Yang Yun, Zhang Zhuo-Min, Li Gong-Ke
Chemistry and Chemical Engineering School, Sun Yat-sen University, Guangzhou, China.
Se Pu. 2002 Sep;20(5):390-3.
A method of microwave-assisted extraction (MAE) followed by gas chromatography-mass spectrometry (GC-MS) for the determination of organophosphorus pesticides (OPPs) in vegetables has been developed. The OPPs studied were diazinon, parathion and isocarbophos. Several extraction solvents were compared on the MAE efficiency. Dichloromethane gave good recovery, and was chosenfor the procedure. A three-level orthogonal array design was used to optimize the MAE process.Factors affecting the MAE efficiency were considered, including the solvent amount and extraction time.The linear ranges of the method were from 4 ng/g to 400 ng/g for diazinon and parathion, and from 20 ng/g to 400 ng/g for isocarbophos. The detection limits were 0.29 ng/g, 1.70 ng/g and 2.30 ng/g for diazinon, parathion and isocarbophos respectively. Two sets of spiked vegetable samples of 200.0 ng/g and 50.0 ng/g were determined. The recoveries were from 72.2% to 102.0%, and the RSDs were from 1.5% to 11.0% (n = 3). The analytical results agreed quite well with those obtained by conventional extraction with mechanical shaking (EMS). The method is fast and solvent-saving.
建立了一种微波辅助萃取（MAE）结合气相色谱 - 质谱（GC - MS）法测定蔬菜中有机磷农药（OPPs）的方法。所研究的有机磷农药为二嗪磷、对硫磷和水胺硫磷。比较了几种萃取溶剂对微波辅助萃取效率的影响。二氯甲烷回收率良好，因此被选用于该方法。采用三水平正交试验设计优化微波辅助萃取过程。考虑了影响微波辅助萃取效率的因素，包括溶剂量和萃取时间。该方法中二嗪磷和对硫磷的线性范围为4 ng/g至400 ng/g，水胺硫磷的线性范围为20 ng/g至400 ng/g。二嗪磷、对硫磷和水胺硫磷的检出限分别为0.29 ng/g、1.70 ng/g和2.30 ng/g。测定了两组加标量分别为200.0 ng/g和50.0 ng/g的蔬菜样品。回收率为72.2%至102.0%，相对标准偏差为1.5%至11.0%（n = 3）。分析结果与传统机械振荡萃取（EMS）法所得结果相当吻合。该方法快速且节省溶剂。
