固相萃取-高效液相色谱同时测定大米中的4种烟碱农药残留量

建立了高效液相色谱法同时测定大米样品中呋虫胺、噻虫胺、吡虫啉、吡虫清4种烟碱农药残留量的检测方法,对4种烟碱农药在ENVI-Florisil和Carb复合固相萃取柱上的保留行为进行了研究。样品用乙腈提取,固相萃取净化,HPLC-DAD分离检测,外标法定量。峰面积与标准溶液浓度在0.1～1.0 mg/L范围内呈良好的线性关系,相关系数大于0.9996。样品加标回收率为75.5%～96.0%,相对标准偏差为0.49%～4.36%(n=6),检出限达到0.004 mg/kg。

DETERMINATION OF FOUR KIND OF NEONICOTINOID RESIDUES IN RICE BY SOLID PHASE EXTRACTION HPLC

Reverse phase high performance liquid chromatography method was developed for the determination of dinotefuran, clothianidin, imidacloprid and acetamiprid residues in rice. The retention behaviors of dinotefuran, clothianidin, imidaeloprid and acetamiprid on the ENVI - Florisil and carb were investigated. Neonicotinoid residues were extracted from the sample with acetonitrile, then were cleaned up with a SPE tube. The target was separated in an XDB - C18 column and detected with a DAD detector, external standard method to quantify. There was a good linear correlation between the peak areas and concentration of the four neonicotinoid residues in the range of 0.1 - 1.0 mg/L with the calibration coeffiicient more than 0. 999 6. The average recoveries in samples were 75.5% - 96.0%. The relative standard deviation were 0.49% - 4.36% （ n = 6） and the detection limit was 0. 004 mg/kg.