液下单滴微萃取-高效液相色谱法测定果汁中苯甲酰脲农药残留  

Determination of benzoyluea insecticides residues in grape juice drink by direct single-drop microextraction-high performance liquid chromatography

作　　者：周建科[1] 刘瑞英[1] 宋歌[1] 张明翠[1] 

机构地区：[1]河北大学理化分析中心,河北省分析科学技术重点实验室,保定071002

出　　处：《食品科技》2009年第8期290-293,共4页Food Science and Technology

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%.

关 键 词：除虫脲 氟苯脲 氟铃脲 高效液相色谱 单液滴微萃取 

分 类 号：TS207.53[轻工技术与工程—食品科学]