当前位置: 首页 > 文章 > 小白菜中残留高效氯氰菊酯及氟氯氰菊酯的超临界流体萃取条件的研究 农业环境科学学报 2005,24 (03) 201-204
Position: Home > Articles > Extracting Conditions of Cypermethrin and Cyfluthrin in Cabbage by Supercritical Fluid Extraction (SFE) Journal of Agro-Environment Science 2005,24 (03) 201-204

小白菜中残留高效氯氰菊酯及氟氯氰菊酯的超临界流体萃取条件的研究

作  者:
杨立荣;陈安良;冯俊涛;郝双红;张兴
单  位:
西北农林科技大学无公害农药研究服务中心
关键词:
超临界流体;残留;高效氯氰菊酯;氟氯氰菊酯
摘  要:
应用超临界流体萃取(SupercriticalFluidExtraction,SFE)技术,建立了高效氯氰菊酯和氟氯氰菊酯的萃取分离及GC检测方法。高效氯氰菊酯和氟氯氰菊酯的SFE优化条件分别为:压力4000psi、温度65℃、CO2体积10mL,萃取率99.96%;压力6000psi、温度45℃、CO2体积30mL,萃取率101.95%。
译  名:
Extracting Conditions of Cypermethrin and Cyfluthrin in Cabbage by Supercritical Fluid Extraction (SFE)
作  者:
YANG Li-rong, CHEN An-Liang, FENG Jun-tao, HAO Shuang-hong, ZHANG Xing(Biorational Pesticide Research and Service Center, Northwest Sci-Tech University of Agriculture and Forestry, Yangling 712100, China)
关键词:
supercritical fluid extraction; residue; cypermethrin; cyfluthrin
摘  要:
An extracting method of Cypermethrin and Cyfluthrin in cabbage using supercritical fluid extraction (SFE) was established in this study. It has been found that it was necessary to treat the sample at certain granularity and content of water before they were extracted using SFE. Therefore, the samples must be smashed in existence of liquid nitrogen and appropriate amount of hydromatrix was added. To investigate optimized extracting conditions of SFE, the orthogonal design of 3 factors and 5 levels was designed. The pressure and the volume of CO2 were found to be the most significant factors in affecting recoveries of both pesticides and the dose of modifier affected the recoveries at a great extent. We analyzed the whole 25 treatments synthetically, consequently, the selected extracting parameters of cypermethrin were: pressure 4 000 psi, temperature at 65 ℃, static time with 20 min, dynamic extraction volume of CO2 10 mL, 0.04 mL·g-1 of methanol as static modifier, and methanol as collecting solvent. The extracted samples could be determined without further treatment. The GC conditions were: column temperature: 80 ℃, detector and injection temperatures: 260 ℃, keeping the temperature at 80 ℃ for 5 min , raising rate of temperature at 10 ℃·min-1, equilibrium temperature 260 ℃(12 min), injection volume: 1 μL, carry gas 7 psi, attenuation 8, compensating gas 47 mL·min-1. We got the results: the recoveries of cypermethrin and cyfluthrin were 99.96% and 101.95% , retention time 26.62 min,26.67 min, respectively.

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