高效液相色谱串联质谱法测定水产养殖水中氟虫腈及其代谢物残留

Determination of Fipronil and Its Metabolite Residues in the Aquaculture Water by High-performance Liquid Chromatography-tandem Mass Spectrometry

为了能够快速筛查水产养殖水中氟虫腈及其代谢物含量,使用液液萃取前处理,高效液相色谱串联质谱联用建立了养殖水中氟虫腈及其代谢物的检测方法。优化后的前处理条件:养殖水过滤后取100.0 mL,以石油醚作为萃取溶剂,摇匀后,取上清液,共提取3次,提取液40℃以下氮吹近干,以1.0 mL甲醇水复溶,过膜,上机检测。色谱条件:色谱柱:Eclipse Plus C18,流动相为甲醇-水,在7 min内氟虫腈及其代谢物分离良好。质谱条件:电喷雾离子源(ESI);负离子模式同时扫描;多反应监测(MRM)采集方式。氟虫腈及其代谢物在10~500 ng·mL^(-1)的范围内均具有良好的线性关系,相关系数不小于0.999,平均加标回收率为65.9%~88.5%,相对标准偏差为1.8%~13%,各组分方法定量限为0.1 ng·mL^(-1)时信噪比均大于10。该方法适用于养殖水中氟虫腈及其代谢物的快速检测。

In order to quickly screen the content of fipronil and its metabolites in the aquaculture water,a method for the detection of fipronil and its metabolites in the aquaculture water was established by using the liquid-liquid extraction pretreatment and the high-performance liquid chromatography-tandem mass spectrometry.The optimized pretreatment conditions were as follows:100.0 mL aquaculture water was selected after the filtration,and the petroleum ether was used as the extraction solvent.After shaking well,the supernatant was taken and extracted for 3 times.The extracting solution was dried by nitrogen below 40℃,redissolved with 1.0 mL methanol water,passed through the membrane,and detected on the machine.The chromatographic conditions were as follows:the chromatographic column was Eclipse Plus C18,the mobile phase was methanol-water,and the fipronil and its metabolites were well separated within 7 min.The mass spectrometry conditions were as follows:the electrospray ionization source(ESI);simultaneously scanning by using the negative ion mode;the acquisition mode with the multiple reaction monitoring(MRM).Fipronil and its metabolites had a good linear relationship in the range of 10 ng·mL^(-1)-500 ng·mL^(-1),the correlation coefficient was not less than 0.999,the average recovery rate was 65.9%-88.5%,and the relative standard deviation was 1.8%-13%.The signal-to-noise ratio(SNR)was all greater than 10 when the limit of quantification of each component method was 0.1 ng·mL^(-1).The method was suitable for the rapid detection of fipronil and its metabolites in the aquaculture water.