摘要
建立了液下单液滴微萃取-高效液相色谱法测定葡萄果汁中3种苯甲酰脲农药残留的方法。Diamonsil C18(5μm,250mm4.6mm)分离柱,甲醇-水(体积比85:15)流动相,流速1.0mL/min,室温,紫外检测波长254nm。最佳萃取条件为:室温,1.5μL的三氯甲烷液滴为萃取剂,转速240r/min,pH3,NaCl含量40g/L,时间10min。除虫脲、氟铃脲和氟苯脲在0.01~10.0mg/L范围内均有良好线性,检出限分别为0.005、0.01、0.01mg/L,添加回收率在80.84%~92.86%之间.相对标准偏差(RSD)为2.04%~3.11%。
A simple and efficient direct single-drop microextraction(SDME) in conjunction with high performance liquid chromatography (HPLC) has been developed for extraction and determination of 3 benzoylurea insecticides residues from grape juice drink samples.The components were separated by a Diamonsil C18(5 μm, 250 mm 4.6 mm). Mobile phase was a mixture of methanol and water (the ratio of volume was 85:15). Factors relevant to the extraction efficiency were studied and optimized. Under the optimized extraction conditions(extraction solvent: trichloromethane, extraction temperature: room tem-perature, sodium chloride concentration: 40 g/L, pH3, microdrop and sample volumes: 1.5 μL and 5 mL respectively, the stirring rate: 240 r/min and the extraction time: 10 min), the results were pleasant. The methodology exhibited good linearity between 0.01-10.0 lag/mL with correlation coefficiency of 0.9995-0.9996. The detection limits of quantification were 0.005-0.01 mg/L. The average recovery of benzoylurea pesticides ranged from 80.84%- 92.86%. The relative standard deviations(RSDs)(n=6) were 2.04%-3.11%.
出处
《食品科技》
CAS
北大核心
2009年第8期290-293,共4页
Food Science and Technology
关键词
除虫脲
氟苯脲
氟铃脲
高效液相色谱
单液滴微萃取
diflubenzuron
hexafluron
teflubenzuron
high performance liquid chromatography
single-dropmicroextraction