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[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。
[Objective] The residues of A-Dimethoate in rice and paddy environment can not be ignored. It is necessary to establish a sensitive, accurate and simple analytical method. [Method] The HPLC-FLD method was developed to determine the residue of carbaryl in rice and paddy field samples by derivatization. Water samples were extracted with dichloromethane. Soil samples, plants, rice and rice husk were extracted with acetone-water (7: 3 by volume), and were purified by liquid-liquid extraction and derivatized with HPLC-FLD. [Result] The minimum detectable amount of the salt was 1 × 10-11 g. The recoveries of carbaryl in water sample, soil sample, plant, rice and rice husk were 70.61% ~ 100.71%, and the coefficient of variation was 2.99 % ~ 4.23%, the lowest detection mass concentration (or mass fraction) were 0.000 1 mg / L, 0.000 5,0.000 5,0.000 3,0.000 5 mg / kg, respectively. [Conclusion] All met the technical requirements of pesticide residue analysis methods.