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作 者:韩永涛 张艳峰[1] 王会利[1] HAN Yongtao;ZHANG Yanfeng;WANG Huili(Key Laboratory of Environmental Biotechnology,Research Center for Eco-Environmental Science,Chinese Academy of Sciences,Beijing 100085,China)
机构地区:[1]中国科学院生态环境研究中心环境生物技术重点实验室,北京100085
出 处:《农药学学报》2020年第6期1033-1039,共7页Chinese Journal of Pesticide Science
基 金:2018年农业农村部农业行业标准制定和修订项目(农财发[2018]46号)。
摘 要:2018年在山东、安徽、广西、河北、黑龙江和河南6地进行异菌脲在葱上的规范残留试验,建立了气相色谱-质谱(GC-MS)测定葱中异菌脲残留的分析方法。样品经乙酸乙酯提取,N-丙基乙二胺(PSA)、十八烷基键合硅胶(C18)和石墨化碳黑(GCB)净化,GC-MS检测。结果表明:在0.02~20 mg/L范围内,异菌脲质量浓度与其峰面积呈良好的线性关系,相关系数大于0.99。在0.05、0.5和20 mg/kg添加水平下,异菌脲在葱中的平均回收率为81%~96%,相对标准偏差(RSD)为3%~9%,定量限为0.05 mg/kg。异菌脲在葱中的消解符合一级反应动力学方程,半衰期为12.2~15.8 d。采用255 g/L异菌脲悬浮剂按有效成分750和1 125 g/hm2施药2~3次,于末次施药后3、5、7和14 d采样测定,葱中异菌脲的残留量为2.53~15.6 mg/kg。采用风险最大化的原则进行长期膳食风险评估,结果表明:一般人群异菌脲的国家估算每日摄入量(NEDI)为2.065 0 mg,占日允许摄入量的54.6%,异菌脲在葱中的残留不会对一般人群健康造成不可接受的风险。Supervised field trials were conducted in Shandong, Anhui, Guangxi, Hebei, Heilongjiang and Henan province in 2018. A highly efficient and simple method was developed for the determination of iprodione in shallot using gas chromatography-mass spectrometry(GC-MS). The samples were extracted with ethyl acetate, purified with primary secondary amine(PSA), octadecylsilane(C18) and graphitized carbon black(GCB), and detected by GC-MS. A good linear relationship between the peak area and the concentration of iprodione was observed in the range of 0.02-20 mg/L with the correlation coefficient greater than 0.99. The recoveries of iprodione in shallot ranged from 81% to 96% with the RSDs of 3%-9% at the spiked levels of 0.05, 0.5 and 20 mg/kg. The limit of quantitation of iprodione was 0.05 mg/kg. Results showed that the dissipation of iprodione in shallot fitted to the first order kinetics with the half-lives ranged from 12.2 to 15.8 d. The 255 g/L suspension concentrate(SC) of iprodione was sprayed at 750 and 1 125 g a.i./hm^2 for 2-3 times on shallot. Then samples were taken and determined at 3, 5, 7 and 14 d after the last application. Results indicated that the residue of iprodione in shallot was 2.53-15.6 mg/kg. Finally, the long-term dietary risk assessment was conducted using the principle of risk maximization. The results revealed that the national estimated daily intake(NEDI) of iprodione was 2.065 0 mg for general population, accounting for 54.6% of the acceptable daily intake,which demonstrated that the terminal residue of iprodione in shallot would not cause unacceptable risk to the health of the general population.
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