稻田样品中丁虫腈及其代谢产物的残留分析方法

建立了固相萃取-气相色谱法同时测定稻田环境样品中丁虫腈及其代谢产物的残留分析方法,即:稻田水样品以二氯甲烷萃取,水稻土样品以丙酮提取后再经乙酸乙酯萃取,稻株样品以乙腈提取后用CarbonNH2固相萃取小柱净化,然后均用气相色谱-电子捕获检测器(GC-ECD)检测。结果表明,稻田水中丁虫腈及其代谢产物的最低检测质量浓度均为0.01 mg·L-1,土壤和水稻植株中目标物最低检测质量含量为0.015 mg·kg-1。在该方法条件下,当添加水平为0.05～1.0 mg·L-1(或mg·kg-1)时,稻田水、土壤和水稻植株中丁虫腈及其代谢产物的平均回收率为75.1%～109.2%,变异系数为1.0%～7.9%。

Determination of Flufiprole and Its Metabolites in Samples From Paddy Field

A method using solid-phase extraction and gas chromatograph-microelectron capture detector(GC-ECD) was developed to detect flufilprole and its metabolites in plant,soil and water in paddy fields.Water samples were extracted with methylene chloride,soil samples first with acetone and then with ethyl acetate and plant samples first with acetonitrile and then with CarbonNH2 and at the end cleaned up with solid phase extraction(SPE) for analysis with GC-ECD.Results of the analysis show that the lowest content of pollutants detected was 0.01 mg·L-1 in the water and 0.015 mg·kg-1 in the soil and the plant.When 0.05-1.0 mg·L-1(or mg·kg-1) of the pollutants were added into the field,the recovery rate of using this method was in the range of 75.1%-109.2% with variation coefficient being 1.0%-7.9%.This method is simple,accurate,and readily applicable in the analysis of paddy field samples.