甲维盐在水稻环境中的残留分析方法

Residue Analysis of Emamectin Benzoate in Rice Field

[目的]甲维盐在稻米和稻田环境中的残留不可忽视,建立一种灵敏、准确、简便的分析方法很有必要。[方法]探索了应用衍生化反应测定稻米和稻田环境样品中甲维盐残留量的HPLC-FLD分析方法。水样用二氯甲烷萃取,土样、植株、稻米和稻壳用丙酮-水（体积比7∶3）提取,经液液萃取净化,衍生化后采用HPLC-FLD测定。[结果]甲维盐的最小检出量为1×10-11 g,水样、土样、植株、稻米和稻壳中甲维盐的添加回收率为70.61%~100.71%,变异系数为2.99%~4.23%,最低检测质量浓度（或质量分数）分别为0.000 1 mg/L,0.000 5、0.000 5、0.000 3、0.000 5 mg/kg。[结论]均符合农药残留分析方法的技术要求。

Emamectin benzoate residues in rice and rice field can not be ignored,developing a sensitive,accurate and simple method is necessary.[Methods]A method of derivative determination of the residue of emamectinbenzoate in rice and rice field by HPLC-FLD was explored.Emamectin benzoate in the water was extracted withmethylene chloride,soil,plants,rice and rice hull were extracted with acetone/water（7∶3,by vol）,the extracts werecleaned up by liquid-liquid extraction,and detected by HPLC-FLD after derivatization.[Results]The results showedthat the minimum detectable amount of emamectin benzoate was 1×10-11g,and the average recoveries in water,soil,plants,rice and rice hull were 70.61-100.71%,and the coefficient of variation were 2.99-4.23%.The minimumdetectable concentrations in water,soil,plants,rice and rice hull were 0.000 1 mg/L,0.000 5,0.000 5,0.000 3 and0.000 5 mg/kg respectively.[Conclusions]All met the technical requirements of pesticide residue analysis.