反相高效液相色谱法测定稻谷中几种农药残留  

Determination of pesticide residues in rice by reversed phase high performance liquid chromatography

作　　者：杨精华[1] 张怡一 钱源[1] 殷实[1] 王立峰[1] 

机构地区：[1]南京财经大学,江苏南京210000

出　　处：《粮食与饲料工业》2016年第5期58-61,共4页Cereal & Feed Industry

基　　金：国家科技支撑计划项目(2014BAD04B03);国家行业性公益专项项目(2013449XXX)

摘　　要：针对稻谷中的多种农药残留,建立了反相高效液相色谱测定吡虫啉、西维因、杀螟硫磷、甲基毒死蜱和溴氰菊酯5种农药残留的检测方法。试验选用Waters Xbridge TMC18色谱柱（4.6×250mm,5μm）,在柱温30℃、检测波长290和240nm、流动相乙腈∶水=90∶10（体积比）、流速1.0ml/min、进样量10.0μl条件下,5种农药浓度在0.1～10.0 mg/kg时呈良好的线性关系,相关系数分别为：R^2吡=0.999 8,R^2西=0.999 9,R^2杀=0.999 8,R^2甲=0.999 1,R^2溴=0.998 7;吡虫啉平均回收率为74.30%～94.43%,相对标准偏差为3.98%～11.24%;西维因平均回收率为79.48%～98.89%,相对标准偏差为0.64%～7.54%;杀螟硫磷平均回收率为75.17%～94.11%,相对标准偏差为1.14%～7.10%;甲基毒死蜱平均回收率为84.29%～100.49%,相对标准偏差为0.44%～7.40%;溴氰菊酯平均回收率为78.52%～99.93%,相对标准偏差为2.15%～9.72%。结果表明,该方法简便快速、灵敏准确,适于稻谷中多种农药残留检验。We studied multiple pesticide residues in rice, and established a method with QuEChERS and reverse-phase high performance liquid chromatography for the simulataneous determination of 5 pesticide residue, which were imidacloprid, carbaryl, fenitrothion, methyl, chorpyrifos methyl and deltamethrin. Samples were extracted with acetonitrile, salting out, purif ying, and then using high performance liquid chromatography-ultraviolet detector for testing. The chromatography column was Water Xbridge TMC18 （4. 6× 250 mm, 5 μm）, column temperature of 30℃, detection wavelength of 290 and 240 nm; mobile phase of acetonitrileand water（90 ： 10）, flow rate of 1.0 ml/min, sample size 10.0 μl. The 5 kinds of pesticide in the range showed good linearity from 0.1 to 10.0 mg/kg, linear coefficients were 0. 999 8,0. 999 8,0. 999 9,0. 999 1,0. 998 7, respectively. The average recovery of imidacloprid was 74.30%～ 94.43 %, the relative standard deviation was 3.98 %～ 11.24 % ; the average recovery of carbaryl was 79.48%～98.89%, the relative standard deviation was 0.64% ～7.54% ; the average recovery of fenitrothion was 75.17 % ～ 94.11%, the relative standard deviation was 1.14%～7. 10 % ; the average recovery of chlorpyrifos-methyl was 84.29%～100. 49%, the relative standard deviation was 0.44%～7. 40% ; the average recovery of delatmethrin was 78.52%～99.93%, the relative standard deviation was 2.15% ～9. 72%. Results showed that the advantages of the meth od was simple, rapid, sensitive and accurate, which was very suitable for testing multiple pesticide in rice.

关 键 词：稻谷 农药残留 QuEChERS前处理 反相高效液相色谱 

分 类 号：S481.8[农业科学—农药学]