金鱼体内吡虫啉及其代谢产物的检测方法

A Method for Detection of Imidacloprid and Its Metabolites in Carassius auratus

本研究采用高效液相色谱-质谱联用法建立了金鱼体内吡虫啉及其代谢产物的测定方法。选用Eclipse C18柱,甲醇-0.1%甲酸作为流动相进行梯度洗脱,离子源为ESI源,选择离子扫描模式(SIM)进行检测,利用外标法进行分析和定量。经质谱数据分析,吡虫啉在金鱼体内的代谢产物主要有吡虫啉脲、烯式吡虫啉、5-羟基吡虫啉和6-氯烟酸。上述方法中吡虫啉、吡虫啉脲、烯式吡虫啉、5-羟基吡虫啉、6-氯烟酸质量浓度与峰面积间的线性相关系数均大于0.99,相对标准偏差分别为3.41%、1.98%、3.79%、2.84%和2.64%。提取方法进行优化后,选用了乙酸乙酯∶水(2∶1,V/V)对金鱼组织进行提取,上述5种物质的平均添加回收率分别为96.08%、99.77%、85.25%、87.24%和100.23%。该方法的精密度和准确度都较高,线性相关性好,可用于金鱼体内吡虫啉及其代谢产物的定量分析。

In this study,imidacloprid and its metabolites in Carassius auratus were determined by high performance liquid chromatogram-mass spectrometry.HPLC analysis of tissue samples from C.auratus was performed on an Eclipse Cis column using methanol-0.1%formic acid as the mobile phase.The ion source was ESI,the ion scanning mode(SIM)and the external standard method were used for analysis and quantification.The results showed that the metabolites of imidacloprid in C.auratus were imidacloprid-urea,imidacloprid-olefin,5-hydroxy imidacloprid and 6-chloro nicotinic acid.The linear correlation coefficients between the mass concentration and peak area of imidacloprid,imidacloprid-urea,imidacloprid-olefin,5-hydroxy imidacloprid and 6-chloronicotinic acid were all above 0.99 and the coefficients of variation were 3.41%,1.98%,3.79%,2.84%,2.64%.After the optimization of the extraction method,the C.auratus tissue was extracted with ethyl acetate:water(2:1,V/V),the average recoveries were 96.08%,99.77%,85.25%,87.24%,100.23%.The results showed that the method could be used for quantitative analysis of imidacloprid and its metabolites in C.auratus with high precision and accuracy,good linear correlation.