of detection （LOD） was 4.7×10^-3 ng. This result can obviously prove that the accuracy, exactitude and sensitivity of this method meet the requirements of pesticide residue analysis.The results of detection showed that the degradation half-lives of deltamethrin were 2.1-2.6 d in Polygonum Capitatum Buch and 3.3-3.4 d in soil respectively. The final residues of deltamethrin in Polygonum Capitatum Buch and soil were less than 0.01 mg/kg.更多还原