【摘要】 本文研究建立了溴苯腈在土壤及水中的残留测定方法。研究了溴苯腈在土壤及水中残留分析的不同检测法、提取净化法,比较了不同提取溶剂和提取次数对水中溴苯腈残留的提取效果及索氏提取法、振荡提取法和超声-微波协同萃取法对土壤中溴苯腈残留的提取效果。结果表明,溴苯腈在土壤及水中的残留测定适合采用高效液相色谱法;确立了溴苯腈在水中的残留测定方法为正己烷作萃取溶剂,液-液分配萃取2次,用高效液相色谱测定。当溴苯腈在水中的添加浓度为0.10～1.00mg·L-1时,标准添加回收率为98.7%～111.1%、变异系数为0.80%～7.85%;溴苯腈在土壤中残留分析的3种提取方法均能达到农药残留分析的要求,通过比较不同提取时间和溶剂用量的提取效果,最终确定了溴苯腈在土壤中的残留分析方法为用丙酮∶水∶冰乙酸=80∶18∶2(V∶V∶V)经振荡提取或超声-微波协同萃取,再经液-液分配净化,最后用高效液相色谱测定。当溴苯腈在土壤中的添加浓度为0.05～5.00mg·kg-1时,振荡提取法相应的标准添加回收率为90.9%～102.0%、变异系数为0.08%～18.44%,超声-微波协同萃取法相应的标准添加回收率为95.6%～109.4%、变异系数为0.18%～16.01%,均符合农药残留分析的要求。更多还原

【Abstract】 A method was developed for the residue analysis of bromoxynil in soil and water. First,through comparing HPLC with GC to determine bromoxynil,made sure HPLC as the proper method,and then studied the effects on different wavelengths of bromoxynil. The results showed that determination of bromoxynil by HPLC would achieve the rapid,good separation effect and symmetrical peak form. Bromoxynil in water was extracted by liquid-liquid separation,and studied different extraction times and solvents. The results showed that hexane was the better extraction solvent and twice was the better extraction times. When the concentration of bromoxynil in water were 0.10 ~1.00 mg·L-1,the average recoveries and coefficient of shaking extractions were 98.7%~111.1%,0.80%~7.85%. To study the effect of shaking extraction,soxhlet extraction and ultrasound-microwave extraction on the residue of bromoxynil in soil,the three extraction methods could all meet the demand of pesticide residue analysis,but soxhlet extraction was more slowly and wasted more solvent than the other two methods. Finally the residue analysis of bromoxynil in soil was extracted with acetone: water: glacial acetic acid (80∶18∶2 by volume) under continuous shaking or ultrasound-microwave. The extract was cleaned up by liquid-liquid separation. Bromoxynil in residues were detected by HPLC. When the concentration of bromoxynil in soil were 0.05~5.00 mg·L-1,the average recoveries and coefficient of shaking extraction were 90.9%~102.0%,0.08%~18.44%,the average recoveries and coefficient of ultrasound-microwave extraction were 95.6%~109.4%,0.18%~16.01%. These results showed that the method met the demand of pesticide residue analysis.更多还原