超高效液相色谱法测定水稻中茚虫威的残留  

Determination of Indoxacarb in Rice by UPLC

作　　者：刘龙腾[1] 龙胜基[1] 陈钟[1] 李雄[1] 胡德禹[1] 卢平[1] 张钰萍[1] 

机构地区：[1]贵州大学精细化工研究开发中心绿色农药与农业生物工程国家重点实验室培育基地和教育部重点实验室,贵阳550025

出　　处：《农药科学与管理》2013年第3期25-30,共6页Pesticide Science and Administration

摘　　要：建立了一种超高效液相色谱法（UPLC）测定水稻基质中茚虫威残留量的方法。稻田水用二氯甲烷直接萃取；稻田土、糙米和稻壳经甲醇溶液提取，旋蒸除去甲醇，浓缩液经二氯甲烷液液分配；稻秆经乙腈溶液提取，旋蒸除去乙腈，浓缩液经二氯甲烷液液分配；采用UPLC—PDA检测残留的茚虫威，在7min中内实现了茚虫威的完全分离。结果表明：茚虫威的质量浓度范围为0．05～5．18μg/mL时，峰面积与质量浓度具有良好的线性关系，相关系数为0．9999，仪器的最小检出量为0．52ng，最低检测浓度为1．25×10^-3mg／kg，茚虫威的平均回收率为79．77％～99．91％，相对标准偏差（RSD）为1．21％-9．25％。该方法适合于水稻基质中茚虫威含量的快速准确测定。A rapid Ultra-high Pressure Liquid Chromatography （UPLC） method was developed to determine the content of Indoxacarb in rice. Paddy water was purified by dichloro-methane; Soil, rice, and rice husk were extracted with methanol-water. Then the solution was evaporated on a rotary evaporator until methanol could be steamed out completely, followed by extraction with dichloromethane; Rice stalk was extracted with acetonitrile-water. Then the solution was e- vaporated on a rotary evaporator until aeetonitrile could he steamed out completely, followed by extraction with dichloromethane; then the Indoxaearb residues was determined by UPLC-PDA. Indoxacarb were completely separated in 7min. The results showed that the linearity range of the proposed method was 0.05-5.181~g/mL with the linear correlation coefficients of 0.999 9. The instrument limit of detection was 0.52ng. The minimum detectable concentration was 1.25x 10-3mg/kg. The average recovery was 79.77%-99.91%. And the relative standard deviation （RSD） was 1.18%-9.27%. The method was appropriate for quick and sensitive determination the content of Indoxacarb in rice.

关 键 词：茚虫威 超高效液相色谱 残留 水稻 

分 类 号：TS212.7[轻工技术与工程—粮食、油脂及植物蛋白工程] O657.72[轻工技术与工程—食品科学与工程]