乙草胺与醚磺隆混合制剂的液谱分析方法

采用反相商诳液相色谱法,以Ｃ１８柱为固定相,用２３６ｎｍ紫外检测器定量测定局草胺和醚磺隆混合制剂的含量。本方法的变异系数分别为０．６８％、１．８６％;标准偏差分别为０．１４５、０．０７７;平均回收率分别为９８．５９％、９８．８１％;线笥相关系数分别为０．９９９３、０．９９９６。     

Cinosulfuron: chemical and biological degradability, adsorption and dissipation in flooded paddy field sediment

Cinosulfuron is a sulfonylurea herbicide largely used in the extensive cultures of flooded rice in North Italy. The degradation of cinosulfuron has been investigated in sterile aqueous solutions at 30 degrees C at different pH values. It was rapidly degraded at acidic pH (half-lives 3, 9 and 43 days at pH 4, 5 and 6, respectively) while the half-life was > 1 year at pH 7 and 9. Two degradation products formed by cleavage of the sulfonylurea bridge were identified by LC-MS. Degradation by selected mixed microbial cultures tested in aerobic and anaerobic conditions was very slow and attributable to chemical hydrolysis due to the acidic pH of the cultural broths. Degradation took place in freshly collected rice field water treated for two years with cinosulfuron but, in this case also, chemical hydrolysis prevailed over microbial degradation. In contrast, in flooded sediment simulating the paddy field environment, the dissipation rate of cinosulfuron was higher than expected from chemical hydrolysis according to the pH of the system, indicating the involvement of soil microflora. Although the herbicide exhibited a reduced affinity for the sediment surfaces demonstrated by the low value of the K(f) Freundlich coefficient (0.87 on a micromolar basis), the rapid dissipation observed in the simulated paddy field should prevent its leaching to ground water.     

醚磺隆在南方三种土壤中的吸附行为

采用批量平衡法,研究了除草剂醚磺隆在3种土壤中的吸附行为,探讨了温度和离子强度等因素对吸附的影响。结果表明,醚磺隆在3种土壤中的吸附均为线性吸附,吸附常数Kd为9.883～15.901mL·g-1,且在试验浓度范围内,土壤对醚磺隆的吸附能力随温度的升高和离子强度的增大而增强。     

醚磺隆在稻株、稻米、土壤和田水中残留的分析方法

研究并建立了醚磺隆(cinosulfuron)在水稻植株、稻米、土壤及田水中的残留分析方法。水稻植株和稻米样品以甲醇提取,经石油醚、二氯甲烷液液分配,固相萃取(SPE)净化,高效液相色谱(HPLC)测定;土壤样品经甲醇提取后,高效液相色谱(HPLC)测定;田水样品经固相萃取(SPE)净化,高效液相色谱(HPLC)测定。醚磺隆的最小检测量为2 ng,水稻植株和稻米中醚磺隆最小检测浓度为0.04 mg.kg-1;土壤中醚磺隆最小检测浓度为0.02mg.kg-1;田水中醚磺隆的最小检测浓度为0.04 mg.L-1。添加浓度0.04~0.2 mg.kg-1时,水稻植株中醚磺隆的回收率为98.1%~105.9%,变异系数3.9%~4.4%;稻米中醚磺隆的回收率为87.8%~98.8%,变异系数2.9%~6.6%;添加浓度0.02~0.2 mg.kg-1时,土壤中醚磺隆的回收率为87.9%~100.5%,变异系数2.5%~7.3%;添加浓度0.04~0.2 mg.L-1时,田水中醚磺隆的回收率为86.2%~107.9%,变异系数为3.3%~8.6%。该方法的准确性、精确性以及灵敏度均符合农药残留分析的要求。