螺螨酯的残留分析方法及其在柑橘和土壤中的动态降解规律研究

螺螨酯的残留分析方法及其在柑橘和土壤中的动态降解规律研究(6500字)
摘　要：为了给螺螨酯在柑橘和土壤中的安全使用提供参考，对长沙、杭州、贵阳三地的柑橘施加螺螨酯，并对其动态降解规律进行分析。采用丙酮提取、Florisil固相萃取净化、建立了螺螨酯在柑橘和土壤中残留量的气相色谱法检测。结果表明,螺螨酯在0. 0001412-5.645 mg/L浓度范围内，色谱峰面积与农药浓度呈现良好的线性关系，相关系数为0. 9996，仪器最低检出量为1.41×10-13 g，螺螨酯在柑橘和土壤样品的检出限为0.0035 mg /kg。柑橘土壤与柑橘全果中螺螨酯的回收率分别为96.8%-109.2%和85.4%-97.9%，变异系数分别为1.08%-3.76%和3.48%-4.38% (n=5), 方法的准确度和精密度均达到农药残留分析检测的要求。螺螨酯在长沙、杭州、贵阳三地的柑橘土壤中的半衰期分别是6.56d、6.951d、7.191d，在柑橘全果中的半衰期是5.18d、7.64d、5.16d，螺螨酯在柑橘和土壤环境中易于降解。
关键词：螺螨酯；柑橘；土壤；气相色谱；消解

Study on the residues analytical method and the dynamic degradation rule of spirodiclofen in orange and soil
Abstract: In order to provide reference for safe use of spirodiclofen in the orange and soil, we analysis the dynamic degradation rule via orange imposed pesticides in Changsha, Hangzhou, Guiyang. This paper has adopted acetone extraction, Florisil solid phase purify and established the gas chromatography test method of spirodiclofen residues in the orange and soil. The results show that spirodiclofen in 0. 0001412 to 5.645 mg/L Chromatographic peak area and pesticide concentration presents good linear relationship, correlation coefficient is 0.9996, the instruments minimum detectable amount is 1.41×10-13g, and the detect limit for spirodiclofen in the orange and soil sample is 0.0035 mg/kg.The recovery rate is 96.8% to 109.2% for soil sample,85.4%-97.9% for orange sample respectively and the variation coefficient is 1.08% to 3.76% and 3.48% to 4.38% (n=5) respectively and the method achieves the accuracy and precision of pesticide residues analysis detection requirements. The Spirodiclofen half-life for soil in Changsha, Hangzhou, Guiyang is respectively 6.552 d,6.581d,10.151d ,for orange is 5.177d、10931d、5.389d and spirodiclofen in the orange and soil environment is easily degraded.
Key words: Spirodiclofen; citrus; soil; gas chromatography; residue detection
 

目    录
摘要    1
关键词    1
1 前言    2
2 材料与方法    3
2.1 供试材料    3
2.2 主要仪器及设备    3
2.3 主要试剂    3
3 实验方法    3
3.1 气相色谱测定条件    3
3.2 标准曲线的绘制    4
3.3 样品提取    4
3.4 样品净化    4
3.5 准确度和精密度    4
3.6 计算公式    5
4 结果分析与讨论    5
4.1 残留分析方法的确定    5
4.1.1 提取溶剂的选择    5
4.1.2 提取时间的选择    5
4.1.3 淋洗曲线的绘制    5
4.2 标准曲线的确立    6
4.3 准确度和精密度    7
4.4 消解动态试验结果    7
5 结论    10
参考文献    11
致谢    12