虫螨腈在稻田环境及水稻中的残留分析方法

Analytic Method for Detecting Chlorfenapyr Residue in Rice and Paddy Field

建立了一种高效液相色谱仪分析方法,用于测定虫螨腈在稻田水、土及稻株、稻米和稻壳中的残留量。水样用二氯甲烷萃取,土样、稻株、稻米和稻壳分别用乙腈、丙酮和甲醇提取,稻株和稻壳样品经中性氧化铝+活性炭柱净化,浓缩、定容,最后用紫外检测器(UVD)测定。添加浓度为0.1、1、5 mg/kg时,水样、土样、稻株、稻米和稻壳中虫螨腈的添加回收率为91.42%～112.33%,变异系数为0.68%～4.41%,虫螨腈的最低检出限为1.0×10-9g。最低检测质量浓度(或质量分数)分别为0.005、0.05、0.1、0.1、0.5 mg/kg。该方法的准确性、灵敏度均达到农药残留分析的要求。

A high-performance liquid chromatography(HPLC) method has established to determine chlorfenapyr residue in water and soil of paddy field,and in rice plant,rice and chaff,respectively.Chlorfenapyr residue in water,soil,rice plant,rice and chaff was extracted with methylene chloride,acetonitrile,acetone and methanol,respectively.The samples of rice plant and chaff were cleaned up with neutral alumina-activated carbon extraction,and then were detected by HPLC-UVD after condensed.When the samples were spiked at 0.1,1.0 and 5.0 mg/kg,the average recovery of chlorfenapyr in water,soil,rice plant,rice and chaff varied from 91.42% to 112.33%;the coefficient of variation was 0.68%-4.41%;the minimum detection limit was 1.0×10-9 g;the lowest determination concentration of water,soil,rice plant,rice and chaff was 0.005 mg/L,0.05 mg/kg,0.1 mg/kg,0.1 mg/kg and 0.5 mg/kg,respectively.Therefore,the accuracy and the sensitivity of the method met the requirements of pesticide residue analysis.