Cho Soon-Kil, Abd El-Aty A M, Park Young-Seok, Choi Jeong-Heui, Khay Sathya, Kang Cheol-Ah, Park Byung-Jun, Kim Sun-Ju, Shim Jae-Han
Natural Products Chemistry Laboratory, Institute of Agricultural Science and Technology, College of Agriculture and Life Science, Chonnam National University, 300 Yong-Bong Dong, Buk-Ku, Gwangju 500-757, Republic of Korea.
Biomed Chromatogr. 2007 Jun;21(6):602-9. doi: 10.1002/bmc.792.
An analytical procedure using accelerated solvent extraction and gas chromatography with an electron capture detector has been optimized to simultaneously determine the residue of two insecticides (diazinon and EPN) and one fungicide (isoprothiolane) in polished rice and was confirmed by GC-mass spectrometry. Several parameters, including temperature, pressure, solvent ratio, cell size and cell cycle, were thoroughly investigated to find the optimal extraction conditions. The average recoveries of the three pesticides were between 82.7 and 126.4% at spiking levels of 0.1 and 0.5 ppm. The relative standard deviations were less than 7% for all of the recovery tests. The optimum accelerated solvent extraction operating conditions were 100 degrees C, 1500 atm, acetone-n-hexane (20:80 v/v) as the extraction solvent, two cycles, and a cell size of 33 ml. The total extraction time was approximately 20 min. The optimized procedure has also been applied to the determination of diazinon, isoprothiolane and EPN in real rice samples. In conclusion, accelerated solvent extraction was used for the first time for the analysis of diazinon, isoprothiolane and EPN in polished rice and offers the possibility of a fast and simple process for obtaining a quantitative extraction of the studied pesticides.
一种采用加速溶剂萃取和带有电子捕获检测器的气相色谱法的分析程序已得到优化,用于同时测定精米中两种杀虫剂(二嗪农和EPN)和一种杀菌剂(异稻瘟净)的残留量,并通过气相色谱 - 质谱联用仪进行了确证。对包括温度、压力、溶剂比例、萃取池体积和萃取循环次数在内的多个参数进行了深入研究,以找到最佳萃取条件。在0.1和0.5 ppm的加标水平下,三种农药的平均回收率在82.7%至126.4%之间。所有回收率测试的相对标准偏差均小于7%。最佳加速溶剂萃取操作条件为100℃、1500大气压、丙酮 - 正己烷(20:80 v/v)作为萃取溶剂、两个循环以及33 ml的萃取池体积。总萃取时间约为20分钟。该优化程序还已应用于实际大米样品中二嗪农、异稻瘟净和EPN的测定。总之,加速溶剂萃取首次用于精米中二嗪农、异稻瘟净和EPN的分析,并为快速简便地定量萃取所研究的农药提供了可能性。